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t5'3.'tS METHODS OF TEST¡NG THE MECHANICAL PROPERTIES OF ORTHODONTIC WIRES A report submitted in partial fulfilment of the requirements for the degree of Master of Dental SurgerY KATHERINE RUTH ALLEN B.D.S. Department of Dentistry Faculty of Dentistry The University of Adelaide South Australia April 1994 BY

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Page 1: Methods of testing the mechanical properties of ... · t5'3.'tS METHODS OF TEST¡NG THE MECHANICAL PROPERTIES OF ORTHODONTIC WIRES A report submitted in partial fulfilment of the

t5'3.'tS

METHODS OF TEST¡NG THE MECHANICAL PROPERTIES OF

ORTHODONTIC WIRES

A report submitted in partial fulfilment of the requirements for the degreeof Master of Dental SurgerY

KATHERINE RUTH ALLEN B.D.S.

Department of Dentistry

Faculty of Dentistry

The University of Adelaide

South Australia

April 1994

BY

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TABLE OF CONTENTS

NOMENCLATURE

LIST OF FIGURES

LIST OF TABLES

SUMMARY

SIGNED STATEMENT

ACKNOWLEDGEMENTS

Chapter 1 ¡rurnooucrtoN

Chapter 2 IIERATURE REVIEw

MECHANICAL PROPERTIES OF ORTHODONTIC TOOTH

MOVEMENT

THE IDEAL ARCHWIRE

TERMINOLOGY USED WHEN DISCUSSING THE MECHANICAL

PROPERTIES OF WIRES

PRODUCT]ON OF WIRES

THE CRYSTALLIZATION OF MOLTEN METALS

THE EFFECTS OF COLD WORKING AND ANNEALING ON THE

CRYSTAL STRUCTURE

HISTORY OF ORTHODONTIC WIRES

THE CHEMICAL COMPOSITION AND MECHANICAL

PROPERTIES OF SPECIFIC WIRES

GOLD

STAINLESS STEEL

xtx

PAGE

VI

xil

XVI

XVIII

11

11

12

13

15

15

15

1

3

3

3

4

M ULTIBRAIDED STAINLESS STEEL 19

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CHROMIUM.COBALT

NICKEL-TITANIUM

BETA-TITANIUM

ALPHA-TITANIUM

SUMMARY

Chapter 3 AtMs oF THE lNVEsrlGATloNS

Chapter 4 MATERIALS AND METHoDS

CONVENTIONAL TENSILE TESTS

BEND TESTS

ELECTROPOLISHING

CANTILEVER TESTS

THREE POINT BEND TESTS

USE OF LOAD AND UNLOAD DATA

RESONANCE

SPEED OF SOUND

MICROHARDNESS TEST

MACROHARDNESS TEST

SURFACE APPEARANCE

DETAILED MICROSTRUCTURAL DATA

Chapter 5 REsuLTs AND DlscussloN

ELASTIC MODULUS VALUES

CONVENTIONAL TENSILE TESTS

20

21

27

28

29

30

32

32

32

38

40

45

47

48

50

52

54

54

56

67

67

69

75BEND TESTS

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ARCHFORM 75

CANTILEVER TESTS B2

OTHER TECHNIOUES 87

TESTING OF ANNEALED SPECIMENS 91

OTHER WIRES

RESONANCE 9B

VELOCITY OF SOUND 103

SUMMARY OF ELASTIC MODULUS TESTS 108

A COMPARISON OF ELASTIC MODULUS VALUES DERIVED 109

FROM DIFFERENT TECHNIOUES USING LOAD DATA

94

EFFECT OF DIAMETER CHANGE ON ELASTIC MODULUS 111

VALUE

THE EFFECT OF DATA MOD¡FICATION ON ELASTIC 111

MODULUS VALUES

MICROHARDNESS TESTS 114

MACROHARDNESS TESTS 116

SURFACE APPEARANCE OF WIRES 117

SURFACE EFFECTS OF PULSE STRAIGHTENING 117

SURFACE CHANGES AFTER ELECTROPOLISHING 117

FRACTOGRAPHY 120

DETAILED MICROSTRUCTURAL DATA 127

Chapter 6 coNclusloNs 132

Chapter 7 FUTURE RESEARcH 135

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BIBLIOGRAPHY

APPENDICES

137

Vol II

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NOMENCLATURE

Unless otherwise Stated the symbols have the following meaning:

A

atct

b

br

ddD

DPN

E

ep

ep 25

F

"fnGPa

h

HVHz

III

m

m

nt

P

ps

rpm

se nt

SEM

SS

ssp

sspp

sspp ps

SSS

sssp

area in mm squared

alpha-titaniumlength or distance

breadth

beta-titanium

diameter

the length of the diagonal of a square in micrometers

length of the diagonal in millimetres

Diamond Pyramidal Hardness Number

elastic modulus (or Young's modulus)

electropolished

electropolished for 25 seconds

measured load

frequency of vibration .

Giga Pascal

height

Vickers hardness number

hertz (cycles per second)

moment of inertia

second moment of area

distance

MASS

metres

nickel-titanium

applied load

pulse straightened

revolutions per minute

superelastic nickel-titanium

scanning electron microscoPe

stainless steel

stainless steel premium

stainless steel premium Plus

stainless steel premium plus, pulse straightened

stainless steel suPreme

stainless steel special Plus

vl

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TEM

TMA

TTR

v

vYS

Dimensions

o

ttp

transmission electron microscope

titanium molybdenum alloY

transition temperature range

velocityextensionyield strength

stress

strain

maximum flexibilitydensitymicrometre

microsecond

pm

ps

018 = O.O18" (O.45mm)

Note: Some orthodontic wires are supplied in imperial units but all

scientific studies should use metric.

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LIST OF FIGURES

71

FIGURE SUBJECT

14

Stress-strain curve illustrating proportional limit, yield

strength, UTS, failure point, elastic modulus.

Stress-strain curve illustrating resilience and formability' 1O

PAGE

26

33

58

2

3

34

4

5

6

A wire specimen wrapped around an aluminium casing

prior to tensile testing

A milled brass wire holder in a stand allowing 36

adjustments in the vertical Plane

steel holder glued to the Mettler 61OO pan with anterior 37

section of archwire in a groove in steel support

Electropolishing unit (Rocky Mountain 70O,USA) 39

A cantilever bend test us¡ng a knife edge to support the 42

free end of the specimen

10 A 3-point bend test

11 Apparatus for resonance testing

12 Apparatus for measuring speed of sound along a wire 51

13 A photomicrograph of microhardness indentations near 53

the edge of the specimen

Stress-strain curve illustrating differences between

stainless steel, nickel-titanium and superelastic nickel-

titanium.

A universal Instron testing machine with an

extensometer in position

Curing characteristics of G-1 Epoxy used for preparing

TEM cross sections

Disc cutting and grinding for cross-sectional TEM

specimen

7

I

9

46

49

15 58

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16

17a

17b

18a

18b

18c

19

20

21

Precision dimple grinder and polisher 59

Magnified view of the grinding wheel and mount on 61

dimple grinder

Dimpled specimen 61

lon milling of a cross-sectional specimen 62

Effect of OctagunTM voltage on specimen thinning rate. 62

Specimen current versus beam angle for argon milling 62

of copper.

Preparation of a single wire specimen to minimise the 64

epoxy

E.A.Fischione model 12O-23O twin jet electropolishing 66

unit

Diagramatic stress-strain curve illustrating tangents to 73

the curve which may be chosen to calculate the elastic

modulus.

Diameter changes with continuous electropolishing of 79

sssp 020

Diameter changes with cumulative electropolishing of 80

sssp O2O

Wave forms as seen on oscilloscope Screen in velocity 1O4

of sound testing

Modification of stress-strain data to improve the fit of 112

the straight line for load data

Modification of stress-strain data to improve the fit of 1 13

the stra¡ght line for unload data

SEM micrograph (75x magnification) of as-received 1 18

sspp 018 wire surface

22

23

24

25

26

27

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28 SEM micrograph (75x magnification) of as-received

sspp ps O18 wire surface

SEM micrograph (75x magnification) of as-received

sspp O2O wire surface

SEM micrograph (3OOx magnification) of as-received

sspp O2O wire surface

SEM micrograph (75x magnification) of sspp 020 wire

surface after 25" electropolishing

SEM micrograph (75x magnification) of sspp 020 wire

surface after 50" electropolishing

SEM micrograph (75x magnification) of sspp 02O wire

surface after 1 50" electropolishing

SEM micrograph showing "tag" formation after

deliberate fracture of a wire specimen.

SEM micrograph showing variation in the extent of

"tag" formation.

SEM micrograph showing variation in the extent of

"tag" formation.

SEM micrograph of a fractured wire surface showing

differences in the direction of the crack path.

SEM micrograph of a fractured specimen showing

distinct steps on the surface.

SEM micrograph of a fractured wire illustrating a zone

normal or possibly inclined in the opposite direction to

the "tag".

118

119

119

121

121

122

124

125

125

126

126

30

29

31

32

33

35

36

37

38

39

34 SEM micrograph (3OOx magnification) of sspp O2O wire ' 122

surface after 150" electropolishing

Number of bends possible until point of wire fracture 123

40

41 128

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42 SEM micrograph of a fractured wire surface where a

pronounced crack separates the "tag" and zone normal

to the wire surface.

SEM micrograph of a fractured wire surface showing

steplike growth of a central crack.

SEM micrograph of a fractured wire surface showing

fine flat dimples typical of ductile fracture.

128

129

130

43

44

45

46

SEM of a "tag" showing the elongated grain structure. 129

A printout of the ED analysis of a stainless steel wire. 130

xt

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LIST OF TABLES

1

2

3

TABLE SUBJECT

10

Elastic modulus values for as-received stainless steel

wires from tensile tests of 016ss wires (Masson 1969)

Elastic modulus values for as-received stainless steel

wires from tensile tests of ss wires (Twelftree 19741

Elastic modulus values for as-received stainless steel

wires from tensile tests of O1O-O2Oss wires (Sokel

1 984)

Elastic modulus values for as-received stainless steel

wires from tensile and bend tests (Masson 1969)

Slopes of stess-strain curves for as-received stainless

steel wires in arch form

Diameter change of stainless steel wires after

continuous electropolishing

Slopes of stress-stra¡n curves for stainless steel wires

tested in arch form after electropolishing

Elastic modulus values for as-received stainless steel

wires calculated from cantilever bend tests with the

support at 18.5mm

Elastic modulus values for as-received stainless steel

wires calculated from cantilever bend tests with the

support at 20mm

Elastic modulus values for electropolished stainless

steel wires calculated from cantilever bend tests with

the support at 18.5mm

PAGE

69

70

71

74

76

4

5

6

7

78

Diameter change of stainless steel wire after interrupted 80

electropolishing

8

9

81

83

83

11 85

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12

13

14

15

16

17

Elastic modulus values for electropolished stainless

steel wires calculated from cantilever bend tests with

the support at 2Omm

Elastic modulus values for as-received stainless steel

wires from cantilever tests with the support at l Omm

Elastic modulus values for electropolished stainless

steel wires from cantilever tests with the support at

l Omm

Elastic modulus values calculated for annealed and

electropolished stainless steel wires from bend tests

with a support at 2Omm

Mean elastic modulus values calculated for annealed

and electropolished specimens

Elastic modulus values for at and nt wires calculated

from cantilever bend tests with the support at 18.5mm

Elastic modulus values for at, nt and sent wires

calculated from bend tests with the support at 2Omm

Elastic modulus values for nt wires calculated from

bend tests with the support at 1Omm

Elastic modulus values for as-received stainless steel

wires calculated from preliminary resonance tests

Elastic modulus values for electropolished stainless

steel wires calculated from preliminary resonance tests

88

86

89

93

94

Elastic modulus values for stainless steel wires

calculated from three-point bend tests

90

Elastic modulus values calculated for annealed stainless 92

steel wires from bend tests with a support at 2Omm

18

19

20

21

22

23

24

Elastic modulus values for at, bt and nt wires calculated 96

from bend tests with the support at 2Omm

95

95

96

98

99

xrll

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25 Elastic modulus values for nt and sent wires calculated

from resonance tests

100

26 101

27 Elastic modulus values for electropolished stainless

steel wires calculated from resonance tests

102

28 103

29 Elastic modulus values for stainless steel wire

calculated fróm speed of sound tests using the troughs

as reference points

105

30 106

31 Elastic modulus values for annealed stainless steel wire 106

calculated from speed of sound tests using the point of

deviation from the horizontal as the reference point

32 107

33 109

34 The effect of w¡re diameter on elastic modulus values 111

Elastic modulus values for as-received stainless steel

wires calculated from resonance tests

Elastic modulus values for stainless steel wire

calculated from speed of sound tests using the peaks

as reference points

Elastic modulus values for stainless steel wire

calculated from speed of sound tests using the point of

deviation from the horizontal as the reference point

Elastic modulus values for new annealed stainless steel

wire specimen calculated from speed of sound tests

using the point of deviation from the horizontal as the

reference point

A comparison of elastic modulus values derived from

different techniques using load data.

The effect of data modification on the accuracy of the

straight line fit for a sspp ps 018 wire

Effect of data modification on elastic modulus values

for sspp ps 018

35 114

11436

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37

38 Vickers hardness numbers for sspp 018

Average values of diagonal measurements of

microhardness test indentations

115

116

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SUMMARY

ln orthodontics a light, continuous force is thought to be most desirable

as it results in maximum tooth movement and minimum patient

discomfort and damage to the supporting tissues. W¡th an increasingly

large selection of wires on the market, selecting the most appropriate

archwire for a given clinical situation is difficult. Choice may be based on

the feel of the wire, clinical impression or from standard mechanical test

data.

of these, the modulus of elasticity is of primary importance since ¡t

determines the stiffness of an archwire, which in turn governs the force

delivered by an appliance. The elastic modulus of a material has been

thought to be a constant value for a particular material. lt was therefore

surprising, to find such a wide range of elastic modulus values quoted in

the literature.

The principal aim of this study was to evaluate available experimental

techniques for the determination of Young's modulus. Tensile, bend,

resonance and speed of sound tests were performed. Elastic modulus

values were calculated from the data acquired, allowing the different

testing methods to be comPared.

Emphasis was placed on stainless steel wires as fundamental questions

remain, despite their long history of use. ln addition some of the newer

archwires such as nickel-titanium, alpha-titanium and beta-titanium were

tested.

It has been proposed that stiffness appeared to be affected when a wire

was electropolished. For this reason, wires were tested in the as-received

condition and after electropolishing, to ascertain whether elastic modulus

was affected.

Elastic modulus values both in the as-received state and after

electropolishing were lower than the textbook quoted values, and were

difficult to reproduce. Electropolishing did not appear to have a

consistent effect on elastic modulus.

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It was proposed that these heavily drawn wires exhibited anisotropic

behaviour and that this may account for the low elastic modulus values.

Wires were annealed to reduce the anisotropic behaviour prior to testing.

This had a varied effect on elastic modulus with values for some wires

increasing while others decreased.

A wire's surface may be more heavily cold worked than the central

region. Wire specimens were embedded in Bakelite and polished to allow

the maximum wire diameter to be microhardness tested. Microhardness

tests did not detect differences between the surface layer and inner core.

lf a surface difference is present it is very small.

The surface appearance of wires was also assessed in the SEM, in the

as-received state and after electropolishing. As-received wires showed a

very elongated grain structure giving a fibrous appearance typical of a

heavily cold worked structure. The striations were removed with

electropolishing, leaving a smooth surface (apart from occasionäl deep

gouges).

To enable any textural differences between the wire surface and inner

core to be assessed, wires were deliberately maltreated to the point of

fracture. Fractured surfaces were then assessed in the SEM'

It is important to remember that it is the microstructure and in turn the

chemical composition and thermomechanical processing during

manufacture, that determines the mechanical properties of wires. For

these reasonS, assessment of the m¡crostructure in the TEM was

attempted. Specimen preparation proved difficult and no suitable foils

were produced. Ability to assess the microstructure would improve our

understanding of these materials and assist with the development of

more advanced materials.

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SIGNED STATEMENT

This report contains no material which has been accepted for the

award of any other degree or diploma in any university. To the best of

my knowledge and belief, it contains no material previously published or

written by another person, except where due reference is made in the

text of the rePort.

KATHERINE R. ALLEN

lgive consent to this copy of my thesis, when deposited in the UniversityLibrary, being available for photocopying and loan.

xvrll

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ACKNOWLEDGEMENTS

I wish to express my appreciation to:

Dr. J.V. Bee, Senior Lecturer, Department of Mechanical

Engineering, University of Adelaide, for his guidance, patience and

humour

Dr. M. R. Sims, Professor of orthOdontics, Department of

Dentistry, University of Sydney, for his advice

Mr. l. Brown, Department of Mechanical Engineering, for his

technical assistance and suPPort

and lastly my husband Paul Heijkoop who made this Masters

degree possible. He worked full-time in private practice, cared for our

eleven month old daughter Bridget, ran the house and gave advice to a

computer illiterate wife even in the small hours of the morning.

xlx

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CHAPTER 1

INTRODUCTION

orthodontic tooth movement is dependent on remodelling of the

periodontal ligament and alveolar bone. The type of force applied to the

tooth affects the physiological response. Light continuous forces avoid

occluding the blood vessels in the periodontal ligament allowing

continuous and rapid bone removal to occur on the pressure side and

new living tissue to be deposited on the tension side (Sandstedt 19O5'

Storey and Smith 1952, Reitan 1960). This allows maximum tooth

movement to occur with minimum damage to the tooth and investing

tissue (Begg and Kesling 1971).

The physical properties of archwires need to be known to allow a light

continuous force to be applied by the archwire to the teeth. The three

most important characteristics of archwires are thought to be springback,

stiffness and formability. For wires which obey Hooke's law for elastic

bodies, the springback and stiffness can be mathematically determined

(Wilcock 1988).

Orthodontic wires are often classified according to their mechanical

properties. However it is the microstructure which determines these

mechanical properties and this in turn is dependent on the chemical

composition and thermomechanical treatment during manufacture (Bee

1991; Burstone and Goldberg 1980; Twelftree, Cocks and Sims 19771'

Austenitic stainless steels and chromium-cobalt wires have dominated the

market for some years. These wires have similar values for strength,

stiffness and range (Proffit 1986). The similarity of the stress-strain

curves for stainless steel and chromium-cobalt allowed archwire selection

to be made from cross-section alone. An increase in stiffness was

achieved by an increase in cross-section of the wire and this resulted in

the phrase "variable cross-Section orthodontics" (Burstone 1981).

Despite the length of time that stainless steel wires have been used in

orthodontics, fundamental questions remain about their metallurgical and

mechanical properties (Khier, Brantley and Fournelle 1988).

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There has been a large increase in the number of archwires available as a

result of the continuing search for improved materials (Andreason and

Morrow 1978). These include the nickel-titanium, beta-titanium and

alpha-titanium wires. The nickel-titanium wires have gained increasing

popularity since their introduction in 1971. The êlastic modulus is about

half that of stainless steel allowing a much lighter force to be produced

compared with an equivalent sized stainless steel wire. This ability to

vary the stiffness by varying the modulus of elasticity is referred to as

"variable modulus orthodontics" (Burstone 1981 )'

"Appropriate use of the available wire types may enhance patient

comfort, reduce chairside time and the duration of treatment" (Kapila and

Sachdeva 1989). Each archwire available has distinct advantages and

clinical limitations. The overall balance of properties and the specific

clinical application should determine which wire is selected (Burstone and

Goldberg 1980; Kusy 1981). There is no single ideal archwire for all

clinical situations.

To allow the most appropriate archwire to be selected and to enable

improved archwire materials to be developed it is important that there is

good understanding of wire structure and the mechanical properties

which it produces.

2

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CHAPTER 2LITERATURE REVIEW

MECHANICAL PRINCIPLES OF ORTHODONTIC TOOTH MOVEMENT

ldeally orthodontic forces should move teeth rapidly with the least

discomfort to patients and minimal damage to the teeth and the investing

tissues (Begg and Kesling 19711. lt is thought that excessive forces

compress the ligament and occlude the blood supply resulting in necrosis

(sandstedt 1904). No tooth movement will occur until the necrosed

tissue has been removed and new living tissue formed. Large orthodontic

forces cause the teeth to become loose and painful and the resultant

orthodontic tooth movement is intermittent and slow. When only light

forces are applied the blood vessels are not occluded and bone on the

pressure side is cont¡nuously and rapidly resorbed and new living tissue

forms on the negative pressure side. This results in continuor-¿s tooth

movement with minimum discomfort and tooth loosening (Sandstedt

1905, Storey and Smith 1952, Reitan 1960, Rygh et al 1986). From

these viewpoints it would appear that the ideal force system should

create a light continuous force (Proffit 1993).

THE IDEAL ARCHWIRE

The ideal properties of a wire will vary depending on its specific

application. Desirable archwire properties include the ability to resist

occlusal forces, provide a light continuous force over a large

displacement, show zero stress relaxation, minimum friction, good

formability, be easily joined, corrosion resistant, biocompatible and

environmentally stable (Kapila and Sachdeva 1989). Some of these

properties are metallurgically opposing and therefore a compromise needs

to be achieved (Wilcock 1988). lt should also be noted that the bracket

design and slot size create the environment in which the wire functions

and limits the properties and effects of the archwire (schudy 1990).

3

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Of all the properties of archwires the following are generally considered

to be the three most imPortant.

1. Springback. This is the degree that a wire may be deflected without

permanent deformation. The terms springback, maximum elastic

deflection, flexibility and working range have been used interchangeably.

