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STRUCTURE AND PROPERTIES OF SPUTTERED ZnO TRANSDUCERS Aly Hassan Fahmy 1 B.Sc. (Eng.) 1 (Cairo Univ.)

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Page 1: STRUCTURE AND PROPERTIES OF SPUTTERED ZnO TRANSDUCERSdigitool.library.mcgill.ca/thesisfile47721.pdf · STRUCTURE AND PROPERTIES OF SPUTTERED ZnO TRANSDUCERS ... Basic Equations The

STRUCTURE AND PROPERTIES OF SPUTTERED ZnO TRANSDUCERS

Aly Hassan Fahmy 1 B.Sc. (Eng.) 1 (Cairo Univ.)

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STRUCTURE AND PROPERTIES OF SPUTTERED

ZINC-OXIDE TRANSDUCERS

by

Aly Hassan Fahmy, B. Sc. (Eng.), (Coiro Univ.)

A thesis submitted to the Faculty of Graduate Studies and Research

in portial fulfillment of the requirements for the degree of

Master of Engineering.

DeflOrtment ci Electrical Engineering,

McGi11 University,

Montreal, Canada.

March, 1971.

o .;ly Ha~sar. Fah:Dy lm

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ABSTRACT

A technique has been perfected for depositing epitaxial Zinc-Oxide

films on c - axis oriented sapphire by R F sputtering of the compound in a reactive

atmosphere. The fi Ims produced are evaluated with regard to their use as ultrasonic

transducers at microwave frequencies. To include the effect of the metal electrode

layers in evaluating the performance of these transducers, a computational algorithm

has been developed for calculating the response of multilayer transducer structures which

also takes into account the effects of finite film resistivity and contact resistance. The

computed response is fitted to the measured data using a simple least squares procedure

in order to obtain the effective electromechanical coupl ing constant of the transducer.

It is demonstrated that films can be obtained which have an effective electromechanical

coupling factor of 0.25, very close to the bulk value of 0.28.

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ACKNOWLEDGEMENTS

The author wishes to acknowledge his gratitude to Dr. E. L. Adler

for his valuable help and guidance.

i i

Many persons aided in the preparation of this thesis. Discussions with

Messrs. R. Mildenberger and P. Ramakrishna were particularly rewarding. Mr. J. Foldvari

has contributed in innumerable ways. 1 am also grateful to Mrs. P. Hyland for on ex­

cellent typing job of a for from clear manuscript.

Thanks are also due to the Defence Research Board of Canada for financial

support (Grant 5525-07) and to Coiro University for granting the author leave of absence.

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i i i

TABLE OF CONTENTS

A BSTRACT

ACKNOWLEDGEMENTS ii

TABLE OF CONTENTS iii

CHAPTER INTRODUCTION

CHAPTER

CHAPTER

CHAPTER

Il

2. 1 2.2 2.3 2.4 2.4 .1 2.5 2.6 2.7 2.8

III

3.1 3.2 3.3

3.3.1 3.3.2 3.3.3

IV

4.1 4.2 4.2.1 4.2.2 4.3 4.3.1 4.3.2 4.3.3 4.4 4.4.1

PERFORMANCE OF MULTILAYER PIEZOELECTRIC TRANSDUCERS

Introduction Basic Equations The Multi layer Structure Problem Acoustic Power Generation Input Impedance and Transducer Loss Acoustic Power Detection The Non-Conducting Case Computer Program Computed Resu Its

R F SPUTTERING OF ZINC-OXIDE TRANSDUCERS

Introduction Sputtering of Zinc-Oxide Factors Affecting the Fabrication of ZnO Transducers Factors Pertaining to the Sputtering Station Factors Pertaining to the Substrate Independent Factors

TRANSDUCER FABRICATION

Introduction Experimental Sputtering Facility Main Vacuum System Instrumentation Pre 1 iminary Experiments Metallic Films Temperature Rise due to Sputtering Effect of R F Power on Deposition Rate Transducer Fabrication Procedure Cleaning Procedure