A high springback is desirable because it enables large activations to be

applied. The working time of the appliance is longer and therefore fewer

archwire changes and adiustments will be needed.

2. Stiffness or load deflection. This determines the magnitude of the

force delivered by the appliance. A wire with low stiffness allows a larger

diameter archwire to be used which will f¡ll the bracket slot to give good

tooth control and yet only produce light physiological forces. However

the archwire must have sufficient stiffness to resist undesirable elastic

deformation and plastic deformation during function'

3. Formability. Most appliances require modification at some stage. The

wire should be highly formable so that it may be easily bent and shaped

without fracture. "Ease of forming is best described in terms of practical

experience with representative formative pliers" (Burstone and Goldberg

1980, Hazel and West 1986, Kapila and Sachdeva 1989)'

For wires which obey Hooke's law for elastic bodies, the springback and

stiffness can be calculated from mathematical formulae. Springback is

proportional to the yield stress divided by the elastic modulus and

stiffness is proportional to the elastic modulus (Wilcock 1988). These

physical terms will be described when discussing the mechanical

properties of wires.

TERM¡NOLOGY USED WHEN D¡SCUSSING THE MECHANICAL PROPERTIES OF WIRES

Orthodontic wires can be classified according to their mechanical

properties. tt should be noted that it is the microstructure which

determines mechanical properties. The' microstructure in turn is

dependent on the chemical composition and thermomechanical treatment

during manufacture (Bee 1991; Burstone and Goldberg 1980; Twelftree,

Cocks and Sims 19771.

4

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The following descriptions of terms have been used to describe the

physical properties of a wire (Phillips 1982).

Stress is the force per unit area in a body which resists an external force.

The two forces are equal in magnitude but have opposite directions. So

that stress and external force can be differentiated, external force is

referred to as load.

The type of stress is classified according to ¡ts direction. A tensile stress

is induced by a load which tends to stretch or elongate a body'

Compressive stress occurs when a a load tends to compress or shorten a

body. A stress which resists a twisting or sliding motion is a shear stress.

It should be noted that it is difficult to produce a pure stress. one stress

may be predominant but the other two may be present as well.

Whenever a stress is present there is also deformation or strain which

may be elastic or plastic. Elastic strain is reversible while plastic strain is

permanent. When a wire is stressed past its elastic limit the wire will not

return to its original length when the load is removed. The tft""t at

which this occurs is referred to as the elastic limit of the material' This is

also equal to the yield stress (yield strength).

lf an archwire is loaded in small increments a stress-strain curve can be

plotted. The curve usually starts as a straight line but curves after a

certain stress value is exceeded. The straight line portion of the graph

obeys Hooke's law which states that stress is directly proportional to

strain when the strain is within the elastic limit of the material. The point

at which the curve changes from a straight line is known as the

proportional limit.

The deviation from linearity is often difficult to determine accurately. For

this reason a proof stress value may be more appropriate. Th¡s is defined

as the stress required to produce a specific amount of permanent strain,

usually O.1o/o or O.2o/o. A line with slope equal to Young's modulus (the

elastic modulus) is constructed from the point representing the specified

plastic strain and the magnitude of stress at the point of intersection with

the stress-strain curve is the proof stress.

Elastic limit, proportional limit and proof stress have different definitions

but have nearly the same value and are therefore often used

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interchangeably. These values represent the StreSS above which

permanent deformation occurs. For good formability a low value is

indicated but to resist deformation such as from masticatory forces a

high value is desirable.

The modulus of elast¡c¡ty (E) is calculated from the stress-strain ratio

determined from any point on the linear section of the graph.

F_

elastic modulus

STTESS

strain

This value is indicative of the degree of stiffness or rigidity of the wire

and the magnitude of force delivered by the appliance. A smalJ elastic

modulus value enables a low constant force to be applied and allows a

given force to be applied with greater ease and accuracy (Kapila and

Sachdeva 1989). A wire with a higher modulus of elasticity is more

resistant to deformation (Drake et al 1982t..

Figure 1 (Proffit 1993), outlines the elastic-plastic behaviour of metal on

tensile loading. However the diagram is actually in error since the yield

point and yield strength refer to the O.1o/o ptoo't stress. The yield strength

actually lies at or very close to the proportional limit.

Archwire stiffness will vary depending on the chemical composition,

thermomechanical processing and the cross-section. To minimise

confusion between the wide variety of wires on the market a numbering

system indicating the relative stiffness has been suggested. Stainless

steel being the most commonly used alloy was arbitrarily set at 1.O

(Burstone 1981).

Appliance design will also affect the stiffness (Burstone 1982). In the

clinical situation the archwire sections between the brackets act as

beams. A beam is said to be stiff if it requires a large bending moment to

cause it to flex or distort (Hazel and West 1986). With the advent of

lingual orthodontics for the aesthetically conscious patient, the reduced

o€

E

o

a

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Ultimate Tensile Strength

Yield Stren gt h Failure PointYield Point

(/)Øq)t-

U)

Proportional Limit

E Stif fness ø E

Springiness a 1/E

-------l l- O.l"l"

Strain

Figure 1: The elastic-plastic behaviour of metal on tensile testing.

Diagram from Proffit 1993.

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interbracket distance results in an archwire being stiffer. To compensate

for this, wire dimension and composition may be altered (Moran 1987)'

ln orthodontics there are situations where a large strain or deformation

may be needed with a moderate or slight stress. Wires which fulfil these

criteria are said to be flexible. "The maximal flexibility is described as the

strain which occurs when the material is stressed to its proportional limit"

(Phillips 1982l..

According to standard engineering formulae the flexibility of a solid wire

is expected to decrease as its cross section increases. However, lngram,

Gipe and Smith's research suggested that this was not the case for

Nitinol (Unitek) and they stated that "range appeared to be independent

of wire size". As already stated flexibility appears to be affected by

many factors including wire Size, shape and modulus of elasticity

(lngram, Gipe and Smith 1986). Flexibility may be calculated from the

yield strength to modulus of elasticity ratio.

oy

E

E : maximum flexibility

oy : yield strength

E : elastic modulus

A high flexibility value allows large activation to be applied resulting in

the appliance having a longer working time with the advantage of fewer

adjustments being required (Burstone and Goldberg 198O; Drake et al

1982; Kapila and Sachdeva 1989).

"Resilience can be defined as the amount of energy absorbed by a

structure when it is stressed not to exceed its proportional l¡mit" (Phillips

1g82). lt is often measured ¡n terms of modulus of resilience and this is

equal to the area under the straight-line portion of the stress-strain curve.

This value represents the work available to move teeth (Kapila and

Sachdeva 1989). A high value should result in increased clinical

efficiency by necessitating fewer archwire changes (Drake et al 1982).

The term resilience is frequently associated with springiness.

I

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ln an interview with Kesling, Wilcock stated that the most important

properties of orthodontic wires were flexibility and resiliency (Wilcock

1988). "Resilience and formability are defined as an atea under the

stress-strain curve and a distance along the x-axis respectively (Fig. 2)"

Proffit 1993.

lf the specimen continues to be loaded, a point will be reached where the

wire will fracture. "strength is referred to as the maximum StreSS

required to fracture a structure" (Phillips 1973). Various strengths are

defined according to the type of load. Tensile strength is defined as the

maximum stress it will support in tension, without failure.

Ductility is "the ability of a metal to undergo plastic deformation once the

proportional limit has been exceeded" (Greener, Harcourt and

Lautenschlager 1972). A ductile metal will elongate considerably before

fracturing, while a brittle material would exhibit minimal elongation. A

degree of ductility is required to enable plastic deformation to occur

during archwire formation. "There are three common methods" for its

measurement: percentage elongation after fracture, reduction in the area

at the fractured ends and the number of turns around a mandrel to

fracture (cold bend test)" (Phillips 1982l..

Whenever one body slides over another body, the force that acts to

oppose the movement is called the frictional force. lt has been shown

that friction increases as wire size is increased (Riley, Garrett and Moon

1979). Different frictional resistances of wires may be explained by

differences in the surface smoothness of a wire. lncreased friction is

generally regarded as unfavourable because larger forces are required to

move the teeth (Garner, Allai and Moore 1986).

"surface hardness is the result of the interaction of numerous properties.

These properties may include material strength, proportional limit and

ductility. The relative hardness of a substance may be based upon the

resistance to indentation" (Phillips 1982).

Several investigators have assessed the mechanical properties of various

orthodontic wires (Twelftree, Cocks and Sims 19771 Drake et al 1982;

lngram, Gipe and Smith 1986; Moran 1987; Johnson and Lee 1989;

Kapilla and Sachdeva 1989). The findings from this research work will

be discussed in a later sect¡on on the chemical composition and

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-Yield StrengthProportional Limit-

Strain

E Resilience and formability a¡e defined as'an area

under the stress-strain curve and a distance along the X-axis re-

spectively, as shown here.

Figure 2: A stress-strain curve illustrating the terms resilience and

formability. Diagram from Proffit 1993.

U)U)q)L

U)

- Formability

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mechanical properties of specific wires. There is however very little in the

literature about the mechanical properties of orthodontic wire in relation

to their chemical composition and microstructure despite the close

relationship.

PRODUCTION OF WIRES

Wires are manufactured from cast metals which are drawn through a

ser¡es of dies of decreasing diameter. This process roughens the outside

surface and results in plastic deformation of the metal which is known as

cold working. The crystallization process of molten metals and the

subsequent effect of cold working will be discussed'

THE CRYSTALLIZATION OF MOLTEN METALS

pure metals are rarely used in dentistry because they tend to be tbo soft.

For this reason two or more metals are often mixed to form alloys, with

superior properties. ln the solid state the atoms composing the alloy are

regularly spaced into a configuration known as a space lattice or crystal.

1. The atomic structures are classified according to the fourteen Bravais

lattices in seven crystal systems.

2. There are several possible atomic arrangements. However, metals and

alloys fall into only three of these: body-centred cubic, face-centred cubic

and close-packed hexagonal crystal structures.

3. The form and dimensions of the space lattice are important in

determining the mechanical properties of the metal.

Defects occur in the crystalline structure. The most important defects are

dislocations and their presence affects the ductility of the metal as will be

discussed later.

As a molten metal solidifies a process known as crystallisation occurs.

Crystal growth is initiated at specific sites called nuclei. The number of

nuclei present is determined to some extent by the amount of impurities

present, seeding and the rate of cooling. Nuclei number will therefore

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affect the number of crystals and in turn crystal size. In general the

smaller the grain size the better its mechanical properties.

Often, "the crystals grow as dendrites which are described as three-

dimensional branched network structures emanating from a central

nucleus. Crystal growth continues until all the material has solidified and

all the dendritic crystals are in contact" (McCabe 199O). Each crystal is

known as a grain. The area between the two grains in contact ¡s called

the grain boundary. The grain boundaries are a very small region of

transition, approximately two to three atom diameters in extent, and the

structure is usually highly disordered. lf the metal is highly polished and

then etched appropriately the grain structure is visible microscopically.

After crystallization the grains have approximately the same dimensions

in each direction as measured from a central nucleus. They do not form

to any geometric shape and are said to be equiaxed. A change from this

equiaxed structure to a more elongated, fibrous structure can result in

important changes in mechanical properties (McCabe 19901. Such

changes may be brought about by cold working the alloy below the

recrystallization temperature which produces work/strain hardening.

Examples of this occur in wire fabrication and the bending of wires or

clasps.

THE EFFECTS OF COLD WORKING AND ANNEALING ON THE CRYSTAL STRUCTURE

Wires are said to have a wrought structure as a result of the cold

working procedure. This results in wires having different properties to

those of cast metals. They become harder and stronger with a higher

elastic limit value and have decreased ductility.

The drawing of a wire from castings is an example of plastic deformation.

As plastic deformation begins, the dislocations present within the grains

move along a slip plane until another defect (dislocation or foreign atom)

is reached. The resultant interactions reduce the mobility of the

dislocations and higher stresses are needed to continue deformation. This

explains the phenomenon of work hardening. lf dislocations reach a grain

boundary, they "pile up". This is due to the fact that the slip planes in

t2

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adjacent grains are not aligned due to the¡r different lattice orientations.

Again higher stresses must be provided to continue plastic deformation.

The effect of crystal size on the mechanical properties is now

comprehendable. As crystal size decreases the concentrat¡on of grain

boundaries increases and consequently the resistance to dislocation

movement increases. Thus materials with a finer grain structure are

harder and have a higher elastic limit (McCabe 1990).

Cold worked metals can be converted back to an equiaxed structure by

heating the structure above the recrystallization temperature. This is

known as a softening heat treatment. The metal reverts to its

undeformed condition, which is softer with a lower elastic limit and has a

higher ductility. ln some cases these changes in mechanical properties

are undesirable and so heat treatment should be avoided. Heat treatment

below the recrystallization temperature is referred to as stress relief

annealing. lt allows the internal stresses to be relieved without affecting

the mechanical properties, since the deformed structure is not- altered

significantly.

HISTORY OF ORTHODONTIC WIRES

precious metal alloys were predominantly used for orthodontic purposes

prior to the 1930's. At this time gold alloys were the only material

available that would tolerate the intraoral conditions. lts physical

properties were only marginal and it was obsolete even before the price

increase in the 1970's (Proffit 1986).

Historically stainless steel (Wilcock) and chromium-cobalt (Elgiloy) have

been the dominant orthodontic wires because of their desirable physical

characteristics. Austenitic stainless steel was introduced in 1929.

Stainless steel w¡res possess excellent formability, have good corrosion

resistance, high values of stiffness and resilience, are environmentally

stable and are of moderate cost (Drake 1982; Burstone and Goldberg

1980; Hazel, Sokel and West 1984). Chromium-cobalt (Elgiloy) wires

have similar strength, stiffness and range properties (Proffit 1 986).

Despite the long history of use of stainless steel wires in orthodontics

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fundamental questions still remain regarding their metallurgical and

mechanical properties (Khier, Brantley and Fournelle 1988).

As a result of a continuing search for improved performance there has

been a large increase in the number of archwire materials available

(Andreason and Morrow 1978). These include the nickel-titanium, beta

titanium and (near) alpha titanium wires. Since the introduction of nickel-

titanium wires in 1g71 they have gained increasing popularity. Some

possess unique properties of superelasticity and shape memory which

will be described later (Hurst et al 1990). Beta titanium has a unique

balance of low stiffness, high springback, formability and weldability

(Burstone and Goldberg 1980). A near alpha titanium is also on the

market. properties of titanium wires will be discussed in detail in sections

5,6 and 7.

The increase in new alloys and wire fabrication techniques has made

archwire selection much more difficult. ln the past owing to the similarity

of stainless steel and chromium-cobalt Stress-strain curves, archwire

selection was made almost exclusively on cross-section alone. lncreases

in wire stiffness were achieved by progressively increasing the cross-

section of the wire. This resulted in the phrase "variable cross sect¡on

orthodontics". Now the archwire stiffness can be varied by varying the

modulus of elasticity and this is referred to as "variable modulus

orthodontics" (Burstone 1981; Combe et al 1985). ln the latter technique

the cross sectional shape, alloy content and heat treatment of the

archwire needs to be assessed (Johnson and Lee 1989).

As a result of these advances "the play between the wire and the

attachment is not dictated by the stiffness required but is under full

control of the operator" (Burstone 1981). The low elastic modulus newer

alloy archwires allow light rectangular wires to be placed even during

early stages of treatment. This results in better tooth control and

decreases the number of archwire changes.

Each archwire on the market has distinct advantages and clinical

limitations. The overall balance of properties and the specific clinical

application should determine which wire is selected (Burstone and

Goldberg 1980; Kusy 1981). "Appropriate use of all the available wire

types may enhance patient comfort and reduce chairside time and the

duration of treatment (Kapila and Sachdeva 1989)."

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THE CHEMICAL COMPOSITION AND MECHANICAL PROPERTIES OF SPECIFIC W¡RES

1. cor-o

pure gold was too soft for most dental purposes so alloys similar to that

of Type lV castings were used for wires, A typical alloy contained 60%"

gold, 15% silver, 15o/o copper and about 1Oo/o platinum or palladium' The

platinum or palladium content raises the melting point and

recrystallization temperature of the wires making them more suitable for

soldering. Gold alloy wires have a lower modulus of elasticity than

stainless steel and therefore apply lower forces (McCabe 1990)' Gold

tolerates the intraoral conditions well. ln general though their physical

properties are only marginal and with the advent of other alloys they

have become obsolescent. Only the Crozat appliance is still occasionally

made from gold (Proffit 1993)'

2. srnlruless steel

There are three major forms of stainless steel - ferritic, martensitic and

austenitic and there is wide variation in their respective compositions and

properties (Phillips 19821. There are also grades which contain two co-

existing phases (ferrite-martensite, or ferrite-austenite) which are termed

dual-phase or duplex stainless steels.

The typical stainless steel orthodontic wire is referred to as 18/8

austenitic stainless steel. The term 18/8 refers to the composition - 18%

chromium and 8o/o nickel. The high chromium content results in good

resistance to corrosion (Proffit 1993). The addition of nickel makes the

austenite-martensite transformation sluggish and lowers the martensitic

transformation Start temperature below room temperature So that no

hardening heat treatments are possible (Greener, Harcourt and

Lautenschlager 1972). lt should be noted that some individuals are

sensitive to nickel and chromium (Kapila and Sachdeva 1989)'

lnvestigations have shown that nominally austenitic sta¡nless steel wires

may not be entirely austenitic. Whether a stainless steel wire is a single

phase austenitic (face centred cubic) structure or a duplex austenitic and

martensitic (body centred cubic) structure is strongly dependent on the

15

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alloy composition and wire manufacturing processes (Khier, Brantley and

Fournelle 1988). The austenitic stainless steel structure is metastable and

can decompose to the martensitic phase under certain conditions such as

proprietary cold working and intermediate heat treatment associated with

wire manufacture (Khier, Brantley and Fournelle 1988; Phillips 1982)' ln

fact, austenite can be metastable with respect to deformation and it is

this which produces martensite in different orthodontic wires (Singh

1991).

By varying the amount of cold working and annealing during manufacture

the properties of stainless steel wire can be altered. lt may be softened

by annealing and hardened by cold working (Phillips 1982l'. A range of

stainless steel archwire materials in partially annealed states are

available. They are categorised according to their ductility for example

soft, half-hard and hard. Fully annealed stainless steel is quite soft and

highly formable. Ligature wire which is used to tie an archwire into the

bracket is an example of "dead soft" wire. As the amount of annealing is

increased formability is progressively enhanced at the expense of

decreased yield strength. The steel wires with the highest yield strength

are brittle and break when bent sharPly (Proffit 1993).

ln Adelaide the commonly used stainless steel wires are produced by

A.J. Wilcock at Whittlesea, Victoria, Australia. They ate available in

several different grades - Special, Special plus, Premium, Premium plus

and Supreme. These wires are made from an 18/8 austenitic stainless

steel. Their properties are varied by the thermomechanical treatment

during manufacture.

Khier, Brantley and Fournelle (1988) investigated the structure and

mechanical properties of as-received and heat-treated stainless steel

orthodontic wires. Two different proprietary brands of stainless steel

were selected (Tru-Chrome and Permachrome). Selected specimens were

heat treated in air at 7OO", 900" and 1 100' for a period of ten minutes

followed by air cooling to room temperature. X-ray diffraction patterns

showed that both brands of the as-received wires consisted of a two-

phase structure. This two-phase structure was converted to austenite

with heat treatment for Tru-Chrome but persisted in Permachrome. The

modulus of elasticity in tension was significantly lower in the latter wires

when compared with the annealed austenitic sta¡nless steels. This can be

16

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attr¡buted to phase transformation and the development of considerable

residual Stress in the heavily cold-worked structure. This is in agreement

with findings from Goldberg, Vanderby and Burstone 1977, Asgharnia

and Brantley 1986, PhilliPs 1982.

When a stainless steel wire is ptastically deformed dislocations pile up

and accumulate at various microstructural obstacles. When the load is

removed the dislocation lines will not move appreciably because the

structure is stable (Orowan 1959). lf the direction of loading is reversed

some dislocation lines can move a considerable distance at a low shear

stress because the barriers behind are not as strong and closely spaced.

As a consequence initial yield will occur with a smaller load. lf a load is

applied in the same direction as the original load there is increased

resistance to plastic deformation. This phenomena is referred to as the

Bauschinger effect.

The reduction in proof Stress and Young's modulus and increased

elongation noted when the direction of deformation is reversed mpy have

the following clinical effects. These include:

i. The amount of stored energy is reduced and therefore there is less

energy to move teeth.

ii. The maximum force that can be applied before the wire is plastically

deformed is reduced.

iii. The lower stress:strain ratio reduces the rate of change of force

magnitude, that is the force level remains more constant over a given

distance.

iv. The wire has increased ductility and is therefore more formable'

To gain the best elastic properties from the wire it should be activated in

the same direction as the original curvature in the wire although this is

not always possible (Gullotta, West and Hazel 1987)'

Stress relief anneals may be carried out after bending to reduce internal

stresses and enhance the elastic properties. Stress relief anneals involve

heating the wire to 450"C for about ten minutes. This can only be done

to stabilised stainless steel wires where small quantities of titanium (or

niobium) have been added. Titanium is added to the alloy to prec¡pitate

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as a carbide in preference to chromium, so that chromium is retained in

solid solution (Phillips 1982).

A study assessing the effects of stress relief generally showed an

increased resilience which was reflected in increased stiffness and range.