4

4 6

10 12 14 15 17 17 18

26

26 27

27 28 31 32

37

37 37 37 39 43 44 45 47 49 49

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CHAPTER

CHAPTER

CHAPTER

APPENDIX

REFERENCES

4.4.2 4.4.3 4.4.4 4.4.5

V

5.1 5.2 5.2.1 5.2.2 5.2.3 5.3

5.3.1 5.3.2 5.3.3 5.3.4 5.3.5

VI

6.1 6.2 6.3 6.4 6.5 6.6 6.7 6.8

6.9 6.10 6.11

VII

DepCNitic~ of Beck Electrode Deposition of the ZnO Fi lm Deposition of the Top Electrode Chemical Etching of ZnO

TESTING OF THE TRANSDUCERS

Introduction Structure Analysis .. General Formulae Governing RED The Zinc-Oxide Structure Experimental Set-up and Procedure Evaluation of the Electrical Performance of the Tran:;ducer Overall Trnasducer Loss De 1 ay Rod Losses Delay Rod Holder Conjugate Matched Transducer Loss Untuned Transducer Loss

EXPERIMENTAL RESUL TS

Introduction Temperature and Deposition Rate

. Effect of Pressure Effect of Gas Composition Rate-Temperature Survey at 10 % Oxygen Crystal Size and C-axis Spread Input Impedance Effective Coupling Constant and Contact Resistance Post-Deposition Treatment Adhesion Reliability and Reproducibility

SUMMARY AND CONCLUSIONS

COMPUTER LISTING

iv

50 51 51 51

53

53 53 54 56 58

60 62 63 65 66 69

71

71 71 75 79 80 84 84

86 88 89 90

96

98

104

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CHAPT ER 1

INTRODUCTION

ln the last decade, several techniques for obtaining piezoelectric thin

1-6 film transducers have been developed. The versatility of these transducers is demon-

strated by their use in a variety of applications su ch as non-destructive testing, low loss

delay lines, acoustic resonators and the processing of complex micraovave Signais?

The thin films used are primarily made of high gap semi-conducting com-

pounds such as CdS, CdSe, ZnS and ZnO. These materials have high crystallographic

symmetry and con be deposited as highly oriented thin films on a variety of substrates.

Other materials, both chemically and crystallographically more complex thon the simple

binary compounds, have also been used, such as L i Ga O2

and LiN b 03

.8

For microwave acoustic transducers in delay lines applications, a material

with high piezoelectric coupling coefficient, K .. , is required.6

The semiconducting •

material with the highest known value of Kt for compressional waves is zinc-oxide, having

a value of 0.28.

Techniques for obtaining thin ZnO films are numerous and have been in-

. d b h b 9 3,5 d R .10,11 h de vestlgate y many researc ers. Den urg, Foster an ozgonyl ove ma

ZnO transducers by D C sputtering of the compound. Wanuga 12 experimented by re­

active sputtering of zinc in a mixture of argon and oxygen. Raimondi and Kay 13 obtained

high resistivity transparent ZnO thin films both by reactive D C sputtering of metallic

zinc and R F sputtering of ZnO . Reactive evaporation of zinc in an oxygen beam is

another technique used by de Klerk 6

and Malbon .14 Ohishi et 0115 successfully produced

ZnO films at low tempe ratures by the oxidotion of vacuum deposited Zn Se films.

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2

Although the techniques for preparing the ZnO films are weil advanced,

little work has been done to corre lote the crystallographic structure of the thin film pro-

duced to the different parameters controlling the process of fabrication, and to the actual

performance of the film as an ultrasonic transducer. 6

Recently, de Klerk obtained single

crystal films by reactive evaporation on a substrate cooled to -lSOoC. Rozgonyi and

Polito 11 obtained epitaxial films of ZnO on (001) single crystal sopphire and c - axis

oriented CdS. However, the structure of the films was sometimes "random polycrystalline

or poorly oriented tt• The authors attributed this fact to changes and modifications brought

to the vacuum system prior to the fabrication of the se films. The sorne result was concluded

by Foster et al for the fabrication of ZnO films by D C sputtering3

and by triode sputter-

• 16 mg.

ln this thesis a study is made of the various parameters affecting the produc-

tion of ZnO films by R F diode sputtering of the compound in a reactive atmosphere.

ln Chapter Il, the frequency response of a multilayer semiconducting piezo-

electric transducer is obtained algorithmically. The multilayer transducer is first reduced

to a conventional three-port structure by defining recursively the mechanical impedance

loading each face of the piezoelectric layer. Electromechanical power conversion theory is

then used to obtain the transducer loss.

Chapter III presents a brief summary of sorne general concepts of R F

sputtering in relation to the formation of ZnO thin films.