This results in a higher initial force magnitude for a given activation level

(Lane and Nikolai 198O). The use of smaller diameter wires enables lower

forces to be applied but this results in poorer bracket fit and

consequently less control of tooth movements. The force produced is

higher than nickel-titanium and beta-titanium but dissipates faster than

either (Kapila and Sachdeva 1989). lt exhibits low friction - less than

Nitinol and beta-titanium (Garner, Allai and Moore 1986).

In Stage I of the Begg technique, traditionally Wilcock O.016" stainless

steel archwire is used. Recently, as a result of more flexible archwires

becoming available, archwires such as O.O16" Japanese NiT¡, O.O16"

Nitinol and O.O1O" Supreme Wilcock wire are being used in Stage l. This

has been shown to considerably decrease the time for initial alignment

(Lew 1988).

Supreme grade stainless steel wire (ultra high tensile) has a flexibility

similar to that of beta-titanium but has nearly three times the resilience. lt

is not as flexible as nickel-titanium but the nickel-titanium flexibility is

probably not fully utilised orthodontically. lt has good formability and the

resiliency of nickel-titanium can be achieved by engineering the yield

stress and diameter (Wilcock 1988).

Stainless steel wires can be joined by soldering or welding but the

technique is demanding (Kapila and Sachdeva 1989). Care must be taken

to avoid overheating as it may cause recrystallization and reduce the

springiness of the wire. ln unstabilised wires it may cause chromium to

react with carbon to form carbides. This phenomena is referred to as

weld decay and results in a loss of corrosion resistance at the soldered

joint and the introduction of a degree of brittleness. To decrease the

potential for this silver solders are used because they contain silver and

copper with small quantities of other elements which lower the fusion

temperature.

Welding is accomplished by passing an electric current through two

pieces of wire held together between two electrodes. Sufficient current

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needs to be used to melt the wires at the point of contact (McCabe

1990).

The corrosion of stainless steel orthodontic wires has been investigated

in the "as received" condition, after forming and after heat treatment in a

hot air oven at 4OO"C for ten minutes. Corrosion rate varied depending

on the strain history. Heat treatment permitted a degree of stress relief

without carbide formation and reduced the corrosion rate of the formed

wires in relation to the "as-received" wires (Toms 1988).

3. MULTIBRAIoED srAlNLEss srEEL

These wires consist of specified numbers of thin stainless steel wire

sections coiled around each other to provide a round or rectangular cross

section. These wires have a high springback, low stiffness, high stored

energy but poor formability. They are biocompatible and environmentally

stable and may be joined by soldering or welding. Little is knowñ about

their friction (Kusy and Dilley 1984).

ldeally the initial archwire should have a great range to enable malaligned

teeth to be accommodated, have low stiffness so that the forces applied

are gentle and have high strength so that it is not easily deformed with

masticatory forces. Historically, looped archwires were formed to

increase the flexibility and reduce the force (Begg and Kesling 197U.

Disadvantages included the increased time required to bend the archwire,

they were mechanically disadvantageous (resulting in bite closure and

excessive incisor proclination) and were difficult to keep clean. An

alternative was the use of multistranded stainless steel wires which have

the flexibility of small diameter wires but the strength of many strands.

Titanium alloys are a third alternative but are more expensive (Kusy and

Stevens 1987).

It has been noted that multistranded stainless steel wires have a similar

springback to nitinol but a larger springback when compared to solid

stainless steel wires or beta-titanium wires. The springback of

multistranded stainless steel and titanium wires is relatively independent

of wire size and therefore does not obey the engineering principal that

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spr¡ngback decreases with increasing thickness (lngram, Gipe and Smith

1986).

Four triple-stranded stainless steel wire products were tested in one

investigation: Twist (American Orthodontics), Wildcat (GAC

tnternational), spiral (ormco) and Hi-T TwistFlex (unitek). The four

different wire diameters tested were 0.0150", 0.0175", 0.0195" and

O.0215". Force storage and delivery properties were determined and

compared with reported values for titanium alloy archwires' Except for

Spiral (Ormco) wire all of the O.O15" multistranded wires demonstrated a

greater working range than Nitinol or TMA. All of the 0.O15" triple

stranded wires were unmatched for application of light forces over a long

distance. Excluding Hi-T TwistFlex (Unitek) the titanium wires are

stronger. The elastic property ratios of triple stranded wires varied widely

and compared favourably with some of the titanium wires offering a

cheaper viable alternative (Kusy and Stevens 1987).

A study comparing 43 patients with either a 0.O15" multistranded

stainless steel or a O.O14" superelastic nickel-titanium initial aligning

archwire showed no statistically significant difference in the amount of

incisor alignment over the mean time interval of five weeks. These results

support the conclusions of Kapilla and Sachdeva (1 989) that a

multistranded stainless steel wire may be a less expensive alternative to

the nickel-titanium wires for initial alignment and levelling (Jones,

Staniford and Chan 199O).

4. cxRorvllurv¡-cosRLr

Chromium-cobalt alloys were originally developed for use as watch

springs but their properties are also excellent for orthodontic purposes

(Phillips 1982). These alloys contain approximatelY 7Oo/" cobalt and 30%

chromium however some cobalt can be replaced by nickel. The carbon

content is never above O.15o/". The distribution and size of the carbide

precipitates within the matrix may determine the hardness and brittleness

of the material. Alloys with lower carbon content are softer (Greener,

Harcourt and Lautenschlager 1972l..

20

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These wires are unique in that they are supplied in a softened state' This

is achieved by heat treating the wires between 1 1OO' and 12OO'C and

then quenching them. As a result the wires have excellent ductility and

are easily formed.

They can be hardened after bending by "age-hardening" at temperatures

between 2600 and 6SOoC (Phillips 1982). This results in the formation of

precipitates which produce the required springback and resilience

properties (Burstone and Goldberg 198O).

Hardness, yield and tensile strength and the modulus of elasticity are

similar to those of austenitic stainless steel (Hazel, Sokel and West 19841

proffit 1gg3). The high modulus of elasticity enables them to deliver

twice the force of beta-titanium and four times that of Nitinol.

They are difficult to join by soldering and care must be taken to avoid

overheating as this can result in annealing with loss of yield strength

(McCabe lggo). Tarnish and corrosion resistance is excellent -(Phillips

1g82). Their advantages over stainless steel include greater resistance to

fatigue and distortion and longer function as a resilient spring. Frictional

forces are comparable to stainless steel (Kapila and Sachdeva 1989)'

Elgiloy (Rocky Mountain Co.) is an example of a chromium-cobalt

orthodontic wire. lts nominal composition is cobalt 4Oo/o, chromium 2Oo/o,

iron 160/o, nickel 15o/o, molybdenum 7o/o and manganese 2% (Elgiloy,

Rocky Mountain Orthodontics Brochure, Denver, Colorado, 1977!.. These

wires are available in several cross-sectional shapes and dimensions.

There are four grades of Elgiloy - red, green, yellow and blue. Each grade

represents different degrees of cold work.

5. ru¡cret-rltRrulun¡

Nickel-titanium was the first of the titanium alloy wires and was marketed

as "Nitinolrnr" (Unitek Corp.) in the late 1970's. "NitinolrM" was initially

developed for the space programme but has proved very useful in clinical

orthodontics. lts name was derived from its metal composition Ni - nickel

and Ti - titanium and the place of origin NoL - Naval ordinance

Laboratory (Proffit 1993).

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These alloys contain almost equal amounts of nickel and titanium with

small quant¡ties of other metals. At high temperatures (880'C), the

crystal structure is austenitic (body centred cubic) beta phase, and at

lower temperatures a martensitic transformation to a (close packed

hexagonal) alpha phase can be produced (Buehler and Cross 1969). The

change in crystal structure alters the mechanical properties. The material

is ductile and may be plastically deformed in the alpha phase (Andreason,

Wass and Chan 1985). ln the beta phase it is difficult to induce

deformation (Miura et al 1986).

The temperature range over which the change in crystalline structure

occurS is referred to as the transition temperature range (TTR)' The

specific TTR is dependent on the chemical composition of the alloy and

its processing history. TTR can be changed by altering the proportion of

nickel to titanium or by substituting cobalt for nickel (Buehler and Cross

1 969).

Nickel-titanium has outstanding elasticity and can almost be bent back on

itself without being plastically deformed. This characteristic offers real

advantages in enabling clinicians to engage an archwire into malposed

teeth (Andreason and Morrow 1978). Studies have shown that nickel-

titanium wires have superior springback characteristics to stainless steel

and beta-titanium (Hudgins, Bagby and Erikson 199O), "Nitinol exhibited

5o/o-55o/o greater working range than single or multistranded stainless

steel wires, depending on the deflection, interbracket distance and wire

(Andreason and Barret 1970)."

Hudgins, Bagby and Erikson's study aimed to quantify the amount of

permanent deformation after deflection of nickel-titanium wire over

different time intervals of one, fourteen and twenty eight days. The

majority of the wires exhibited more deformation at the later time

intervals, especially twenty eight days, suggesting that deformation may

be a function of time (Hudgins, Bagby and Erikson 1990)'

The elastic modulus of nickel-titanium is about half that of stainless steel.

Clinically this means that nickel-titanium wires will produce a lighter force

than an equivalent sized stainless steel wire, The low elastic modulus but

moderately high strength results in nickel-titanium having high resilience.

The stored energy of nitinol is much larger than stainless steel

(Andreason and Morrow 1978).

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The outstanding elasticity and low elastic modulus allow large dimension

wires (which nearly fill the bracket), to be used without the risk of

deforming during bracket engagement or exerting too great a force at an

early treatment stage. This decreases the number of archwire changes

and keeps chairside time to a minimum. Treatment time to derotate and

level teeth is shortened and patient discomfort lessened (Andreason and

Morrow 19781 Lew 1988; Chen 1990). These properties make nickel-

titanium favourable as a starting and intermediate wire (Kusy 1981)'

The nickel-titanium wires initially available for orthodontic use were in the

stabilised martensitic form at room temperature. These wires possess

excellent springback, but shape memory and superelasticity are poor due

to manufacture by a work hardening process (Miura et al 1986).

"Titanal" (Lancer Pacific), is a newer martensitic nickel-titanium alloy. lt

has very similar strength and spring characteristics to the early nickel-

titanium wires but has the advantage of being highly formable (Proffit

1993).

ln the late 1980's nickel-titanium wires with a primarily austenitic grain

structure became available. Like the original nickel-titanium wires they

exhibited low stiffness and high springback. ln addition they

demonstrated superelasticity and/or shape memory (chen 199o)' A three

point bending test was designed to differentiate between wires with and

without superelasticitY.

Shape memory is described as the ability of a wire to return to its

previously manufactured shape when it is heated through its transitional

temperature range (Andreason, Wass and Chan 1985). This change can

be metallurgically explained by a stress-induced martensitic change. This

is a partial transition in structure from an austenitic to martensitic form.

The shape memory effect is brought about by a high temperature heat

treatment which alters the crystal structure of the alloy. The nitinol wire

must be held in the desired shape at a temperature between 23O"-260"C

for 1O minutes (Andreason 1980). This allows the archw¡re to be formed

in the laboratory ahead of time, saving chairside time and making it more

accurate (Miura, Mogi and Okamoto 1990). Providing the wire is

deformed at temperatures beneath the TTR, the original shape can be

recovered by heating it through its unique temperature trans¡tion range.

For clinical purposes the TTR should be sufficiently high to avoid a return

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to the original shape at room or oral temperature (Andreason and Morrow

1978; Hurst et al 199O).

ln contrast to other metals where deformation is predominantly induced

by lattice slip, with nickel-titanium it is obtained by martensitic

transformation. To obtain maximum shape recovery the amount of plastic

deformation should be limited to 7-8o/o of the original length. This enables

the process to be repeated many times. The change from the distorted to

the original form involves a transformation of nickel-titanium from the

martensitic to the austen¡tic phase (Andreasen and Brady 1972l..

The shape memory effect has been quantitatively analysed. Maximum

shape memory was determined by calculation of the amount of recovery

that occurred. The mean percentage recovery ranged from 89 to 94o/" for

N¡-Ti, Nitinol, Orthonol, Titanol, Sentinol Light and Sentinol Medium.

Sentinol Heavy wire showed a mean recovery of approximately 41o/o

(Hurst et al 199O). This is in contrast to earlier findings by Buehler and

Cross, and Andreason and Brady, where it was suggested that shape

recovery was usually 1OOY" (Buehler and Cross 1969; Andreason and

Brady 1972l,.

This temperature transition or shape memory potential of nickel-titanium

wires is not fully understood or utilised in orthodontics at this stage but it

is an area that warrants further investigation (Andreason, Wass and Chan

1985; McCabe 199O).

"Nitinol" has a lower elastic modulus and can be deformed almost five

times more than stainless steel but the stress-strain curve is similar to

that of StainleSS steel and chromium-cobalt. "Japanese NiTi" wire

produces a totally different cUrve. When Stretched Up to 2o/o, sLress and

strain are almost proportional, but additional strain is accumulated at

constant stress. lnit¡ally the curve appears to be similar to that shown

when plastic deformation occurs. However on unloading the specimen

the stress and strain values are almost proportional followed by a period

where the stress remained constant despite a decrease in the strain. This

phenomena is known as superelasticity (Miura et al 1986). Clinically this

means that the archwire can be deflected a small or large distance and

yet exert the same force (Chen 1990).

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Superelastic nickel-titanium wires are unusual in that the unloading curve

differs from its loading curve (F¡g. 31. This may be interpreted as the

force needed to activate the wire is not the same as the force that the

wire delivers (Proffit 1993).

Several factors affect the force level of superelastic nickel-titanium wires.

These include the heat treatment conditions, the processing method, and

most importantly, the constituent ratio of the alloy. Heat treatment and

reduction of the nickel content reduce the forces produced by the wire.

Wire size and the amount of deflection do not affect the superelastic

force (Miura, Mogi and Okamoto 1990).

The bending properties of superelastic (Nitinol SE, Sentinol and NiTi) and

non-superelastic (Nitinol, Titanol and Orthonol) wires have been assessed

in the as-receíved condition and after heat treatment at 5OO and 6OO"C.

Permanent deformation for the superelastic wires after unloading from

80'activation were 1O-15" and about twice this for the non-superelastic

wires. A superelastic region of nearly constant bending moment was

noted in the round wires but was less evident in rectangular wires. The

slopes of the non-linear bending plots were considerably less for the

superelastic wires. Heat treatment only produced small changes in the

bending plots for the non-superelastic but considerable response for the

superelastic wires. The maximum amount of activation and deactivation

decreased with heat treatment. Heat treatment at 6OOoC for 1O minutes

resulted in complete loss of the superelastic properties (Khier, Brantley

and Fournelle 1991).

Nickel-titanium wires have limited ductility and are therefore not easy to

bend without fracturing (McCabe 1990). They cannot be bent with sharp

cornered instruments and bending adversely affects springback. ln

addition they cannot be soldered or successfully welded without being

annealed (Andreason and Morrow 1978). These properties limit the

usefulness of the wire (Kusy 1981).

These wires have more surface roughness than stainless steel which may

be significant to corrosion and friction (Garner, Allai and Moore 1986).

The numerous surface irregularities could predispose the wire tocorrosive attack in the mouth (Harris, Newman and Nicholson 1988). The

corrosion resistance findings are inconsistent. According to some studies,

their frictional resistance is higher than stainless steel but |ower than

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EEË(')

c(l,

Eo

=o)ctc(l)@

2000

1 500

1

50

Stainless Steel

20 40 60

Deflection (degrees)

80

Figure 3: Stress-stra¡n curves for a range of orthodontic wires: stainless

steel, Nitinol (martensit¡c NiTi) and NiTi (austen¡t¡c N¡T¡). (Proffit 1993)

0

Nitinol

NiT¡

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beta-titanium (Garner, Allai and Moore 1986; Kapila and Sachdeva

1989).

Nickel-titanium wires are costly and as a result some clinicians are

reusing them. This necessitates the wires being sterilised and being

subjected to repeated mechanical stress. No appreciable loss in physical

properties has been noted after repeated cycles of sterilising/disinfection

(Buckthal and Kusy 1988; Mayhew and Kusy 1988). The loss of elastic

deformability may be the limiting factor in the number of times that the

wire may be reused (Harris, Newman and Nicholson 1988).

6. BETA-TtrANtuM

Unalloyed titanium has two allotropic forms - a low temperature

hexagonal close packed, alpha, and a high temperature (above 88O"C)

body centred cubic, beta, structure. Additions of certain elements such

aS iron, molybdenum, vanadium and chromium stabilise the beta phase

and when in sufficient amounts allows the beta to be present at room

temperature. Other additions such as tin and zirconium suppress the

formation of an embrittling omega phase in beta (Burstone and Goldberg

1980; Wilson and Goldberg 1987).

Beta titanium dental alloys consist of titanium with additions of

molybdenum which stabilises the body centred cubic phase even when

cooled to room temperature' Beta-titanium is marketed as TMA (titanium

molybdenum alloy) (Ormco/Sybron) (Wilcock 1 988). Unlike nickel-

titanium, beta-titanium was developed primarily for orthodontic use

(Proffit 1993).

The extent of deformation and the number of passes used to draw the

wire affects the properties. With increased deformation the tensile

strength increases but the elastic modulus remains unchanged. Lower

reductions per pass improve elongation and yield strength (Shastry,

Elinson and Goldberg 1982).

These wires offer a desirable combination of strength (greater than

stainless steel) and springiness and are reasonably ductile and therefore

formable (Kusy 1981). Formability is similar to stainless steel although it

cannot be bent over as sharp a radius (Wilson and Goldberg 1987).

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The modulus of elasticity value is less than half that of stainless steel

but is twice that of nitinol. This enables these wires to impart a low force

per unit of activation. Springback is superior to stainless steel permitting

beta-titanium wires to be deflected over long distances without

permanent deformation. This allows the wire to have a greater range of

action (Burstone and Goldberg 1980). The flexibility of beta titanium

wires is much less than nickel-titanium wires (Kusy 1981).

Beta-titanium can be joined by welding alone without reinforcement

solder. The welding must be done within a narrow optimal voltage setting

to avoid affecting the wire properties. Overheating could result in the

wire becoming brittle (McCabe 199O). Corrosion resistance is similar to

stainless steel and chromium-cobalt wires. Friction levels are higher than

stainless steel, chromium-cobalt and Nitinol (Garner, Allai and Moore

1 986).

The properties of beta-titanium are intermediate between stainless steel

and martensitic nickel-titanium (Proffit 1993). These characteristics make

it suitable for an intermediate and finishing wire (Kusy 1981)'

Some of the titanium alloys are amenable to thermomechanical

processing to produce alpha plus beta structures. The presence of the

alpha phase improves the tensile ductility in comparison to when only the

beta phase is present but the fracture toughness is inferior. The proof

stresses for both structures are similar (Cornet, Mille and Muster 1982l-.

7. ALPHA-TITANIUM

This new alloy wire is titanium-based and contains aluminium and

vanadium. ln equilibrium at room temperature it has a close-packed

hexagonal crystal structure termed alpha-titanium, lt is slow to form from

the high temperature body-centred cubic phase. There is some retention

of the beta phase at room temperature and due to this it is usually

referred to as a near-alpha alloy. The fewer slip planes in the hexagonal

lattice render it less ductile (Wilcock 1988).

Alpha-titanium wire has similar tensile properties (proof stress and elastic

modulus) to gold. The elastic deflection or springback is similar to high

tensile stainless steel. This allows the wire to be activated more than

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stainless steel wires, without problems of permanent deformation or an

excessive force being produced. lts properties lie between the low moduli

nickel-titanium wires and beta titanium and the high moduli stainless steel

and chromium-cobalt.

The formability of the wire is affected by the surface finish. Poor surface

finish or surface cracks in the wire decrease the formability. Alpha-

titanium wire is corrosion resistant and much harder than beta-titanium

alloy wires (Hazel, Sokel and West 1984).

SUMMARY

As stated in the literature there is a lack of knowledge about the

metallurgícal and mechanical properties of stainless steel orthodontic

wires despite their long history of use. The use of wires is determined by

their mechanical properties. Particularly important is the elastic modulus

as this determines the stiffness and resilience of a wire.

The elastic modulus values measured for orthodontic wires have

generally been lower than the standard values quoted in metallurgical

references for bulk materials. ln addition there is large disagreement in

absolute values between authors.

A study is therefore warranted on the determination, accuracy and

reproducibility of Young's modulus in commonly used mechanical tests.

Results from these studies should then be compared with values obtained

using more sophisticated mechanical and physical test methods.

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CHAPTER 3AIMS OF THE INVESTIGATION

In the literature survey, it was noted that there was disagreement in

elastic modulus values for orthodontic wires. Most of the elastic modulus

values were determined from tensile and bend tests and these values did

not agree with bulk metallurgical values. For these reasons it was

decided to look at different methods of measuring the elastic modulus

and to check the reproducibility of the results. Current orthodontic wires,

including stainless steel, nickel-titanium, alpha-titanium and beta-titanium,

were assessed.

Knowledge of mechanical properties of as-received wires would

complement observations by Singh 1991 on microstructure. Some wires

were also assessed after being electropolished. This was prompted by a

comment made by an experienced clinician that wire stiffness appeared

to change after electropolishing.

1. Mechanical property data was acquired using

a. Simple tensile test using a 1O tonne Instron universal testing machine

b. Bend tests

Three different bend tests were used in order to compare the load-

deflection behaviour and the elastic modulus values obtained. The tests

are as l¡sted below:

(1) wires in arch form(2) a conventional cantilever bend geometry

(3) three point bend sYstem.

The properties of the wires were determined in both the as-received

condition and after manipulative treatments such as electropolishing

and/or heat treatment.

c. Resonance tests.

d. Measurement of speed of sound along a length of wire.

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e. Microhardness / Macrohardness tests

2. Etfect of electropolishing on surface structure

The surface structure of wires in the as-received state and after different

times of electropolishing was assessed in the SEM.

3. Fracture behaviour

Orthodontic wires are heavily cold worked with most deformation in the

surface layers. As-received wires were deliberately cold-worked to the

point of fracture and then assessed in the scanning electron microscope

to assess the extent of the heavily distorted surface layer and the

distribution of deformation through the wire cross-section.

Electropolished specimens were also assessed, to determine if the heavily

cold worked surface layer was removed.

4. Another objective was to study the detailed microstructural data in

transverse and longitudinal sections of specified wires using transmission

electron microscopy. Fine scale features such as grain size, dislocation

density, and second phase size, shape and distribution were to be

assessed.

No-one other than Singh 1991

orthodontic wires. Comparison

between different studies and

therefore probably meaningless.

has looked at the m¡crostructure of

of mechanical property data results

especially different sized wires are

The more a wire is drawn, the more cold worked ¡t is, the finer the

effective grain size and consequently the higher the strength. To

understand any differences in wire properties we must know if the

structure is different.

3T

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CHAPTER 4MATERIALS AND METHOD

The materials studied included orthodontic wires of (1) stainless steel

(special plus, premium, premium plus, supreme and pulse straightened

grades), (2) nickel titanium and (3) superelastic nickel-titaniumr.

1. a. Conventional tensile tests using a universal lnstron testing

instrument (model 8501 ), 1OOkN load cell, in conjunction with an

extensometer, with a cross head speed of 0.5mm per minute to comply

with the Australian standard 1964-1977 (Fig. 41. The stainless steel

wires assessed were as listed below2.

i. sssp

ii. sspp

iii sss

o1 6, 01 8, O20, O22

o12, O14, 016, 018

010

Approximately 24Omm lengths of wire were attached to aluminium

casings before entering the lnstron grips which were spaced

approximately 2OOmm apart (F¡g. 5). This overcame the problem of the

wires failing prematurely at the point of grip. The wires were loaded until

fracture.

b. Bend tests. Three different bend tests were compared to obtain

information on the load deflection behaviour : wire in arch form, a

cantilever bend geometry and a three point bend system.

Testing apparatus

The testing apparatus consisted of:

A milled brass wire holder held in a stand which allowed adjustments to

be made in the vertical plane, using a micrometer drive (calibrated in

lThe material/condition abbreviated identifications are given in the forward p' (vi).

2Although Sl units should be used in scientific studies the nomenclature 018 = 0.018"

(0.45mm) is used for identification since most orthodontic wires are supplied in imperial

units and will be familiar to practitioners.

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I

Figure 4: A photograph of a universal Instron testing instrument with an

extensometer in Position.

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Figure 5: A photograph illustrating a stainless steel wire wrapped around

an aluminium casing.

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ímperial units) (Fig. 6). Slots in the wire holder enabled the wires to bepositively located. When the wires were tested in archform the distancebetween the distal ends when placed in the slots was 7Omm.

A milled steel holder was glued to the scale (Mettler 6100) pan. Theanterior section of the archwire was placed into a groove in the steelholder. In the cantilever tests the wire was either supported in a slot (Fig.

7l or knife edge while the three point bend test specimens weresupported on two knife edges 25mm apart.

Vertical movement of the brass holder would then apply a load on thesupported anter¡or segment of the wire which could be recorded on theMettler scale.

Tests performed

The wires were loaded in increments of ten thousandths of an ínch(O.25mm) and the load reading recorded in grammes to two. decimalplaces. The wire was then unloaded in ten thousandths of an inchincrements and readings recorded.

Some archwires were then electropolished where indicated and the testrepeated.

(1.) Arch wire preoaration

Plain archwires without circles were formed with anchor bends of varyingsizes, from 140mm lengths of ss wire of nominated diameter. 1O

millimetre lengths of steel tube were glued to each end of the wire wíthSelleys five minute Araldite (epoxy adhesive). This allowed the wire to be

reproducibly located in the apparatus used to apply a load in increments.

35

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Figure 6: A milled brass wire holder in a stand with a micrometer drive

which allowed vert¡cal adjustments

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,+

Figure 7: A bend test of a wire specimen in archform in a slot support.

Support glued to the scale pan to allow load/unload values to be

recorded.

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Archwires tested

¡.) Archwires with 45" anchor bends were formed from three different

spools of Australian Wilcock stainless steel wire and then loaded and

unloaded as described above.

sspp 016sspp 018ssp O2O

5 specimens

3 specimens

5 specimens

i¡.) Six archwires were formed from sssp O2O. Archwires 1-3 had 35'anchor bends while archwires 4-6 had 25" anchor bends. This allows the

effect of different anchorage bends to be assessed.

sssp O2O 6 specimens

The wires in groups ¡.) and ii.) were electropolished later and then

retested.

i¡i.) Eight archwires were formed from three different spools of

stainless steel Wilcock wire of varying diameter and grades including the

recently released pulse straightened wires. 45" anchor bends were placed

in the archwires excluding sssp O2O (12-13) where 55" anchor bends

were formed. This enabled the effects of different sized anchorage bends

to be assessed.

sspp 018

sspp ps O1 Isssp O2O

2 specimens

2 specimens

4 specimens

Electrooolishing

An electropolishing unit (Rocky Mountain 7OO, USA) containing 85o/"

orthophosphoric acid was used to electropolish the archwires at the fixed

potential of 13V D.C., for varying lengths of time as listed. The specimen

was attached with a crocodile clip placed at the opposite end to the steel

tube. Care was taken to ensure that the specimen was fully immersed to

avoid the archwire overheat¡ng and annealing. The specimen was also

gently agitated during electropolishing (F¡g. 8).

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Figure 8: An electropolishing unit. Specimens were attached to a

crocodile clip, fully immersed in orthophosphoric acid and then a current

passed through the wire.

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Ten sections of sssp O2O (O.50mm) were cut. Six specimens were

electropolished continuously for 25,50,75, 1O0, 125 or 150 seconds

respectively. Four wires were electropolished for twenty-five second

intervals until a total of either 25,50,75 or lOO seconds was reached'

This was to assess ¡f the intermittent electropolishing affected the wire

properties differently to continuous electropolishing. Wire diameter was

recorded at three different locations before and after electropolishing;

near the point of attachment, midwire and furthest from the attachment.

Wires tested in the as-received state were then electropolished for

varying lengths of time as stated below prior to loading and unloading.

i.)

ii. )

sspp 018sspp 018

2 specimens

1 specimen

sspp 016sspp O16

3 specimens

2 specimens

ep30"ep45"

ep3O"

ep45"

ep30"

ep45"

ep25"ep5O"

ssp O2O

ssp O2O

sssp O2O

sssp O2O

3 specimens

2 specimens

3 specimens

3 specimens

plus

plus

ep5O"

ep50"

Archwire diameters were recorded before and after each electropolishing

with a micrometer (Mitutoyo Japan).

(2.) Cantilever tests

Many of the bend tests reported in the literature are conventional

cant¡lever tests. The American Specification, No 32 specifies that a one

inch length of wire should be used for cantilever tests. Drake et al, 1982

stated that one inch lengths were used ¡n the cantilever tests. For these

reasons a similar length was used in this study.

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:¡:il;i

Thirty five millimetre lengths of wire were cut to take into consideration

the lOmm lengths of steel tube glued to one end.

(diagram from Ware 1967)

i.) The following wires were assessed in the as-received state. A steel

milled holder with a slot was glued to the scale pan and used to support

the free end of the archwire at a distance of 18mm. Some wires were

also electropolished as listed below and retested.

F

L

at

nt

sspp

sspp

sspp

sssp

O18 x O25

016016018

ps O18

o20

ep30" or ep45"

ep30" or ep45"

ep25" plus ep50"

ep50" plus ep50"

ii.) A knife edged milled steel holder was glued to the scale pan to

support .the free end of the wire (F¡g. 9). A distance of 2Omm was left

between the steel tube and the knife edge support' The wire types and

electropolishing times were the same as for (2) ¡.).

¡ii.) Six lengths of sspp ps O18 wire specimens were prepared. Each

specimen was tested twice, using a distance of 10mm and 2Omm

between the steel tubing and knife edged support. This was to assess

whether distance affected the results.

Two specimens were tested by loading and unloading, prior toelectropolishing.

4l

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'1

Figure 9: A cantilever bend test with a knife edged support glued to a

scale pan to record load/unload values.

42

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One of these specimens was then electropolished for periods of twenty

five seconds until a total electropolishing time of one hundred seconds

was achieved. After each period of electropolishing the wire was loaded

and unloaded at lOmm and 20mm.

The remaining four specimens were electropolished for 25, 50, 75 and

1OO seconds respectively and then tested. This was to establish if the

results were altered when the electropolishing was interrupted.

iv.) Annealed cantilever specimens were assessed using a distance of

2Omm between the steel tubing and knife edged support. The wires

assessed were as listed.

at

btnt

SSS

SSPP

SSPP

sspp

sspp

sssp

018 x O25

O17 x O25

016010012014016018o20

One specimen each, excluding sssp 020 where two Speclmens were

tested.

v.) Four specimens of annealed sssp O2O were prepared. These

specimens were tested using a distance of 2Omm between the knife

edged support and steel tub¡ng.

One wire was electropolished for intervals of 25 seconds and retested

after each period of electropolishing, until a total of 1OO seconds

electropolishing time was reached.

The remaining four wires were electropolished for 25,50, 75 and 1OO

seconds respectively and then tested.

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Plastic deformation of the annealed wires probably occurred with loading.

Fewer unload values were consequently recorded when compared with

the load values.

vi.) After assessment of the initial elastic modulus values calculated

from the cantilever tests some tests were repeated.

It was noted in previous tests that the load and unload values took a long

time to equilibrate possibly due to stress relaxation. To standardise, thirty

seconds was allowed to elapse between altering the extension and

recording the load/unload value. lnstantaneous values are probably more

accurate but are too difficult to measure.

(¡.) Six new sssp O2O specimens were prepared and tested on a knife

edge support at a distance of 20mm. These wires were not annealed or

electropolished. Three specimens were tested without rernoving the

curve present as a result of being on a spool. The other three specimens

were straightened with fingers prior to loading.

The initial reason for repeating tests on sssp 020 was that the elastic

modulus values calculated from the load data, were significantly higher

when tested in the annealed state compared to the as-received state.

(ii.) Six annealed sssp O2O specimens were prepared and tested on a

knife edged support at 2omm. Two specimens were tested after

annealing but no electropolishing.

One specimen was electropolished for 25 second intervals and retested

until a total electropolishing time of 100 seconds was achieved'

The remaining four wires were electropolished 25, 50, 75 and 1OO

seconds respectively and tested.

The reason for repeating these tests was that the elastic modulus value

increased when the electropolishing time was 50 seconds compared with

a 25 second electropolishing time. The general trend noted was a

decreasing value for elastic modulus as the electropolishing time

increased. The initial increase noted may be explained by hydride

formation and precipitation hardening'

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vii.) To assess for potential effect of wire diameter on elastic modulus the

following wires were assessed in the as-received state on a knife edge

support at 2Omm. The specimens were 35mm long and had l omm

lengths of steel tubing glued to one end.

nt

sent

o14 I 016 / 018

016/018x025 lO22xO28

The nickel-titanium wires were retested at a distance of 1Omm.

(3.) Three ooint bend tests

Two milled steel knife edge supports were glued to a scale pan with the

edges parallel to each other and spaced 20 mm (Fig' 1O)'

F

L

(diagram from Ware 1967)

Six 25mm lengths of sspp ps 018 wire were cut. Two specimens were

tested in the as-received state while the remaining four were

electropolished 25,50,75 and 1OO seconds respectively. The diameters

were recorded before and after electropolishing. A milled steel circular

plunger was attached to the stand and centrally placed on the wire

specimen. lt was then loaded in increments of ten thousandths of an inch

(O.25mm). Load readings were recorded in grammes to two decimal

places. The wire was then unloaded in ten thousandths of an inch and an

unload value was recorded.

45

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I,l

rt

t

f--

It*r

Figure 1O: A three point bend test with two knife edge supports glued to

the scale pan and a centrally placed circular plunger to load and unload

the wire.

46

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Use of the load and unload data

The thousandths of an inch measurements were converted to a metric

unit and a graph with a stra¡ght line of best fit was drawn to show the

load and unload separately, in relation to the extension. Where the

accuracy of this line of best fit was poor the values at the start or

completion of loading and unloading were not used.

The equation of best straight Iine fit y = mx + c was determined. A

value of 1 was used for x to determine the y value. ln this case x and y

values refer to the x and y axis respectively.

Elastic modulus for cantilever tests were calculated from the follow¡ng

formula (Beam Theory Methodology)

-3- I'a3vI

where F : load/unload value (y axis)

a : distance between steel tube and support

slot knife 4

I L

/ : extension (x axis)

Calculation for 1 (second moment of area) varies depending

on whether the wire is round or rectangular in cross section.

E

a

I for circular wire : d: diameter

ó : breadth

*do64

bh3

t2I tor rectangular wire :

å : height

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To calculate values of elastic modulus for three point bend tests the

following formula was used

Fa'48yI

The formulas used for calculation of the elastic modulus are from Blake,

1982.

c. Resonance

The following wires were tested in the as-received state

sss Ol O

sspp 012,014,016,018sspp ps 016,018

sssp O2O

1 15mm lengths of wire were cut and one end was clamped inside a

milled brass wire holder. A 1g plastic weight was attached l OOmm from

the support. The distance was reduced to 50mm with the more flexible

sss O1O wire.

The wire was manually displaced to oscillate the wire specimen. The

frequency of a Strobotac type 1531 General Radio Company, Concord,

Massachusetts, USA was adjusted until the wire appeared stationary

(subjective approximately SHz) (Fig. 11). This was best done in a

darkened room. The modulus of elasticity can be calculated from:

E

I2n

trErI-

\ mt'

Where "fnEIm

I

.f^

: frequency of vibration: elastic modulus: moment of inertia: mass: distance

48

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Figure 11 Equipment used to determine the natural frequency of

vibration of wire spec¡mens.

49

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The formula appeared very sensitive to diameter changes. A Mitutoyo O-

25mm O.OOOI mm accuracy m¡crometer

diameter. The diameter used was an

measurements.

was used to measure w¡re

average of three different

The sspp 016 and sssp O2O were tested after electropolishing. Three

specimens of each were electropolished for 25" and another three

specimens of each were electropolished for 1O0".

d. Soeed of sound

The speed of vibration through a wire is thought to be the most accurate

method of elastic modulus calculation. A Systron Donnor Corporation

Datapulse 1 16 Pulse Generator was used to generate a voltage which

was amplified in a SOW amplifier prior to being passed through a l2Omm

length of as-received sssp O2O wire. A piezoelectric crystal

(cyanacrylated to transducers) detects the vibration, which is then

passed through a Charge Amplifier Type 2635 Bruel and Kjaer and finally

to a Hewlett Packard 54601A Oscilloscope (Fig. 121. The vibration was

then detected by a second piezoelectric crystal spaced at either 40,60,80, lOO or 12Omm and as before passed to the oscilloscope. Two wave

forms appear and cursor placement (at the peak of the wave crest, depth

of the trough or at the first sign of deviation) allows the time elapsed

between the vibration detected at the first and second crystal to be

calculated in microseconds:

v

Where : velocity : distance x time: elastic modulus: density ( SMgm-3 for stainless steel 304 )

Different amounts of tension were placed on the wire. Tension did not

appear to affect the consistency of the results. Varying the distance

between the piezoelectric crystals may have an effect. This may be due

to proximity of the crystals to the grips holding the wire specimen.

v

Ep

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Q,Ê ç

Figure 12 Equipment used to calculate the speed of sound through

wire.

a

51

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The formula used to calculate the velocity was taken from Ashby and

Jones 198O.

A sssp O2O wire specimen was annealed and then tested under similar

conditions. This was to remove the potential anisotropic effect possible in

such heavily cold drawn wires (Goldberg et al 1977l.'

e. Microhardness test uring the Leitz Wetzlar Germany 4262 miniload

hardness tester. A length of as-received sspp 018 wire was shaped to

enhance mechanical retention in the Bakelite (coloured phenolic resin)' A

Buehler Simplimet ll was used to embed the specimen in Bakelite. The

specimen was polished to a mirror finish, placed on the hardness tester,

viewed at 4Ox magnification and then tested using a "confocal" small

pyramidal diamond indentor. A 30 second time period was allowed to

elapse from the time of release of the (camera) trigger used for applying

the load, before removing the load. Approximately 5Oo/o of this time was

the actual loading time. This method of loading was continued across the

width of the wire and repeated with a 25 pond and then a 50 pond

weight. A pond (P) is equivalent to a 1 gram force.

Due to the Bakelite mounting the specimen needed to be gold / palladium

coated prior to viewing in the Philips 505 SEM. Photomicrographs were

recorded at 1.42F.3 to assess for changes in hardness. A collage was

then made. The length of the two diagonals were calculated from the

photomicrograph. When assessing the photom¡crographs ¡t must be

remembered that the specimen is thinner near the edges so greater

deformation would be anticipated. These values would be less reliable

(Fig. 131.

From this information the Vickers microhardness number could be

calculated from tables or the following formula.

1854 x Pd2

Where P: applied load in grams

d:the distance of the diagonal of the square in micrometers

HV

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Figure 13: Photomicrograph of microhardness test (magnification 142Oxl

which illustrates the greater deformation near the edge of the specimen.

53

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Macrohardness test using the Vickers Pyramid Hardness Tester.

The standard Vickers indentor is a diamond in the form of a square based

pyramid. VHN is independent of applied load but for ease and greater

accuracy of measurement it was recommended to choose a load which

gives an impression that fills two thirds of the field of view. A 2O-3Okg

load was recommended for steels.

The specimen used for microhardness test was polished sufficiently to

remove the gold palladium coat¡ng. A 20kg load was initially attempted

but it was not possible to indent the wire only and consequently a

calculated hardness number would be meaningless. Even when a Skg

load was used it was very difficult to indent the wire only. A microscope

was used to measure the lengths of the diagonals of the indentation.

From these measurements the hardness number was calculated by either

of the following formulae.

DPN

t.854P

P

A

or DPND,

Where DPN : Diamond Pyramid Hardness Number

P : the applied load in kilograms

A : the surface area of the pyramidal impression in

millimetres squared

D : distance of the diagonal in millimetres

The formulas used to calculate microhardness and macrohardness tests

are from the Miniload Hardness Tester Manual, 1968.

2. Surface appearance.

a. A sample of as received sspp 018 and sspp ps 018 were prepared to

enable surface differences as a consequence of pulse straightening to be

assessed in the SEM. Pulse stra¡ghtened wires feel smoother to the

fingers.

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b. Wire surfaces were examined for changes after electropolishing. Seven

lOmm lengths of wire, were cut from sssp O2O wire' Six were

electropolished for 25,50, 25 + 50, 50 + 50, 25 + 50 + 50, 50 + 5O

+ 50 seconds respectively. The wire sections were then attached to

stubs with conducting "silver dag" and assessed in the scanning electron

microscope (Philips 505 SEM) at magn¡fications of 75 and 3OO' The

seventh specimen was not electropolished to act aS a control to

compare surface changes.

c. Fractography. Wires were deliberately maltreated by bending in pliers

at a single point many times until point of fracture. This is not indicative

of clinical practice but the aim was to assess the fractured surface to see

if there were textural differences between the surface layer and central

core. The range of wires chosen included sspp 01 2, 014, 016, 018, sspp

ps 016 and 018, nt 016, se nt 01 6, O2O,018 x O25, 0215 x 028. The

first bend was 9Oo and subsequent bends were 18O". The number of

bends required to fracture the wire were recorded.

Seven 25mm specimens of sspp 018 were cut. Four specimens were

electropolished for 25, 50, 75 and 10O seconds respectively. All

specimens were then work hardened until point of fracture. The fractured

specimens were attached to stubs with silver dag, assessed in the Philips

5O5 SEM at varying magnifications and photographed.

Another Seven specimens of the wire from the same spool were

prepared. Prior to manipulation these wires were heat treated at 3sO"C

for ten minutes and then allowed to bench cool. A high temperature

(14OO'C) chamber furnace was used and the temperature was checked

using a "Carbolite" thermocouple and ten minutes were allowed for

equilibration to occur. The reason for the heat treatment was to remove

the potential effect of hydrogen embrittlement. Steels, especially high

strength steels are prone to hydrogen embrittlement'

The composition of Some specimens were assessed using a Tracor

Northern TN 55OO Model EDS system. Aluminium was present in some

areas assessed despite being well away from the stub. An additional two

fractured specimens of sspp 018 were prepared, one from the same

55

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spool and the other from a new spool. These were then attached to a

graphite covered aluminium stub prior to ED analysis.

3. Detailed microstructural data.

Specimen preparat¡on determines the quality of TEM micrographs'

Mechanical grinding is the fastest technique but may cause unacceptable

damage and is generally not feasible for final thinning. Chemical and ion

or fast atom thinning methods thin slowly and unevenly resulting in only

small electron transparent areas but produce minimal damage. Dimple

grinding produces an exceptionally smooth surface and reduces specimen

thickness w¡th m¡nimal damage. lt is precise enough to produce a final

thickness of less than 3pm in the centre and leave a thick supporting rim.

A short period of chemical/particle beam thinning to produce electron

transparent areas is then required.

All diagrams are copíed from the "TEM specimen preparation of

semiconductors, ceramics and metals by ion milling" handbook (Gatan

1992).

Four different wire types were initially selected:

1. sspp ps O18

2. ss O175 multibraided

3. ss O21 x 025 braided

4. nt 016

Since foil preparation of multibraided stainless steel wires proved

particu¡arly difficult due to the small cross section of the individual wires

this was discontinued.

56

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The final wires that were prepared for foil specimens in cross section

included

1. sspp 0182. sspp ps O18

3. at O18 x O253

4. nt 016

As many short lengths of wire as possible were embedded in Gl Epoxy /

Hardener (Gatan) (10 parts resin to 1 part hardener) withín tub¡ng of

approximately 3mm external diameter to approximate the size of grids

used in TEM holders. The wires and steel tub¡ng were first cleaned with

acetone to remove any contaminants. Thick walled tubing was used to

minimise the amount of epoxy present. Wire samples from spools tended

to be curved, so to assist placement in the tubes the wires were first

straightened. The epoxy was syringed into the empty tub¡ng and the

wires were individually coated with epoxy before being placed ¡nto the

tubes to minimise the chances of air entrapment.

The samples were then placed in an oven for five minutes at 1OO"C for

the epoxy to be cured (Fig. 14). Curing was indicated by a colour change

of the epoxy from amber to Pink.

The tubing was cut in cross section to approximately O.5mm thickness,

using a carborundum disc at slow speed and an oil water coolant to

avoid overheating. The specimens were held in a milled steel holder and

manually thinned on silicon carbide 12OO grit paper with water to

approximately 0.1 - O.O7mm (Fig. 15).

A dimple grinder Gatan Model 656 (Fig. 16) was used to thin the

sections after centralising the specimens on the platform with cross hairs

under magnification. A 2Og weight was applied during grinding and the

slowest speed was chosen (1OO revolutions in 1 minute and 38

seconds).

A 15mm spherical bronze wheel 656-0106 with Gatan Desc diamond

cutting compound 2-4pm and water lubricant were used. To avoid

contamination a wheel is used with only one polishing compound. To

minimise surface scratch¡ng the specimens were polished with Gatan

57

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r60

40 G-l EPOXYO

I rzolõo)q rooto)t--gsofO

60

40 ll50 r00

Curing Time (minules)

Figure 14: Curing character¡st¡cs of G - 1 epoxy used for prepar¡ng TEM

cross sect¡ons.

I

D¡sk Cutl¡nq

70-100pm

Oisk grinding

Figure 15: This diagram illustrates cutting the tub¡ng in cross section of

SOOpm and then disc thickness after manual gr¡nd¡ng to 70 - 1OOpm.

58

Page 78: Methods of testing the mechanical properties of ... · t5'3.'tS METHODS OF TEST¡NG THE MECHANICAL PROPERTIES OF ORTHODONTIC WIRES A report submitted in partial fulfilment of the

ønleMþht

bad scåle0 - sogm

ra¡s€ loer€r mlcroíreler sp€omnplatformcam dr¡ve

wtÞel o€r nragætclumtaue

Figure 16: Precision dimple grinder and polisher

III

oroa

116,l

*

o

fÍi/otsdplâtlom

59

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Alumina Pol suspension using a felt wheel. After dimple grinding the

centre of the specimen should be approximately .0o5mm (F¡9. 17).

Specimen thinning from both sides was attempted to start with. Due to

the thinness of the foil it proved difficult to invert the specimen without

disrupting the epoxy matrix. Sticky wax (a low melting point

thermoplastic polymer) was used at first to firmly attach the specimens

to the stub. To form a strong and uniformly thin bond the wax must be

heated to around 130'. The effect of heating the sticky wax to remove

the specimen after dimpling, was sufficient to soften the epoxy and

dislodge the wires. Superglue was then used to the adhere the specimens

to the stubs and 75% acetone was used to dissolve the superglue.

Specimen removal was still difficult due to close adaptation of the

specimen to the stub and limited exposure of the superglue to acetone.

An alternative method was devised where the specimen was

mechanically held with a mounting plate fixed with screws.

lnitially specimens were thinned in the Gatan dual ion mill model 60O at

room temperature using a grinding angle of 15", gun current O.5mA DC

and gun voltage 3kV (Fig. 18). The time required to perforate the

specimen was much greater than that stated in the manual where 30

minutes was suggested.

The specimens disintegrated and were lost before perforating due to

preferential loss of the epoxy. The performance of the G1 Epoxy I

Hardener (Gatan) was questioned as its shelf life was approaching twelve

months. ln addition, although storage at room temperature was stated to

be adequate, in Australia where high temperatures are experienced,

refrigerated storage may be more appropriate. New epoxy was ordered

and specimens were reprepared. However the problem was not

overcome.

To avoid loss of the specimens the foils were placed between two nickel

lOO slotted grids placed at right angles to each other. The grids were 2o/o

nitrocellulose coated followed by carbon coat¡ng. Only one gun was used

with the same current and voltage but at a lower grinding angle of 8". An

earlier attempt at ion milling between copper grids was unsuccessful due

to the copper being milled at a faster rate than the specimens.

60

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ba1smm dia.

lOmmdia. .5Ém

Figure 17: ThiS diagram illustrates: (a) a standard grinding wheel and

mount and (bl the thickness of the specimen centrally after dimple

grinding.

61

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alon Beam

10

9ECM€N

30

b25

0

lon Beam

Maler¡al: Copp€rGun Current: 0-5mABeam Angle: 20degreesGas: Argon

2_

t0

e3zoÈfo-cØ3ls-9g(I)(õ lO(ro,.Ecc7sl-

6 I t2

40

Gun Voltage (kV)

Effect of OctogunrM Voltage on Specimen Thinning Rate

c00

ao-E(ú

Co)

f()c(l)

E'õq)oU)

þN BEAM

e

40

0 20

Beam Angle (degrees)

Specimen Current vs Beam Angle for Argon Millingof Copper

Figure 18: These diagrams illustrate the thinning action of the Gatan dual

ion mill. The effect of OctagunTM voltage, spec¡men current and beam

angle on thinning rate are ¡llustrated.

gl¡orcas. l.rúlldal gün úed)

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The specimens were removed every two hours for viewing in the

scanning electron microscope to assess the thinned areas' After

approximately ten hours of ion milling the specimens appeared to have

sufficiently thinned areas. They were then transferred to folding copper

grids (because the nickel grids were not able to be attached) which had

also been coated in with 2o/o nitrocellulose and carbon. This proved

difficult owing to the fact that the Specimens were now magnetic'

Floating the specimens on a water bath minimised handling of the

specimens but small fragments did appear to break off from the fo¡ls.

The specimens were examined in the JEOL l OOS but no electron

transparent areas were found. The goal is to examine these specimens in

the transmission electron microscope (JEOL 2OOOFX) to assess the

crystalline structure and diffraction patterns.

Gatan was contacted regarding the problems being experienced. Their

suggestions included using a tube of the Same material as the wire which

is feasible with the stainless steel wires but not for the alpha-titanium or

nickel-titanium wires. The importance of minimum epoxy and maximum

wire density was re-emphasised. Stainless steel rods were milled with an

O.O16" and O.018" central hole and a slot of 0.O18" x O.025" to allow

new specimens to be made with minimum epoxy present (Fig' 19)' ln

addition the rectangular specimens were cured under pressure using a

small G clamp.

The wire surface was also roughened with 12OO grit paper before

embedding to enhance mechanical locking of the epoxy to the specimen.

Desc. Cubic Boron Nitride (4-6pm and O-2¡rm) were recommended as the

polishing paste and a low angle ion mill was also recommended'

Longitudinal

Two wire types were selected:

1. ntO182. sspp ps O18

The specimens were attached to double sided cellotape and mechanically

thinned on 12OO grit paper to O.1mm. This was a very labour intensive

procedure.

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Figure 19: Rods of stainless steel were milled with a central hole the

same size as the wire specimen to minimise the epoxy present.

64

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A m¡croprocessor-controlled table top machine called Abramin was

utilised for automatic grinding, lapping and polishing of all materials. Wire

specimens were attached to acrylic blocks with sticky wax and then

placed in a specimen holder. The specimen holder and polishing disc

rotate at 1Sorpm. The holder is eccentrically positioned relative to the

polishing disc to ensure a fast and good polish without creating comet

tails. A lOON grinding pressure was used on 22OP and lOOOP grit paper

with a water lubricant.

For final polishing and thinning to perforation an E. A. Fischione model

12O-23O twin-jet electropolishing machine was used (F¡g. 20)' A 3mm

length of the thinned specimen was cut and placed in the lollipop holder

ensuring that there was contact with the platinum ring on either side.

The polishing solution consisted of 1oo/o petchloric acid, 20% glycerol

and 7Oo/o ethanol. This was cooled to approximately -2O"C with liquid

nitrogen. Once the solution was cooled the speed was adjusted so that

the jets would just meet. A 25V D.C. voltage was selected. When the

specimen perforated it was removed from the lollipop, rinsed in ethanol

and placed on a copper grid and viewed in the JEOL 2OOOFX.

Despite careful preparation no suitable thin foils could be produced'

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Figure 20: Twin-jet electropolishing machine used to perforate prethinned

specimens.

66

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CHAPTER 5RESULTS AND DISCUSSION

Tests are performed on resil¡ent orthodontic wires to determine their

mechanical properties. There are three main methods of testing the

mechanical properties of an archwire. They include using a tensile testing

machine, utilising a cantilever beam set up and measuring the resilience

of a wire.

The Australian Standard (AS 1964) requires three tests; tensile strength'

wrapping ability and resistance to bending. The force required to fracture

the wire being held between the two grips is used to calculate the tensile

strength (standards Association of Australia 19771. The American

Specification, No. 32, tests similar wire properties; flexure yield strength,

modulus of stiffness and resistance to bending. Flexure yield strength is

derived from cantilever beam tests and from this the modulus of stiffness

is mathematically catculated (Council on Dental Materials and Devices

19771.

Stainless steel wires have dominated in orthodontics because of their

desirable physical characteristics. They possess a good balance of

environmental Stab¡l¡ty, stiffness, resilience, formability and low coSt.

Despite their long history of use fundamental questions st¡ll remain

regarding their metallurgical and mechanical properties (Khier, Brantley

and Fournelle 1988). For these reasons emphasis was placed on

assessing stainless steel orthodontic wires in this research project'

Elastic modulus values

Stiffness, springback and formability are generally considered to be the

three most important properties of an archwire. The stiffness of a wire

determines the magnitude of the force delivered by the appliance.

Although light physiological forces are desirable for tooth movement, the

archwire must have sufficient stiffness to resist undesirable plastic

deformation during function.

Goldberg and Burstone 1979 (as stated in Sokel 1984) considered that

wires with a low load deflection rate have distinct clinical advantages.

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The desirable characteristics include the ability to apply lower forces; a

more constant force over a longer period of time; greater ease and

accuracy in applying a given force; the ability to use larger act¡vat¡ons

and the assoc¡ated increased "working time" of the appl¡ance.

Stiffness may be mathematically calculated for wires which obey Hooke's

law for elastic bodies. lt is proportional to the modulus of elasticity which

may be calculated from the stress-strain ratio determined at any point on

a linear section of the graPh.

ln this research project elastic modulus values were calculated from data

acquired from a simple tensile test, bend tests, natural frequency of

osc¡llation and measuring the velocity of a vibration along a wire.

properties of orthodontic wires were assessed in the as-received state

and after manipulative treatments such as electropolishing and heat

treatment.

Modulus of elasticity for a pafticular material has traditionally been

thought to be an invariable property (whittle 1993). The value for

young's modulus is determined by the atomic number of the metal and is

said to be only marginally affected by heat treatment or cold work¡ng

(lngerstev, 1966). Forsyth and Stubbington (1975) (as stated in Sokel

1g84) drew attention to the importance of the crystal orientation to the

value of the modulus with respect to the titanium alloys."

Masson 1969, assessed 016" orthodontic wires and noted that Young's

Modulus of Elasticity for stainless steel orthodontic wire in the cold-

worked or heat treated condition is not a constant value. The accepted

value for the modulus of elasticity of stainless steel wires was

approximately 30 x t 06 lOs/¡n2 (ZOlCea) but Masson claimed that we

have been mistaken in making this assumption. Later in 1977, Goldberg

et al showed a substantial decrease in the value of modulus in stainless

steel with heavY cold working.

It ¡s of interest to note that values of 155 GPa, which are twenty percent

below the published values of 193-2OO GPa, have been calculated for

016 unspecified stainless steel wire (Yoshikawa et al 1981). At the other

extreme values as high as 248 GPa have been reported by Goldberg'

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Accurate measurement of the modulus of elasticity for thin wires poses

some difficulties (Goldberg et al 1983a/b).

A. Conventional tensile tests

Masson 1969 stated that the elastic modutus value for stainless steel

varies depending on which wire is being assessed. The variation is most

likely due to the amount of cold work and stress relief heat treatment

that the wire has undergone during manufacture, The values for the

Modulus of Elasticity (lbs/sq.in.) in tensile testing arc listed below

together with the metric equivalents3. Values increased through the

range of .016 Wilcock wire from "Regular" up to "special Plus" as listed

in Table 1.

Table 1: Elastic modulus values for as-received stainless steel wires from

tensile tests of O.O16" stainless stee¡ (ss) wires (Masson 1969)'

It was noted that an .O16 Dentaurum Remanit "Super Spring Hard" is a

precipitation-hardening stainless steel that has been heat treated and its

E was the highest of all the wires tested at 26.1 t O.8 x 106 lbs/in2

(180 + 5 GPa).

Twelftree 1g74, noted that elastic modulus values calculated from tensile

testing varied from 150 to 174GPa depending on the grade of stainless

steel (Table 2). This finding was in agreement with Masson's 1969'

3Ahhough orthodontic wire is supplied in imperial units and many early results

(particularly American) also used imperial units, scientific results are now invariably

presented in S.l, units. lt has been decided in this thesis therefore to present where

necessary both original published results and their metric equivalents.

170 Í 524.6 * O.8Special Plus

160 * 623.2 * O.9Special

160 + 523.2 * O.7Regular Plus

157 t622.8 ¡ O.9Regular

(GPa)

ELASTIC MODULUS

(106 lbs/¡n2)wrRE 016 SS

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Table 2: Elastic modulus values for as-received stainless steel wires from

tensile tests of stainless steel wires (Twelftree 19741'

sokel (1984) compared the tensile properties of different wilcock

stainless steel wires and noted the large variation in values for Young's

modulus of elasticity (Table 3). Values for Young's Modulus showed a

considerable scatter with a range of 154 - 199 GPa and a mean value of

174 GPa was noted.

174f6premium plus

17o^ f 6mrum

164 t4S al lus

150 i 5S cial

ETASTIC MODULUS

lGPa)

WIRE STAINLESS STEEL

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166

154020 Premium

161

189018 Special Plus

163

163

018 Regular

188

199

193

016 Regular

185

164014 Special Plus

156

181

014 Regular

173

184012 Special Plus

168

168012 Special

172

179O1O unspecified (probably supreme)

ETASTIC MODULUSWIRE TYPE

Table 3: Elastic modulus values for as-received O.O1O"-O.O2O" stainless

steel wires from tensile tests (Sokel 1984)'

No obvious correlation was noted between the elastic modulus value and

either wire diameter or wire grade.

Sokel ment¡oned the difficulties in the tensile testing of orthodontic wires

due to the the¡r high tensile strength and elast¡c modulus and low

ductility. For these reasons experimental apparatus must be extremely

accurate s¡nce very small percentages of elongation are being measured'

Secondly any defect in the wire such as a kink would greatly affect the

results. Wire spec¡mens and the grips were closely assessed for defects

before testing. The third difficulty is in accurately read¡ng the results.

ldeally the stress-stra¡n sect¡on is straight in the elastic region while an

ever increasing curvature is noted in the plastic region.

'tt

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Many wires used are in the cold drawn condition and consequently the

Stress-Strain curve was found to be curved almost from the start of

loading. Young's Modulus is determined by measurement of the slope of

the ¡n¡t¡al portion of the curve. Many different tangents could be chosen

and therefore values obta¡ned were subject to a large var¡ation (Fig. 211.

As a consequence a range of elastic modulus values may be more

appropr¡ate than a single elastic modulus value.

Despite the difficulties to measure elastic modulus values the results are

comparable to the 175 GPa quoted by Yoshikawa et al (1981)' The

values are well below the figure of 193 GPa quoted by Goldberg and

Burstone (1g79). lt was proposed that a different experimental method is

required to measure Young's modulus with greater accuracy.

Singh lggl noted after preliminary tensile tests on alpha-titanium

straightened and combination wires, consistently low elastic modulus

values despite repeated test¡ng and the use of an extensometer. These

low values were found to be similar to those obtained by Hazel, Sokel

and West , 1984.lt was interesting to note that values for yield strength,

tensile strength and O.2o/o proof stress were consistent w¡th published

values for alpha-titanium (Singh 1991).

Tensile testing is unable to test the formability of wires. A wire may look

promising according to the quantitative tensile tests but may be clinically

unsuitable due to poor formability. Despite this limitation of tensile

testing and the large variation in elastic modulus values, tensile testing is

still important because of the comparable data available.

It has been suggested therefore that the use of tensile data to determine

flexural data for fine orthodontic wire is inappropriate. Orthodontists

primarily stress wire in bending in the clinical situation (Goldberg 1983b;

Nikolai et al 1g88). For these reasons alternative methods of test¡ng the

mechanical properties of wires were explored such as bend tests'

Not much information is available as to the effect of bend versus tensile

testing on the elastic modulus values. The imperial values from Table 4

are taken from the thesis of Masson 1969. Again metric values have

been calculated to aid comparison with other data'

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U)U)11,

E.t--(/)

DB

A-

c./

STRAIN

Figure 21.. Diagrammatic representation of a stress-strain curve

illustrating two tangents A - B and C - D which could be chosen to

determine the elastic modulus.

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157 ¡. 522.8 + O.8Unisil (ss wire from Unitek)

016

170 + 524.6 + 0.8Wilcock Special Plus 016

(GPa)

TENSILE

ELASTIC MODULUS

(1 06 lbs/in2)

MATERIAL

Table 4: Elastic modulus values for as-received stainless steel wires from

tensile and bend tests (Masson 1969).

It was noted that the value for Young's modulus of Elasticity for Wilcock

"Special plus" wires in tension was very similar to the value obtained in

bend tests. This was not the case for "unisil" wires where values

obtained from tensile tests were lower than those from bend tests'

Masson 1969 believed that the Wilcock stainless steel Special Plus wire

values were similar in tensile and bend tests because of the stress-relief

heat treatment. Stress-relief heat treatment is discussed later in Section

3(2). Unisil was in the cold-worked cond¡t¡on and therefore contained

many internal stresses which are unpredictable.

lf tensile testing is to be used, it would be preferable to load and unload

the same specimen prior to fracture several times, as the initial load

stress-strain curve is unreliable due to kinks in the wire. The initial slopes

of any load (excluding the first curve) and unload stress-strain curves

should be the same and may be used to mathematically calculate the

elastic modulus. Sokel 1984 cyclically loaded and unloaded specimens to

measure the elastic modulus of wires but elastic modulus values with

large variations were still produced.

171 + I24.8 + 1.2Unisil (ss wire from Unitek)

016

168 t 1024.3 *. 1.5Wilcock Soecial Plus 016

(GPa)

BEND

ETASTIC MODULUS

(106 lbs/in2)

MATERIAL

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ln the present study, some preliminary tests were performed, but due to

major problems with extensometers and computer software, the results

obtained were unreliable and not reproducible. lt was decided therefore

to concentrate on other testing techniques which more closely followed

clinical orthodontic application or corresponded to other accepted dental

material standards.

B. Bend tests

Wires were ¡n¡tially tested in archform to assess them in a similar

configuration to that used in clinical practice and provide comparitive

data to results from the more conventional test methods. Due to the

complexity of calculating the elastic modulus for this geometry, elastic

modulus values could not be calculated and cantilever and three-point

bend tests were used in preference in the later sections. sections 1-5

will refer to tests on stainless steel wires while Section 6 will be "other

wires".

1. Preliminary experiments in arch form.

(1 ) as-received sPecimens

Bend tests were performed on wires, as-received in archform. 45o anchor

bends were placed unless otherwise stated. The stress-strain curves for

each test are in the Appendix: graphs 1 - 27. Straight lines of best fit

were computer chosen for the data plotted. Equations for these lines are

included in the form y = c I mx (m : slopel.

Many of the stress-strain curves were curved despite the specimen being

tested within the elastic limit. Several different tangents could be

selected as discussed by sokel 1984 and illustrated in Figure 21. As a

consequence the slopes and equations for the lines of best fit would

vary.

Elastic modulus values were not calculated due to the complexity of

mathematics required but the wires may be compared by the slopes (rn)

of the stress-strain curves which are listed in Table 5.

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The data presented is in its raw state and the number of decimal places

is not a reflection of the accuracy.

Table 5: Slopes (m) of stress-strain curves for as-received stainless steel

wires in arch form

.o64.069

.093108059065.055.061

.o63.069sso 020

.1 89.19455"

364.34955"

.229232

.177183

038038350

045038350

039.04135"

.096.09925"

.068.o7425"

079.o8725"sssp 020

231214208.194018

177.189.1 89194.053061

046.050.049055ssoo 01 8

.038.o44o44.051

o29.031

030034.o28030ssoo 01 6

m(UNLOAD}

m(LOADt

ANCHORBEND

MATERIAL

The slopes from unload data were generally 5% lower than those for load

data. This is evident from the lower m value. This was surprising given

that the wire was not plastically deformed and may be as a consequence

of the experimental set-up, in that frictional forces between the wire and

support slot may differ on loading and unloading.

The range of values for some wire types (sspp O16, sspp ps O18 and ssp

O2O) were narrow. However for sssp O2O and sspp O18 wires large

variations were noted. Values ranged from 0.038 to 0.349 (although the

bend angles may have some, probably small, effect) and O.O5O to O.189

76

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respect¡vely, with factors of more than 9 and almost 4 difference which

could not be explained.

(2) after electropolishingAn experienced clinician commented that wire stiffness appeared to

change after electropolishing (personal communication with M.R.Sims).

Electropolishing removes the outer surface of the wire which may affect

the surface appearance and diameter of the wire.

Sokel, 1984 ment¡oned the possibility of an oxygen embrittled surface

layer on near-alpha titanium wires.

Wilcock wire is deliberately oxidised by heat treatment during

manufacture. On occasions oxygen is forced through the oven to ensure

adequate oxidation. The oxidation cleans the wire and leaves it with a

roughened surface which ensures that lubricant adheres to the wire. The

lubricant protects the dies as the wire passes through during the drawing

process (Masson 1969). A similar oxygen embrittled surface may be

present on stainless steel wires. Removal, such as by electropolishing'

may alter the wires ProPerties.

Orthodontic wires are heavily cold worked and when magnified the wire

surface shows very elongated grains giving a fibrous appearance' The

wire may appear homogeneous but the surface is theoretically more

severely cold worked than the central area during wire drawing (Dieter

1961 as stated in Twelftree 1974). This heavily cold-worked surface area

may represent the tag often noted after wire fracture. The loss of this

heavily cold-worked surface layer may result in altered wire properties.

Analysis of wires in cross section may reveal differences in the surface

and central areas of the wire.

(¡) Surface changes

Photomicrographs are

appearance".

were assessed in the PhiliPs

included later in the section F

505 SEM.

on "surface

(iil Diameter changes with electropolishing

To catculate the elastic modulus of a wire, the diameter is required. Some

formulae, such as that used for the calculation of elastic modulus from

resonance tests, were shown to be extremely sensitive to diameter

77

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changes. An average of three values measuring wire diameter were used

when calculating the elastic modulus.

A Mitutoyo micrometer with ratchet was used to measure the wire

diameters. This removes potential operator error induced by pressure

variation used to t¡ghten the jaws of the micrometer. An alternative

method may be measurement from sEM photomicrographs.

The results for changes in wire diameter are given in Table 6.

Table 6: Diameter change of stainless steel wires after continuous

electropolishing (eP).

* may be explained by variation in the start diameter of this particular

wrre

Closest to the attachment preferential polishing appears to occur. When

catculating the mean an average of the diameters midwire and furthest

were used. A maximum error of .O2mm was noted.

The data listed in table form above is also shown below graphicallY (Fig.

22t.

O.42 + .O2o.440.40o.201506

O.42 + .O2o.440.400.331255

O.44 ¡ .O20.45o.420.451004

0.46 + .Olo.470.450.48*753

0.48 t .Olo.48o.470.45502

o.500.500.s00.50251

MEAN

OF

MIDWIRE/

FURTHEST

(mm)

FURTHEST

FROM

ATTACHMENT

(mm)

MIDWIRE

(mm)

NEAR

ATTACHMENT

(mm)

EP

(secs)

SPECIMEN

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Figure 22: Diameter change with electropolishing sssp O2O'

DIAMETER CHANGE WITH ELECTROPOLISHING SSSP O2O

DIAMETER (mM)

o.5

o.45

o.4

o.35

o.3

o.25

o.2

o.15

o 25 50 75 100 125 150

CONTINUOUS ELECTROPOLISH¡NG TIMI(secs)

near attachment A mid wire X furthest fromattachment

+mean

Minimal w¡re diameter changes are noted after twenty-five seconds

electropolishing. After lengthy periods of electropolishing the diameter

red uces significantlY.

It was noted that diameter changes were not even along the length of

the wire. The effect on diameter was reduced with increasing distance

from the clip although the diameter immediately under the po¡nt of

attachment was minimal. Variation in diameter increased as the

electropolishing t¡me lncreased. lt is noted that the electropolishing times

are much longer than that used clinically. Lengthy electropolishing times

were deliberately chosen to highlight any potential changes.

When calculating the elastic modulus, variation in wire diameter after

electropolishing and in the as-received state needs to be considered

although var¡ation of the tatter is probably not as marked. The results

above suggest a range (mean with a standard deviation) of elastic

modulus values may therefore be more appropriate than a single value.

The results for changes in wire diameter due to interrupted

electropolishing are given in Table 7.

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o.460.460.460.3925+25+25+25

4

o.47o.47o.470.4325+25+25

3

o.47o.47o.470.4525+252

o.490.490.490.48251

MEAN

OF

MIDWIRE/

FURTHEST

(mm)

FURTHEST

FROM

ATTACHMENT

(mm)

MIDWIRE

(mm)

NEAR

ATTACHMENT

(mm)

EP

(secs)

SPEC¡MEN

Table 7: Diameter change of sta¡nless steel wire after interrupted

electropolishing (ep).

Mean diameter values were calculated again from midwire and po¡nts

furthest from the attachment diameters. Data in table form was then

plotted graphicallY (Fig. 231.

Figure 23: Diameter change with electropolishing sssp O2O.

DIAMETER CHANGE WITH ELECTROPOLISHING SSSP O2O

o.45

DIAMETER (mm)

o.4

o.35

o 25 25+25 25+25+25 25+25+25+25

CUMULATIVE ELECTROPOLISHING TIME (secs)

X furthest fromattachment

o.5

A

E

E near attachment A mid wire +mean

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Bend tests were performed on wires after electropolishing to determine

whether the elastic modulus values were altered. Wires in archform with

45o anchor bends, unless otherwise stated, were tested after varying

times of electropolishing. The data was plotted and from the stress-strain

curves a line of best fit was chosen. The equation for the straight line y

: C * mx where m : slope allows the data to be compared. The slopes

are listed in Table 8. The slopes are listed for each of the stress-strain

curves which are included in the Appendix numbers 28 - 46. Slopes for

load graphs were cons¡stently h¡gher than for unload graphs.

lnstabi¡it¡es were often noted in these stress-strain curves for load and

unload data making selection of the l¡ne of best fit difficult. This was also

noted in stress-strain curves in both the as-received and electropolished

condition.

Table 8: Slopes (m) of stress-strain curves for stainless steel wires tested

in arch form after electropolishing (ep).

o60.0664505506045

.o7108030058o6230.066.07330sso O2O

08508950+5025"

.051.05350+5025"

.054.05750+5025"

o24o2625+50350

.03704025+50350

.03804025+5035"sssp 02O

05806745o47.05130o38.o4230o18

o22o2345o25.o2745o26.03030046.05330

o2703030sspp 016

m(UNLOAD)

m(LOAD)

EP

secsAnchor

Bend

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Although these tests provided comparative data, without actual elastic

modulus values few conclusions can be drawn.

ln the literature many of the bend tests are conventional cantilever tests.

Cantilever bend tests, using short lengths of wire, mimics the clinical

situation where the archwire is more comparable to a series of short

beams between brackets. ln addition simple mathematical formula are

available to calculate the elastic modulus value. For these reasons it was

decided not to pursue archform bend tests but rather to perform

cant¡lever bend tests.

2. Cantilever tests

(1) as-received

From the experimental data stress-strain curves were plotted and a line of

best fit was computer chosen to calculate the slope. The curves and lines

of best fit included in the Appendix were those initially drawn. As stated

earlier, the initial portion of the stress-strain curves were often curved.

fgnoring ze(o, the straightest portion of the stress-strain curve was

identified and the appropriate data replotted and a line of best fit chosen.

By modifying the graphs in this manner the slopes and elastic modulus

values increased. This was repeated for all stress-strain graphs where

appropriate. The elastic modulus values were then calculated using the

beam theory methodology described in the materials and methods

sect¡on.

lnitial Stress-strain curves are included in the Appendix section(i) graPhs 47 - 50(ii) graphs 51 - 62'

The results giving the elastic modulus values calculated in each test from

the loading and unloading curves are given in Table 9 and 1O.

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(il Table 9: Elastic modulus values (E) for as-received stainless steel wires

calculated from cant¡lever bend tests with the support at 18.Smm.

45.4162.18sssp 020

1 19.81148.2618

97.7097.15018

61.8980.48ss 016

E

(GPa) UNLOAD)

E

(GPal (LOAD)

WIRE TYPE

The elastic modutus values exhibit a very large scatter and are much

lower than the published data which suggest values of 193 to 2OO GPa'

These exper¡mental values were therefore dismissed. lt was thought that

the slot support may result in friction between the wire and support,

sufficient to invalidate the results. A knife edge was used as an

alternative supPort.

(ii) Table 1O: Elastic modulus values (E) for as-received stainless steel

wires calculated from cantilever bend tests with the support at 20mm'

104.17*+151.75

gg.06*127.82*

129.39*+

155.81

106.96149.58

100.39122.70

101.161 19.46

113.28't28.75sssp 020

167.1186.02

168.89190.24

169.49193.01sspo ps 01 B

172.65196.24ssoo 01 8

171.18201.89016

E

(GPa) (UNLOAD)

E

(GPa) (LOADI

WIRE TYPE

* curvature resulting from wire being spooled removed prior to testing

83

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lgnoring differences in wire types (ie premium plus and special plus) the

elastic modulus values decreased as wire diameter increased from O16 to

O18 to O2O. As discussed in section A on tensile test¡ng Masson 1969

and Twelftree 1974 stated that elastic modulus varied depending on the

grade of stainless steel wire. The values for the 016 and O18 wires are

closer, but still low, when compared to the published values for elastic

modulus. Elastic modulus values for the 020 wires were much lower'

Elastic modulus values for the O16 and 018 wire groups were reasonably

consistent with mean values of 2O2GPa and 191 t 4GPa respectively.

Values for the O2O group were scattered and inconsistent and there

appeared to be two groups with mean values o'f 126 + SGPa and 153 +

15GPa. Two groups of O2O were tested where in one group the

curvature resulting from the wire being spooled was removed prior to

testing but this did not explain the d¡fferences as the two groups cut

across this category. Another explanation may be the presence of large

variation along the wire but th¡s would seem unlikely.

lnitial elastic modulus values showed that pulse straightening appeared to

have little effect.

(21 Effect of electroPolishing

As previously mentioned a clinician suggested that electropolishing may

affect the elastic modulus value. Additional tests to compare elastic

modulus of as-received wires with electropolished wires were performed.

lnitial stress-strain curves for the bold data are included in the Appendix

(i) graphs 63 - 68

(ii) graphs 69 - 84.

The results are presented in Tables 11 and 12.

(i) Slot support at 18.5mm

selected wire samples were assessed after electropolishing using a

cant¡lever bend test w¡th a slot support at 18.5mm and the results are

given in Table 1 1. Values for the wires tested in the as-received state (in

non-bold type) are included for comparison.

84

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79.6592.5150+50

11.4323.5325+50

45.4162.18ssso 020

45.6360.6645

59.8768.1930

97.7097.15018

71.61a2.9245

58.O076.1230

61.8980.48016

E

(GPa) (UNLOAD)

E

(GPa) (LOAD)

EP

(secs)

WIRE TYPE

Table 11: Elastic modulus values (E) for electropolished ("p) sta¡nless

steel wires calculated from cantilever bend tests w¡th the support at

18.5mm.

Again the figures were very low and of limited value'

(ii) Knife-edge support at 2omm

Cantilever bend tests were performed on wires after electropolishing

using a knife edge support at 2Omm. These elastic modulus values are

¡isted in Table 12. As-received values are included again (in non-bold

type) for comparison.

85

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145.37176.5750+50

141.33176.3925+50

136.33162.2450

127.50160.1925

+104.17+

151.75

gg.06*127.82+

129.39*

155.81 *

106.96149.58

100.39122.70

101 .16119.46

113.28128.75sssp o20

141.O2152.55100

136.18152.2025+25+25+25

169.201A2.9275

157.52167.5525 + 25 +25

150.62165.2550

129.41147.9525+25

136.27152.34

160.6217A.7325

167.15186.02

168.89190.24

169.49193.01018

155.69179.3445

167.13193.5830

172.65196.24018

184.68212.4645

189.OO220.5930

"171.18201.89016

E

(GPa) (UNLOAD)

E

(GPa) (LOAD)

EP

(secs)

WIRE TYPE

Table 12: Elastic modulus values (E) for electropolished ("p) sta¡nless

steel wires calculated from cantilever bend tests with the support at

2Omm.

*curvature resulting from wire being spooled removed prior to testing

86

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No particular pattern could be given to the effect of electropolishing on

the elastic modulus values. The elastic modulus values for the

electropolished o18 wires appeared reduced compared with the as-

received specimens but not proportionately to the electropolishing time.

This observation may be explained by the high surface stresses being

removed with electropolishing. In contrast elastic modulus values

increased after electropolishing when compared with the as-received

values for both 016 and o2o wires so the theory of removing the high

stress surface does not hold making the effect of electropolishing on

elastic modulus values confusing. However it is likely that errors in

measurement are much greater than any effect if it exists.

3. Other techniques

To compare the effect of changing experimental parameters and of

different methods of testing on elastic modulus values samples were

tested on a knife edge support at lOmm or using a three point bend test.

lnitial stress-strain curves for bold values are included in the Appendix

(1)(i) graPhs 85 - 86(ii) graphs 87 - 94

(2)(i) graPhs 95 - 100

(11 Cantilever tests on a knife edge support at lOmm

It would seem appropriate to determine the mechanical properties of

orthodontic wires using very short lengths of wire in a cantilever bending

test as this mimics the clinical situation (Brantley and Myers 1979). lt has

been shown that varying lengths of the same mater¡al between half, one

and two inch specimens, gave elastic modulus values which differed by

more than lOOo/o (Brantley 1978 as stated in lngram et al 1986)'

Reducing the distance of the support to lOmm would have the effect of

reducing specimen length.

87

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il as-received

These results are given in Table 13. Results for the same wire type

tested on a cantilever support but at 2Omm are included (in non-bold

type) for comparison.

Table 13: Elastic modulus values (E) for as-received sta¡nless steel wires

from cantilever tests with the support at 1Omm.

Reducing the distance of the knife-edge support from 20mm to l Omm

reduced the elastic modulus values'

iil electropolished

The modulus values obtained after electropolishing are given in Table 14.

Again, results of electropolished wires tested on a knife edged support at

2Omm are also included (in nin-bold type) for comparison.

167.15186.02

168.89190.24

169.49193.0120mm

107.3817A.78

124.51172.82sspp ps 01 B

E

(GPa) (UNLOADI

E

(GPa) (LOAD)

WIRE TYPE

88

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141.O2152.5520mm

94.97116.23100

1 36.1 8152.2020mm

92.57't23.1525+25+25+25

169.20182.9220mm

130.40170.1775

157.52167.5520mm

95.42130.7325+25+25

150.62165.252Omm

1 15,57158.6850

129.41147.9520mm

98.28127.3825+25

136.27152.34

160.62178.7320mm

101.29157.85

95.96140.425

107.38178.78

124.51172.82018

E

(GPa)

(UNLOAD)

E

(GPa) (LOAD}

EP

(secs)

WIRE TYPE

Table 14: Elastic modulus values (E) for electropolished ("p) stainless

steel wires from cantilever tests with the support at lOmm'

The elastic modulus values calculated from tests at l Omm are lower than

the values calculated with the support at 20mm with the possible

exception of one spec¡men electropolished 25 seconds. The elastic

modulus values calculated at 2Omm were already less than the publ¡shed

89

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elastic modulus values. Varying the position of the support appears to

have an effect on the elastic modulus value. This is in agreement with

Brantley 1978 as stated in lngram et al 1986.

(2) Three-point bend tests

Twenty-five millimetre lengths of wire were supported by two knife

edges placed 2Omm apart and then loaded centrally. These results are

given in Table 15.

Table 15: Elastic modulus values for stainless steel wires after

electropolishing (ep), calculated from three-point bend tests.

All values are much lower than those quoted in the published data.

Elastic modulus values after electropolishing were above and below those

of wires tested in the as-received state. This is not surprising given the

difficulty of achieving a consistent result even when retesting a wire'

As previously reported Goldberg et al 1977 showed a substantial

decrease in the value of modulus in stainless steel with heavy cold

working. As stainless steel orthodontic wires are progressively drawn to

smaller diameters they ate increasingly cold worked. Goldberg et al

1983b mentioned the anisotropic tendency of heavily drawn wires.

Forsyth and Stubbington (1975) Sokel 1984, have also drawn attention

to the importance of the crystal orientation to the value of the modulus

with respect to the titanium alloys.

153.66153.6725+25+25+2b113.80159.6525+25+2585.98149.9625+25

76.65136.8525

96.21149.62o

95.59147.97osspp ps 01 I

E

(GPa) (UNLOAD)

E

(GPa) (LOAD)

EP

(secsl

WIRE TYPE

90

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It was thought that the reduced elastic modulus values noted in both

tensile and cantilever tests may be associated with the heavy cold-

working procedures. Cold-worked metals can be converted back to an

equiaxed Structure by heating the structure above the recrystallization

temperature. This is referred to as annealing the wire'

Masson (1969) noted that Wilcock wires are heat treated after each

drawing but the actual temperature of treatment is not available. All that

Wilcock revealed was that the process is " more than a stress-relieving

process" although the heat treatment temperature after the final draw

could not be very high since the cold worked properties need to be

maintained. A stress-relief process at low temperature only releases some

of the residual strain induced by plastic deformation. There does not

seem to be a consensus on the optimal temperature and length of time

required for heat treatment (Funk, 1951; Backofen and Gales, 1951;

Kemler, 1956; Mutchler, 1961; Howe et al., 1968 recommend different

temperatures and times). The approximate temperature lies between 371

and 484"C which is below the recrystallisation temperature'

4. Testing of annealed specimens

Specimens of orthodontic wire were annealed to minimise the anisotropic

behaviour prior to cant¡lever bend tests. The aim of the annealing was to

achieve elastic modulus values closer to the published data. Goldberg et

al 1g77 had noted that the elastic modulus value of cold-drawn sta¡nless

steel wire was considerably less than that normally quoted but when

recrystallized the wire possessed a modulus closer to textbook values

(being 177 to 2O3 GPa) as stated by Braden et al 1979 in a review of

dental materials.

A knife edge support was used at a distance of 2Omm

lnitial stress-strain curves for bold values are included in the Appendix

(1) graPhs 1O1 - 1O9

(2) graphs 110 - 125

Less data was recorded and therefore plotted for the unload curves for

annealed specimens due to the reduced springback'

9l

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(1) annealed

The modulus values for annealed samples are given in Table 16' Where

available the results from wires tested in the as-received state are

included (in non-bold type) for comparison.

Table 16: Elastic modulus values (E) calculated for annealed stainless

steel wires from bend tests with a support at 2Omm'

*curvature resulting from wire being spooled removed pr¡or to testing

Elastic modulus values were calculated from the load data. The sss O1O

specimen elastic modulus value was close to the accepted value of

between 193 to 2OO GPa.

Elastic modulus values for as-received and annealed specimens of sspp

016, sspp 018 and sssp O2O tested on a knife edge support at 2Omm

were compared. Values for annealed sspp 016 and O18 wires were lower

than when tested in the as-received state. sssp 02O elastic modulus

values were higher when compared to as-received values. This result was

unexpected. O2O special plus wires are drawn less than 018 or 016 wires

and are therefore less cold-worked. lt would be anticipated that annealing

104.17-151 .75-98.06*127.82-

129.39-155.81 -106.96149.58100.39122.70101 .16119.46113.28128.75as-received

2a166.7270.67140.7867.O2166.5146.66168.59ssso O2O

172.65196.24as-received

119.73121.46018

171.18201.89as-received

170.63172.60o1

31.59186.8801481.89150.9001295.56205.33sss 01O

E

(GPa) (UNLOAD)

E

(GPa) (LOAD)

WIRE TYPE

92

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would have a greater impact on the elastic modulus value of the more

cold-worked wires but the reverse was true.

The elastic modulus values calculated from the unload data were all

extremely low and less than values calculated from the load data. This

may be accounted for by the reduced springback of annealed wires.

(2) Annealed and electroPolished

The effect of electropolishing on annealed samples was also assessed

and results given in Table 17.

Table 17 Elastic modulus values (E) calculated for annealed and

electropolished (ep) stainless steel wires from bend tests with a support

at 20mm.

44.35t158.14r153.30150.351 00"74.66147.6510.69157.1625" +25" +25" +25"

121.97t123.4Or126.73128.0875"55.36145.62

129.57146.7225" +25" +25"

136.33162.28not annealed / eP50

3.63r138.22¡81.37170.1550"61.60143.0829.34188.6225" +25"

127.501 60.1 Inot annealed I eP25

19.O3r116.15r9.O2153.14

74.13158.8254.94144.O825"

28.85166.7270.67140.7867.02166.5146.66168.59annealed / not epssso 020

E

(GPal (UNLOAD)

E

(GPa) (LOAD)

EP(secs)

WIRE TYPE

r denotes retest of wire immediately above

93

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There is insufficient data to determine an effect of interrupting the

electropolishing versus continuous electropolishing. Given that no

differences were noted when diameter changes were compared after

continuous versus ¡nterrupted electropolishing, ¡t is unlikely to be

significant. For these reasons it was decided that results of wires

electropolished for the same total time could be grouped together to

provide the average values given in Table 18.

Table 18: Mean elastic modulus values (E) calculated for annealed and

electropolished (ep) sta¡nless steel specimens'

There is no systematic change in Young's modulus with increasing

electropolishing time.

A comparison can be made for as-received wires after ep25" and 50"

(16OGPa and 162GPa respectively). Again, annealing of the wires did not

have the anticipated effect of increasing the elastic modulus values.

It was noted that the elastic modulus values for the retested wires were

lower excluding the wire electropolished 1OO seconds'

5. Other wires

These wire specimens were all tested in the as-received state. Wires

have been grouped together according to the tests performed. lnitial

stress-strain curves are included in the Appendix(1) graPhs 126 - 127-

(2) graphs 128 - 132(3) graphs 133 - 138

(4) graphs 139 - 141

153100

13575

16050

14325

1610annealed sssp 020

E mean(GPa) (LOAD)

TOTAL EP TIME(secsl

WIRE TYPE

94

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For preformed nickel-titanium archwires, the straightest section of the

archwires were used.

(11 Cantilever bend tests using a slot support at 18.Smm

These results are given in Table 19.

Table 19: Elastic modulus values (E) for alpha-titanium (at) and nickel-

titanium (nt) wires calculated from cantilever bend tests with the support

at 18.5mm.

*measurement given as height x breadth

Very low elastic modulus results were noted previously when' a slot

support was used, and again l¡ttle reliability could be placed in these

results.

(21 Cantilever bend tests with a knife edge support at 2Omm

These test results are given in Table 20.

Table 20 Elastic modulus values (E) for alpha-titanium (at), nickel-

titanium (ntl and superelastic nickel-titanium (se nt) wires calculated from

bend tests with the support at 2Omm.

18.9123.75nt 016

19.1138.40at 018 xO25*

E

(GPa) (UNLOADI

E

(GPa) (LOAD}

WIRE TYPE

19.6122.56se nt 022 x 025

30.1615.88sent018x028

23.8235.00se nt 016

45.5052.52nt 016

41.8854.49at 018 x 025+

E

(GPa) (UNLOAD}

E

(GPa) (LOAD}

WIRE TYPE

*measurement given as height x breadth

95

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(3) Cantilever bend test us¡ng a knife edge support at lOmm

These test results are given in Table 21

Table 21: Elastic modulus values (E) for nickel-titanium (nt) wires

calculated from bend tests with the support at lOmm'

r denotes retest of wire immediately above

(41 Gantilever bend test using a knife edge support at 2Omm

These results for the annealed specimens are given in f able 22'

Table 22= Elastic modulus values (E) for alpha-titanium (at), beta-titanium

(bt) and nickel-titanium (nt) wires calculated from bend tests with the

support at 2Omm.

Data calculated from tests (2), (31 and (4) will be discussed according to

wire type.

5570.89r

44.9866.50nt 018

41.83r52.84r

38.9557.11nt 016

25.76¡30.50r

21.4928.17nt 014

E

(GPa) (UNLOAD}

E

(GPa) (LOAD)

WIRE TYPE

61.0974.48nt 016

102.44263.1 Ibt 017 x 025

41.8158.63at018x025

E

lGPa) (UNLOAD)

E

(GPa) (LOADI

WIRE TYPE

96

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1. alpha-titaniumTwo specimen of 018 x O25 were tested resulting in elastic modulus

values of 55 and 59GPa. These values are lower than the range 78 - 99

GPa as quoted by sokel 1984.

2. beta-titanium

One beta-titanium O17 x O25 wire was tested. The elastic modulus value

of 263Gpa was very high. A wide range of elastic modulus values are

quoted for beta-titanium wires ranging from 55 - 11OGPa (Goldberg and

Burstone 1979) and 65GPa (Burstone 198O).

3. nickel-titaniumpreliminary tests using a cant¡lever bend test with a knife edge support at

1Omm, indicated that the elastic modulus value increased from 28GPa to

67GPa as the wire diameter was increased from 014 to 018.

The cantilever test was repeated for nt 016 using a knife edge support at

2Omm. The elastic modulus value was 53GPa which was lower than the

57Gpa recorded at 1Omm. This is in contrastto trend noted in section 3.

(1) where the elastic modulus values calculated with the support at

2Omm were higher than those calculated with the support at lOmm'

Burstone and Goldberg 1980 quoted an elastic modulus value of 33GPa

for nickel-titanium wires.

No elastic modulus values are quoted in the literature for the superelastic

nickel-titanium wires. lnitial tests showed a range of 16 - 35GPa for the

wires tested. When discussing elastic modulus values for these wires

with one company it was stated that an actual value is not quoted but

the shape of the stress-stra¡n curve is what is relied on for quality

control.

There was considerable scatter of the data. only limited data was

plotted, to enable the straightest section of the stress-strain curve to be

drawn. Despite this, a large range of elastic modulus values were

calculated.

97

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Mechanical tests still appear unsatisfactory so

methods of assessing the elastic modulus were

included resonance and the velocity of sound.

alternative physical

investigated. These

G. Resonance

A wire specimen with a 1 gramme plastic weight attached to one end

was manually displaced to oscillate the wire specimen. The frequency of

a strobe light was adjusted until the wire specimen appeared stationary'

A frequency was recorded in rpm. The elastic modulus value was

calculated using the formula described in the materials and method

section.

1. Preliminary(1) Wire size

Several different diameter stainless steel wires were tested. The results

are listed in Table 23 according to wire diameter.

Table 23: Elastic modulus values (E) for as-received stainless steel wires

calculated from preliminary resonance tests.

1363.29E-150.0010.1s.8333333500.000509sssp

o20

1612.05E-150.0010.153000.0004s2sspp

018

1482.01E-l50.0010.14.752850.00045sspp ps

018

1751.41E-l50.0010.14.333333260o.000412sspp

016

1551.41E-150.0010.14.O833332450.000412sspp ps

016

1478.O6E-160.0010.131800.000358sspp

014

't373.98E-160.0010.12.0333331220.0003sspp

o'12

1581 .98E-160.0010.054.3666672620.000252sss 010

E VALUE

(GPal

I VALUEMASS

(ko)

LENGTH

(metres)

FREO

{Hz)

FREO

(rpm)

DIAMETER

(metres)

WIRE

TYPE

98

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The elastic modulus values for the sta¡nless steel premium plus wire

ranging from 012 to O18 were inconsistent. The sspp pulse straightened

016 and 018 wires elastic modulus values were lower when compared

with the same dimension non-pulse straightened stainless steel'

(21 Electropolishing effects

The sspp 016 and sspp O2O wires were electropolished for either twenty-

five or one hundred seconds prior to testing. These results are given in

Table 24. Results for as-received wires are also included (in non-bold

type) for comParison.

Table 24: Elastic modulus values (E) for electropolished ("p) stainless

steel wires calculated from preliminary resonance tests.

A twenty-five second period of electropolishing did not appear to affect

the elastic modulus. A period of one hundred seconds electropolishing

appeared to slightly reduce the elastic modulus values'

(31 Other wires

A limited range of nickel-titanium and superelastic nickel-titanium wires

were assessed. lt was difficult to oscillate these wires for a sufficient

length of time to allow the strobe frequency to be adjusted until only one

1312.95E-150.0010.15.4166673250.000495sssp 020

ep1 00"

1353.22F-15o.0010.15.75345o.o00506sssp 020

ep25"

1363.29E-15o.0010.15.833333350o.000509sssp 02O

1691.19E-150.0010.13.9166672350.000395sspp 01 6

eol 00"

1751.31E-150.0010.14.1666672500.000404sspp 016

ep25"

1751.41E-150.0010.14.3333332600.000412016

E VALUE

(GPa)

I VALUEMASS

(ks)

LENGTH

(metres)

FREO

(Hz)

FREO

(roml

DIAMETER

(metres)

W¡RE

TYPE

99

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image was seen. Although reducing the distance at which the weight

was suspended assisted experimentation, tests were only pursued on

stainless steel wires. The results are given in Table 25'

Table 25: Elastic modulus values (E) for nickel-titanium (nt) and super

elastic nickel-titanium (sent) wires calculated from resonance tests'

Results for nt 016 and nt se 016 were significantly lower when

compared with values for the same wire types from cantilever tests in

section 5. No comparable data was available for nt se O2O.

2. Detailed tests

Three specimens of each wire type were prepared and then tested. The

wires were tested in the as-received state. Six additional specimens of

sspp O1G and sssp O2O were prepared. Half were electropolished twenty

five seconds and the remainder one hundred seconds.

(11Wire size

Results from tests on as-received stainless steel w¡res are listed in Table

26 according to diameter.

Table 26: Elastic modulus values (E) for as-received stainless steel wires

calculated from resonance tests.

25.23.35E-150.0010.057.1666664300.000511sent 020

20.21.35E-150.0010.02511.5690o.oo0407sent 01 6

28.21.23E-150.0010.025137800nt 016

E VALUE

(GPa)

I VALUEMASS

lko)

LENGTH

(metres)

FREO

(Hz)

FREO

(rom)

DIAMETERWIRE

TYPE

100

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wire 3 o.000 I 5.s83333335 0.1 3.29E-150.001 125wire 2 360 0.16 0.001 1453.27E-15

0.000508wire 1 385 0.16.416667 0.001 1663.26E-15

o20

wire 3 2800.000448 4.666667 0.0010.1 1.98E-15 145

0.000449wi¡e 2 285 0.14.75 0.001 1491 .99E-15

0.00045wire 1 4.833333290 0.1 2.01E-l50.001 153

sspp ps

018

wire 3 2900.00045 4.833333 0.0010.1 2.01E-l5 153wire 2 3000.00045 5 0.0010.1 2.O2E-15 163

wire 1 3050.00045 0.15.083333 0.001 1692.01E-15

18

wire 3 2450.00041 4.083333 0.0010.1 1.39E-15 158wi¡e 2 2400.000412 0.14 0.001 1491.41E-15wire 1 2450.000411 4.083333 0.0010.1 1.4E-15 156

sspp ps

016

wire 3 2500.000411 4.166667 0.0010.1 1.48-15 163

0.000412wire 2 250 0.14.1 66667 0.001 1621.41E-15wire 1 2450.000411 4.083333 0.0010.1 1.4E-15 156ssoo 01 6

wire 3 0.000358 3.833333230 0.1 8.06E-160.001 240wi¡e 2 1950.000358 0.13.25 o,001 1728.06E-16wire 1 1800.000358 3 0.0010.1 8.04E-16 147

o'14

0.000303wire 3 160 0.12.666667 o.001 4.12E-16 227wi¡e 2 1500.000303 2.5 0.1 4.148160.001 199wire 1 1450.000301 2.416667 0.0010.1 4.O5E-16 190

012

wire 3 2550.000253 4.25 0.0010.05 2.O1E-16 148wi¡e 2 2550.000254 4.25 0.0010.05 2.03E-16 146

0.000254wire 1 4.166667250 0.05 o.001 1402.048-16sss 010

DIAMETER

(metres)

WIRE

TYPE

FREO

(Hz)

FREO

(rpm)

LENGTH

(metres)

MASS

(ks)

I VALUE E

VALUE

(GPa)

101

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The elastic modulus values for the sspp O12 wires are close to the

published data. All othervalues are lowexcluding sspp 014 wire 3 which

is too high. lt is interesting to note the large range of values for both the

sspp 014 and sspp O2O wires. No particular pattern was observed'

(21 Electropolishing effects

The effects of electropolishing on modulus values are listed in Table 27

according to wire type and electropolishing time.

Table 27: Elastic modulus values (E) for electropolished ("p) stainless

steel wires calculated from resonance tests.

O16 as-received E values were 1 Pa 162GPa and 163GPa

020 as-received E values were 166GPA 14 Pa and 125GPa

E VALUE

(GPa)

I VALUEMASS

(kql

LENGTH

(metres)

FREO

(Hzl

FREO

(rom)

DIAMETER

(metres)

WIRE

TYPE

wire 3 2350.00040s 0.13.916667 0.001 1531.32E-15

0.000406wire 2 4.25255 0.1 1.33E-150.001 179wire 1 2350.000404 3.916667 o.0010.1 1.31E-15 154

sspp 01 6

ep1 00"

wire 3 2400.000409 o.14 0.oo1 1531,38E-15wire 2 2500.00041 4.166667 o.0010.1 1.39E-15 165wire 1 2550.00041 0.14.25 o.001 1721.38E-15

sspp 01 6

eo25"

wire 3 3600.000505 0r16. o.001 1483.19E-1 5

wi¡e 2 340o.000505 5.666667 0.0010.1 3.2E-15 1320.000s06wire 1 355 0.15.916667 3.21E-15o.001 143

sssp 020

ep1 00"

wire 3 3600.000508 6 0.o010.1 1453.28E-15

0.000s08wire 2 360 0.16 0.001 1453.28E-15

0.000505wire 1 5.75345 0.1 3.2E-150.001 136

sssp 020

ep25"

toz

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Despite using an alternative technique it was still proving difficult to

produce a consistent elastic modulus value. A large range of elastic

modulus values were calculated. ln addition the values were still

significantly lower than the textbook figures often quoted' For these

reasons it was decided to pursue a further technique which measures the

veloc¡ty of sound.

D. Velocity of sound

1. Preliminary experiments

A vibration was passed through as-received sssp O2O wire with attached

piezoelectric crystals spaced at either 40,60, 80, lOO or 12Omm' Two

wave forms appear on the oscilloscope screen which represent the

initiating and "received/dampened" vibration. The distance between the

two wave forms was measured by cursors to calculate the time elapsed.

The reference po¡nts used were varied: peak to peak, trough to trough

and the points of first deviation from the horizontal. The diagram of the

wave patterns observed on the oscilloscope screen illustrates the

different reference points used (Fig. 241.

(1) The distance between the peaks was used as a reference. These

results are given in Table 28. lt was noted that it was not easy to

determine accurately the crest of the peak.

Table 28: Elastic modulus values (E) for stainless steel wire calculated

from speed of sound tests using the peaks as reference points.

92.981 1 621 9013409.0913.52E-Oso.12

84.33105414073246.7533.08E-05o.1

73.4691 827363030.3032.64E-050.08

37.2746581442158.2732.788-050.06

20.16251 95261587.3022.528-050.04

E VALUE

(GPa)

(vELOClrY)2VELOCITYTIME

(us)

DISTANCE

(m)

103

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PEAK

+

DEVIATION

TROUGH

+

(11 wave detected by first piezoelectric crystal

(2) wave detected by second piezoelectric crystal

Figure 24: Dtagrammat¡c representation of wave pattern on oscilloscope

screen after a single vibration passed along the wire length. The different

reference points used to measure the time elapsed are also illustrated.

*

(1)

(21

104

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The elastic modulus values were all very low. lt was noted that as the

distance between the piezoelectric crystals is increased the elastic

modulus values increased'

l2l A different reference point (the base of the troughs) was chosen to

see ¡f more accurate values could be calculated. These results are given

in Table 29.

Table 29: Elastic modulus values (E) for stainless steel wire calculated

from speed of sound tests using the troughs as reference points'

The elastic modulus values were higher than when the peaks of the wave

form were used as a reference, but still lower than the published data.

Again it is noted that the values for elastic modulus increased as the

distance between the piezoelectric crystals increased.

(31 An alternative reference point was tried, in which it was attempted to

determine the first deviation from linearity in the crystal output. The

results of the point of first deviation from the horizontal as a reference

are given in Table 30.

133.281 66597254081.6332.948-05o.12

114.78143480263787.8792.64E-050.1

101.14126419753555.5562.258-050.08

78.139765625312510.06

s6.8971111112666.6670 50.04

E VALUE

(GPa)

(vELOClrY)2VELOCITYTIME

{us)

DISTANCE

105

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167.82209777984580.1532.62E-05o.'t2

168.34210420004587.1562.18E-05o.1

144.861810774',|'4255.3191.88E-O50.o8

146,94183673474285.7140.0000140.06

158.021 97530864444.4440.0000090.04

E VALUE

(GPa)

(vELOClrY)2VELOCITYTIME

(ps)

DISTANCE

(ml

Tabte 3O: Elastic modulus values (E) for stainless steel wire calculated

from speed of sound tests using the point of deviation from the

horizontal as the reference point.

The elastic modulus values were much better but still low. As the elastic

modulus values were most promising using this reference point ¡t

continued to be used.

(4) Annealed

To minimise the anisotropic behaviour of heavily cold drawn orthodontic

wires ¡t was decided to test an annealed section of sssp o2o. The

variation in modulus with distance between the piezoelectric crystals is

given in Table 31.

Table 31: Elastic modulus values (E) for annealed stainless steel wire

calculated from speed of sound tests using the point of deviation from

the horizontal as the reference point.

The elastic modulus values were much higher than when tested in the as-

received state and most were close to the published data range. The

value of 2OO is within this range.

214.O3267538645172.4141.74E-O50.09

20025000000s0000.0000160.08

181.41226757374761.9051.26E-050.06

312.539062s0062506.4E-060.04

E VALUE

(GPa)

(vELOClrY)2VELOCITYTIME

(ps)

DISTANCE

(m)

106

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The high elastic modulus value of 312.5GPa may indicate that the

distance between the piezoelectric crystals is too short.

The results of repeating these tests using a new sect¡on of annealed wire

are given in Table 32.

Table 32: Elastic modulus values (E) for new annealed stainless steel wire

specimen calculated from speed of sound tests using the point of

deviation from the horizontal as the reference point'

Unfortunatety when the tests were repeated the majority of elastic

modulus values were too high. Where the crystals were separated 90 to

lOOmm the values were more in keeping with anticipated results'

Early tests indicated that ¡t was not easy to achieve consistent results.

The use of a square wave form which would give a well defined

reference point may be advantageous.

The potential for variation in wire tension to affect the elastic modulus

value needs to be investigated. lf tension does affect the elastic modulus

values a weight may need to be hung from the wire to eliminate this

variable.

246.91308641 985555.s562.16E-05o.12

232.60290753565392.1 572.04E-050.11

208.25260308205102.0411.96E-050.1

204.5225564954s056.181.78E-05o.09

276.82346020765882.3531.36E-O5o.08

355.56444444446666.667o.0000090.06

355.56444444446666.6670.0000060.04

E VALUE

(GPa)

(VELOCITY}2VELOCITYTIME

(rrs)

DISTANCE

(m)

ro7

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Summarv of the elastic modulus tests

A comparison of elastic modulus values derived from different techniques

using load data

Table 33 has been compiled to allow easy comparison of elastic modulus

values for different wire types and test methods. Where more than one

wire specimen was tested, mean elastic modulus values with a standard

deviation are quoted . All values are calculated from load data only'

108

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Table 33: A comparison of elastic modulus values derived from different techniques using load data.

sspp ps 01 6

EP 100secEP 45secEP 30secEP 25sec

sspp 0l 6sspp 014sspp 01 2sss 010

2 o28sent018x028

snt 018

nt 016nt 014

o25at018x025

Wre Type

8376

81

24

38

SlotSupport18.Smm

GPa

213221

202

2316

35

53

55

KnifeedgeSupport20mm

GPa

69r355r3

29 r.2

KnifeedgeSupport1Omm

GPa

173187151

205

75

26359

Knife edgesupport(annealed)20mm

GPa

3-pointbendtest

GPa

155r4164 + 13

166 r 10164r8

177 r.58188r38148 r.7

2520

28

Resonance

GPa

Speedofsound

GPa

Speedofsound(annealed)0.08deviatíonGPa

109

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Table 33 continued

EP 100secEP 7SsecEP 50sec

+25+25+25

EP 25sec+50

EP 50sec+50

EP 25secssso 020

EP 100secEP 75secEP 50secEP 25sec

+25+25+25

EP

018EP

EP 30secssop 01 I

Wre Type

93

24

62

148616897

SlotSupport18.Smm

GPa

133162176160

137r15153183165152152168148179

190r4179194196

KnifeedgeSupport20mm

GPa

116170159158123131127140

176t4

KnifeedgeSupport1Omm

GPa

154r4155r4

154 r 16153r4147 r.1166t23143 r 19

161 r 13

122

Knife edgesupport(annealed)

20mm

GPa

154160150137

149 r 1

3-poíntbendtest

GPa

139 r I

140 r 6143 t 17

149r3

152 r.7

Resonance

GPa

145

Speedofsound

GPa

239 r 38

Speedofsound(annealed)

0,08deviationGPa

110

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Effect of diameter change on elastic modulus values

A comment was made earlier about the effect of wire diameter on elastic

modulus values. To assess this, the wire diameter value was increased

by 2o/o and the elastic modulus values were recalculated without

changing any other parameters. sspp ps 018 wire specimens were

chosen and the wire diameter was increased from 0.45 to O.46mm and

the results are as listed in Table 34.

Table 34: The effect of wire diameter on elast¡c modulus values

The elastic modulus values decreased significantly when the diameter

was marginally increased. The cant¡lever bend test at lOmm appeared to

be most sensitive to diameter change with a 22o/o reduction noted

compared with a 12o/o change noted with the other test methods. This

emphasises the importance of accurately measuring wire diameter'

The effect of data modification on elastic modulus values

The difficulty in selecting the most appropr¡ate tangent to the stress-

strain curve to calculate elastic modulus has been discussed. The effect

of ignoring zero and limiting the data chosen on the accuracy of the line

of best fit, and consequently the elastic modulus values, were assessed.

Load and unload data for an as-received sspp ps 018 wire tested on a

knife edge support at lOmm was modified as can be seen in Tables 35

and 36.

135153Resonance test

130148Three-point bend test

167190Cantilever test 20mm

135173Cantilever test 1Omm

Diameter of O.46mm

GPa

Diameter of 0.¿15mm

GPa

Test

Figures 25 and 26 illustrate the effects of modifying the data.

111

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a

b

o

y = O.I ló32 + O.9Z]7OX R^2 = O.991

2

zao

o

Er(ension (mm)

I=3.4912c-3+ 1.0628x R^2= rl

zdo

o(,

Ertcnsion (mm)

Figure 25: Modification of load data. The first graph shows the slope of

the l¡ne of best fit when all data were ploffed. ln the second graph data is

limited to the first six values.

Lt2

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a2-4{v10rc-2 < O6?485x l{^2 =O-9tì(r

o

zóodð

2€Gocé

zdoa.J

z

o

o

2

o

12

(, l

b

o4 o6 o_a

Extcnsion (mm)

Extcnsion (mm)

0.245?0 . 0.8ó951r R^2 = 0.99)

to r:Ertension (mm)

t = -o.rs222 + 0.77212¡ R^2 =o.s(

(, l

c

08

o.6

o.4

o2.

0-ol4 t6

Figure 26: Modification of untoad data. ln the first graph all data are

plotted. ln the second graph, only eight data po¡nts are plotted and zero

po¡nt is ignored. ln the last graph the slope is calculated from five data

po¡nts only.

Lt3

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o.9990.9950.986UNLOAD

1.000o.991LOAD

R^2 (3)R^2 (21R^2 (11

Table 35: The effect of data modification on the accuracy of the stra¡ght

line fit for a stainless steel premium plus, pulse straightened O'O18" wire'

R^2 indicates the accuracy of the straight line fit to the stress-strain data

plotted. For column 1 all data were plotted. When load data was limited

to six points, a perfect straight line fit was achieved. For the unload data,

a nearly perfect fit of 0.999 was noted when five data points were

plotted and zero ignored.

Table 36: Effect of data modification on elastic modulus values for a

stainless steel premium plus, pulse straightened 0.O18" wire.

Despite modifying the data, only relatively small changes in elastic

modulus values of less than 5% were noted.

E. Microhardness and Macrohardness tests

1. Microhardness

After embedding the sspp 018 wire specimen in Bakelite, it was polished

to a mirror finish, exposing the maximum wire diameter for

microhardness testing. This enabled the microhardness of the wire

surface to be compared with the inner core.

The surface layer of the wire is more heavily cold drawn and therefore

harder. Removal of the surface layer, such as with electropolishing, may

make the wire softer. lf the wire was homogeneous surface layer removal

would not be significant.

103103108UNLOAD

177172LOAD

E

GPa (3)

E

GPa tzt

E

GPa (1)

l14

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Both the diagonal distances of the indentation square were measured

from photomicrographs (magnification 142Oxl in millimetres. An average

of these two distances are listed in Table 37 below according to the

loads used. Values are listed as measured, from one surface across to

the other.

Table 37: Average values of diagonal measurements of microhardness

indentations, in a stainless steel premium plus 0.018" wire.

lf there is a surface difference, due to variation in wire texture (ie a more

heavily cold drawn surface), it must be very small or thin as excluding

the larger values at the edge due to specimen geometry, there were only

minor differences in diagonal dimensions across the wire.

5.75

5.75

10.257.755.75

1075

1075.5

1075.25

107.255.25

9.575.75

9.7575.25

9.575.5

9.756.755.5

9.7575.5

9.756.755

9.2575.25

9.756.755

9.575.5

106.55

106.55.25

10.257.256

50P

mm

25P

mm

BASE LOAD

mm

115

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The measurements were adjusted to allow for the magnification (1'42 x

163¡ used. An average of all the values (excluding the edges) were used

to calculate the Vickers hardness numbers given in Table 38. This varied

between fifteen and seventeen measurements for each'

Table 38: Vickers hardness numbers for a stainless steel prem¡um plus

0.O18" wire.

*Vickers formula as stated in the materials and methods section.* *tables for the determination of Vickersharte with the LEITZ-MIniload

Hardness-Tester.

As the load was increased, from base load to 25P to 5OP, HV increased.

lf these wires do have a more heavily cold worked surface layer, it would

be expected that as the load was increased, HV would decrease. The

rationale for this being that a lighter load would only penetrate the outer

hard surface while a heavier load would penetrate the softer core. The

value of the latter would be an average of the hard outer surface and the

softer core lowering HV. This was not noted.

2. Macrohardness

It proved difficult to position the diamond indentor on the wire specimen

alone. As a consequence bakelite hardness may be being tested rather

than the sta¡n¡ess steel wire. lnit¡ally a 2Okg load was used but only half

the indentation was located across the wire. A 5kg load was used to

indent the specimen at three locations.

The hardness values calculated were 501,753, 516. The middle value of

753 is so different to the other values and should be rejected as a

consequence. The macrohardness values were lower than the

62362312.1850P

5996058.7525P

5845886.88base load

HV

(referenced from

table* *)

HV

(mathematically

calculated*)

¿ (pm)LOAD

116

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microhardness values. This is to be expected ¡f the macrohardness values

are an average of the hard surface layer and softer core.

As a consequence of the curved surface of wires, a small indentor is

probably a more accurate method of calculating the hardness as it would

allow a more planar wire surface to be examined.

F. Surface appearance

a. Surface effects of pulse straightening.

ln premium plus O18 wire, closely spaced striations (S), parallel to the

long axis of the wire, are evident on the surface (Fig. 271. The elongated

grains give a fibrous appearance. which is typical of heavily cold worked

wires. The low temperature stress relieving heat treatment after the final

draw is below the recrystallization temperature so this does not affect

the fibrous appearance. The surface roughness is possibly a function of

die wear.

Differences in the number of striations, height of the ridges and the

presence of porosity and pits, may help to explain the different

mechanical properties (Slngh 1991).

fn the pulse-straightened condition (Fig. 281 there are no significant

differences in the surface of the wire compared w¡th the untreated

premium plus.

b. Surface changes after electropolishing

The surface structure of as-received 020 special plus wire is shown in

Figure 29. Many evenly spaced striations (S) are present throughout the

longitudinal section. The striations are parallel to the wire axis. lndividual

grain boundaries cannot be distinguished because of the large amount of

distortion during the drawing process.

Non metallic inclusions which may impair the mechanical properties of

wires if present would have been drawn to such an extent that they

cannot be detected (Honeycombe 1968 as in Twelftree 19741.

rt7

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-vsC¡ --?-. -j- :=- r-É _ _ <

70pm

Figure 27: Scanning electron micrograph of a longitudinal section of

stainless steel premium plus o.o18" as-received viewed at a

magn¡fication of 75x showing closely spaced striations (S).

fD- 'If

Figure 28: A scanning electron micrograph of a longitudinal section of as-

received stainless steel premium plus pulse straightened o.o18", at a

magnification of 75x.

,a .-\,II

tI t

t

r*'l:r'f.À¡'

Fl

)(t

/.

:lio'i

70pm

118

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69pm

Figure 29: A scann¡ng electron m¡crograph of a longitudinal section of as-

received stainless steer special plus 0.020" at a magnification of 75x

showing many evenly spaced striations (S)'

Figure 30: A scanning electron micrograph of a longitudinal section of as-

received stainless steel special plus 0.020" wire at a magnification of

3OOx showing the striations (S).

This is the same specimen as Figure 29 but at increased magnification.

0.[nn26.1 kU 3.øøEe 6608/øE KÊ

119

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Singh 1991 noted that premium plus O16 ss wire showed less striations

than special plus 02O ss.

At higher magnifications the striations (S) seem to be evenly spaced

although some (wider) gouges are present (Fig. 3Ol. However in this

material hardly any pits are visible.

After electropolishing for 25 seconds these wires have a very different

appearance to that in the as-received state, the surface striations are

only just visible (Fig.31l. This has the potent¡al to reduce friction.

Studies on the effect of electropolishing on friction would be interesting.

After further electropolishing of 25 seconds, no surface striations are

evident (Fig. 321. The surface appears slightly irregular and gives the

impression of very shallow depressions being present, although an

(unidentified) intermittent larger defect can be seen in the centre of the

wire surface.

A long electropolishing time of 150 seconds was used to exaggerate the

effects of electropolishing. This is not a clinically realistic electropolishing

time. No surface striations are present and the surface appears very

smooth excluding a deep gouge (G) possibly placed at the time of

drawing (F¡g. 331. lf the gouge was placed at the time of drawing the

wire appears to be rotated as it is drawn through the die as the scratch is

not parallel to the edges.

At higher magnification it can be seen that the original surface striations

have been removed leaving a very smooth surface excluding the deep

gouges (G) noted above which were not removed by electropolishing

(F¡9. 341.

c. Fractography

Wire surfaces were assessed in the SEM after being deliberately

maltreated to the point of fracture. Examination of the fractured surfaces

enabled the wire cross-section to be examined to locate variation in

texture between the surface and inner core.

r20

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Figure 31: A scanning electron micrograph of a longitudinal section of

stainless steel special plus O.O2O" wire which has been electropolished

tor 25" and viewed at a magnification of 75x'

Figure 32: A scanning electron micrograph of a longitudinal section of

stainless steel special plus O.O2O" wire which has been electropolished

for 5O" and viewed at a magnification of 75x'

72¡tm

l2l

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Figure 33: A scanning electron micrograph of a longitudinal section of

sta¡nless steel special plus O.02O" which has been electropolished for

15O' and viewed at a magnification of 75x. A deep gouge (G) was

noted.

/

Figure 34: A scanning electron micrograph of a longitudinal section of

stainless steel special plus 0.020" which has been electropolished for

150" and viewed a magnification of 300x. A deep gouge (G) was noted.

This is the same specimen as Figure 33 but at increased magnification'

t22

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The number of bends required before the point of fracture were recorded

and this data is graphically illustrated (Fig. 35).

BEND UNTIL FRACTURE TEST

Figure 35: Number of bends required before point of fracture.

30

25

20

NUMBER OF BENDS 15

10

Emeanhlgh

_to*

o

l)12.tPP

o14t3PP

016rsPp

016ppps

o18ttPp

016ntsc

o20nt!c

018 016ppps nl

018 x O215x026 024ntsc ntsê

WIRE TYPE

The nickel-titanium wires could w¡thstand many more bends prior to

fracture than stainless steel wires.

After fracture the wires were assessed in the SEM. Photomicrographs

were recorded and ED analysis performed to allow the chemical structure

to be assessed.

The extreme loading condit¡ons applied by reverse bending produced

generally consistent fractures, typified by the formation of "tags" (Fig.

36). The only minor var¡ations noted were in the extent of the "tags"

(Figs. 37 and 38).

At higher magnifications, some differences in fracture behaviour can be

seen. ln Figure 39, the fracture surface appears relatively uniform with

only a gradual change in direction of the crack growth path from almost

normal to the surface (at A) to parallel to the axis (at B) where the fibres

appear to be parallel to wire axis probably due to elongated grains

produced in wire drawing. Distinct steps are also visible on the fracture

surface (at C) which are often clearly associated with similar features at

123

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Figure 36: A scanning electron micrograph of a deliberately fractured

stainless steel premium plus O.O18" wire surface showing "tag"

formation.

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Figures g7 and 38: Scanning electron micrographs of the fractured

surfaces of deliberately maltreated stainless steel premium plus O'O18"

wires showing variation in the extent of "tag" formation.

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._:_-

Figure 39: A scanning electron micrograph of a fractured wire surface at

higher magnif¡cation. The direction of the crack path appears normal to

the surface at (A) while at (B) it appears parallel to the axis'

Figure 40: A scanning electron micrograph of a fractured wire surface.

Distinct steps (C) are visible on the surface'

BlmmZSBl.r.r t!'JIE:' f.1 Uril ,.1 '' r;- - -

t26

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the wire surface (Fig. a0) and represent ¡ncremental changes in the plane

of the crack. However in another sample (Fig.41), there is a clearly

different zone (at D) normal to the wire surface, or even inclined in the

opposite direction to the "tag". The remaining surface area of the

fracture surface is similar to that described above. A similar fracture can

be seen in Figure 42, but here the two zones are separated by a

pronounced crack (at E). Another photomicrograph (Fig. 43), shows that

these central cracks can grow in a steplike manner to produce the step

features noted in all the "tag" samples.

At even higher magnifications, the fracture surfaces again appeared

largely similar. ln the "tag" areas, fractures were generally associated

with the heavily elongated grains (at F) produced in the manufacturing

process for the wire (Fig. 441. However other areas exhibited regions of

fine flat dimples (at H), typical of ductile fracture {F¡9. a5l. Both these

features are characteristic of ductile failure in drawn wires, for which the

formability has been almost exhausted during manufacture. This type of

fracture is known as fibrous fracture.

The scanning electron micrographs included are typical of many fractured

samples viewed with l¡ttle difference being noted between samples'

However few conclusions can be drawn, other than that the failures are

typical of the material.

Microanalysis of the sample in Figure 42 showed that it contained iron,

chromium and nickel (Fig. 46), as expected with no major impurities

which might influence properties or fracture.

G. Detailed microstructural data

Most authors support the concept that advances in testing and

developing orthodontic wires would be gained ¡f microstructure were

correlated with mechanical properties (Williams and VON Fraunhoffer

1971 as in Twelftree 1974l..

TEM studies would reveal detail of the wire structure by allowing the fine

granular structure to be assessed. Different phases (matrix or

tn

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I r1r'

r-

o

P] I rn rn - r"-t;'-' = a"tF

I

Figure 41: A scanning electron m¡crograph of a fractured wire surface

illustrating a zone normal, or even inclined in the opposite direction (D).

Figure 42: A scann¡ng electron micrograph of a fractured wire surface

where a pronounced Crack (E) separating a "tag" and zone normal to the

wire surface, or even inclined away from the "tag"'

o.1nm2B.6 kU 1.58E2 BBBI J L_ì!ì Þ_-,

?

-

{{l

\-

@

.4

a/

I

i

-

i-

128

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Ê1mm1'f-l' fr

l-tà'2

\-i

-)

ãÞ

\

f

¿-

t\

---T'r-')

- - - .1--t

Figure 43: A scann¡ng electron m¡crograph of a fractured wire surface

showing the steplike growth of a central crack'

Figure 44 A scann¡ng electron micrograph of a

magnification showing the elongated grains (F).

at higher

ð

t

"tag"

- -I E um3E I t'

-: þi iF ; s:1 Llri ; ¡1 -

129

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æ1

1.

t-

:fl\

\

\

\r.

I

\,a'-

a

.a

),i { I .1+. rl'

!

Figure 45: A scanning electron micrograph of a fractured wire surface at

high magnif¡cation showing fine flat dimples (H) typical of ductile

f racture.

rl E H I'l =. F Ur'i c,+ F¡¡elEiae Pr,i I rf¡s 5ur= :'1r-¡¡l :<:1-l'ìlìY-E=:

Cut'sol^: Ø.@@ØKeV = Ø RÖI (3:i cl €rqlo: l¿.ØØØ

I-..

-' - Fq,qcTi iÊE StlFFFllE ': '-trr TT; :Þ1TTË

tili!

:

;l

:!.'..:-...i

:l

ø taulo

lElA

VF5 = 4O96 LØ.?4ø

Figure 46: A printout of the EDS analysis of sta¡nless steel wire showing

the presence of iron, chromium and nickel'

130

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prec¡p¡tate), ¡mpurities and defects or heavily deformed regions may be

revealed

The preparation of thin 3mm foils for TEM assessment is not easy due to

the small diameter of the wires. One way of overcoming this was to

prepare the fo¡ls from wires of larger diameter. Although the structure

could be assessed the effects of cold drawing would not be present

(Singh 1991).

Several different techniques were pursued to produce suitable TEM foils

of the wires in cross section as discussed in the materials and methods

section, but unfortunately none were successful.

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CHAPTER 6coNcLUsroNs

A knowledge of the mechanical properties of orthodontic wires isimportant as it enables the most appropriate archwire for a given clinical

situation to be selected and assists with the development of newer

improved wires. A variety of different properties were tested in the as-

received state and after manipulative treatment.

Stainless steel wires were predominantly tested, as despite their long

history of use, fundamental questions remain about their mechanical

properties.

The stiffness of an archwire is considered to be one of its most important

propert¡es. Stiffness determines the force delivered by an appliance. ln

general a low, continuous force is thought to be most desirable, to

achieve maximum tooth movement with minimum patient discomfort.

The stiffness of a wire is proportional to the elastic modulus. Despite the

use of an extensometer, elastic modulus results from tensile tests by

previous authors have been lower than textbook quoted values. An

alternative testing technique was used to assess the elastic modulus for

this reason and the fact that orthodontists primarily stress wire in

bending not tensile direction.

Bend tests were first performed on wire specimens shaped into an

archform to mimic the clinical situation more closely. Only the slopes of

the stress-strain curves could be compared as actual elastic modulus

values were not calculated due to the complexity of the mathematics.

The range of values for the slopes varied for different diameter wires:

some exhibiting almost constant values while others showed large

variations up to 9 times.

To enable elastic modulus values to be calculated, short lengths of wire

were tested in a cantilever or 3-point bend test. Bend tests using a

slotted support produced very low elastic modulus values which had to

be discarded. The low values may be explained by friction between the

archw¡re and support. A knife edge support was used as an alternative.

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Although elastic modulus values were increased they were still low when

compared to the textbook quoted values.

Less conventional test methods of resonance and the speed of sound

were also used to determine the elastic modulus. Despite using these

alternative techniques it was stilt proving difficult to produce a consistent

elastic modulus value. lt appears that determining the mechanical

properties of fine orthodontic wires is not easy.

The influence of wire diameter on elastic modulus values was assessed.

Diameter is critical when calculating elastic modulus for mechanical and

resonance tests where d is used to the fourth power. A 2o/o error in

diameter changed the elastic modulus values between 12 and 22o/". The

speed of sound test method avoids this source of error as wire diameter

is not used to calculate the elastic modulus value.

A comment had been made by an experienced clinician that

electropolishing appeared to affect the stiffness of an archwire. Wires

were tested in the as-received state and after electropolishing. No

particular pattern could be established between electropolishing and

elastic modulus value.

Orthodontic wire surfaces were assessed in the SEM in the as-received

state and after electropolishing. Wires in the as-received state had a

fibrous appearance due to the elongated crystals which is typical of a

heavily cold worked wire. As the wires were electropolished for longer

periods of time, the wire surface appeared smoother and smoother.

Although surface striations were removed, deep gouges probably

produced during the drawing process, remained.

It was proposed that orthodontic wires may exhibit anisotropic

behaviour. Wires were annealed to reduce the anisotropic effect and then

tested in the hope that elastic modulus values closer to textbook quoted

values may be achieved. Elastic modulus values were calculated from the

load data as the unload values were limited and extremely low. This may

be explained by the reduced springback of annealed wires. The effect of

annealing on elastic modulus values was not consistent with values for

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O16 and O18 sta¡nless steel wires decreasing while for O2O wires

increasing.

Wires were deliberately maltreated to the point of fracture and then the

fractured surfaces were assessed in the SEM. This was to assess for

textural differences between the wire surface and inner core. The wires

exhibited a ductile fibrous fracture but no significant textural differences

were noted.

Microhardness tests were also performed across the diameter of an

embedded and polished wire. lf there are differences between the surface

layers and inner core they must be small as no variation was noted when

HV was calculated.

Although wires may be selected according to their mechanical properties,

it is the microstructure and in turn the chemical composition and

thermomechanical treatment during manufacture that determines these

properties. TEM studies are the only method of examining in detail the

internal structure. Foil preparation was difficult and time consuming and

despite many different techniques being trialled, no successful foils were

produced. Microstructural assessment would improve our understanding

of mechanical properties and assist in the development of new improved

materials.

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CHAPTER 7

FUTURE RESEARCH

1. Further tensite tests on orthodontic wires should be performed using

accurate calibrated load cells w¡th extensometers and a large number of

accurate determinations of wire diameter to provide a good average'

2. Most tests reported in the literature use stra¡ght lengths of wire when

determining the elastic modulus. Brantley (1978) (in lngram et al, 1986)

used beam theory technique, to show results for the measurement of

varying lengths of the same material which gave elastic modulus values

that differed by more than l}Oo/o between half, one and two inch

specimens. This should be investigated in more detail.

3. The formula being used to calculate elastic modulus values from

tensile and bend tests may not be appropriate for orthodontic wires due

to their small diameters. This should be investigated.

4. Refining the velocity of sound technique by using a Square wave form'

may assist with accurate identification of the same reference point on the

two wave forms.

5. An article in "Materials Forum" (Bell et al 1993), discussed a new

method of determining hardness and elastic modulus values of thin films

and cross-section using an ultramicroindentat¡on system. This alternative

method of test¡ng the micromechanical properties would provide

additional data for comParison.

6. lf stiffness changes are noted after electropolishing, it may be the

result of precipitate formation (eg hydride formation) or the removal of an

oxygen embrittled or work hardened surface layer. This would need to be

investigated with quantitative and qualitative element identification in the

TEM.

7. The wire surface appeared smoother after electropolishing. This has

the potential effect of reducing friction. Frictional studies should be done.

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B. Testing should be extended to include other tests to provide additional

mechanical data such as proport¡onal limit, elastic limit, yield point'

tensile strength, proof stress, ductility, resilience and toughness'

9. Alpha-titanium has been reported to become brittle after being placed

in the oral environment. Such wires should be tested before and after

exposure to an oral environment to assess for changes in the mechanical

properties.

10. TEM on wires to determine the microstructure in cross-section.

Findings from these tests may explain some of the tensile/bend test

findings.

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