The experimental method used for the fabrication of the transducers is

described in de ta il in Chopter IV, while the methods used for both structure analysis and

electrical testing are discussed in Chapter V .

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Finally in Chapter VI, the results obtained frorn experiments carried out

according to the methods outlined in the earlier chapters are presented and discussed. Some

results of experiments on post-deposition heat treatment, film adhesion, as weil as sorne re­

producibility tests are also described in this chapter.

ln summary, this thesis relates the fabrication procedure of zinc-oxide thin

films to their crystolline structure and their performance as microwave ultrasonic transducers,

and defines the guide lines to be followed for successfully depositing efficient transducers.

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CHAPTER Il

PERFORMANCE OF MULTILAYER PIEZOELECTRIC TRANSDUCERS

2. 1 Introduction

The launching of plane acoustic waves into a certain medium by compo-

site layered transducers composed of a piezœlectric semiconducting thin film and other

lossless loyers has been extensively discussed in the recent literature .17,18,19

The coaxial geometry shown in Figure 2.1 is a typical one used in most

experimental and analytical studies. The top layer (s) - normally only one - preceding

the transducer is a metallic contact to which the electrical signal is applied. The trans-

ducer is followed by another metallic layer (second electrical terminal) and other layers

TOP ELECTRODE

PIEZOELECTRIC LAYER

BACK ELECTRODE

DELAY ROD

ADDITIONAL LAYERS

FIGURE 2.1. MULTILAYER TRANSDUCER STRUCTURE.

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acting os a mechanical transformer to achieve sorne prescribed behaviour such os matching

to the de lay rod impedance. 19

For a theoretical treatment, a weil justified assumption Is that the

lateral dimensions of the structure ore large cornpared to the acoustic wavelength ; this

effectively reduces the problem to one dimension. Another assumption which is only

theoretically feasible, is that the crystal orientation of the piezoelectric layer is properly

chosen so that only one pure mode of vibration is excited.

To the author's knowledge, two approoches ore presently used for the

evaluation of the frequency response of the transducer. The first approoch starts from

the piezoelectric equations of state, Moxwelt's equations and Newton's equation of

motion, and works out the solution os an electrornechanical problem assuming a finite

. .. f h . d . • 1· • 1 20,21,22 reslstlvlty 0 t e semlcon uctrng plezoe ectrrc materra • the second approoch

23 is bosed on using an electric circuit model (known os "Mason circuit" after W. P. Mason )

f h . 1 1 h' h be . 1 d 17,18,24 Ith h h or t e plezoe ectric ayer. T IS as en extensIve y use • A oug t ere is

no basic difference in the computational wak between the two approoches, the first one

has the advantage of keeping the physical arguments of the problem, making it possible

to take the loss of the piezoelectric material into account and to handle "active" semi-

conducting films.

ln the following anolysis, the solution for "transducer loss" os obtained

previously for a piezoelectric film looded at one face bya hypothetical lood,22 is ex-

tended to multilayer structures looded at bath faces by real mechanical loods. First, the

case of a finite resistivity semiconducting piezoelectric thin film is considered. The case

of infinitely high resitivity is then approoched as a simplification of the more general case.

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2.2 Basic Equations

For piezoelectric materials, which may also be semiconducting, the thermo-

dynamical equations of state are:

T c c 5 - e E 2. 1

2.2

where T and 5 are the stress and strain, 0 and Ethe electric displacement and field,

c the elastic stiffness tensor at constant field, Ethe electric permittivity tensor at constant

strain, and e the piezoelectric tensor. The assumptions of a one dimensional problem and

single mode of vibration (compressional or longitudinal) makes the variables in Equations

2. 1 and 2.2 sca lors, wi th the proper choice of the tensor e lements for c, e and E.

Consider plane waves of the form U • exp (i k x - i w t) where U is the_ ampl itude of

the displacement and x is the distance measured along the transducer axis toward the delay

rod (Figure 2.1). The above equations, together with Maxwell's equations, charge trans-

port equation and the equation of motion result in a quartic dispersion relation, k (w), in

20 the complex wave vector k.

where

With a little manipulation, this quartic can be written as :

w z = VT

s

z +

+ i ( wc) • z2 '. (z2 - 1) = 0 w

a dimensionless function of the wave vector,

2.3

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2 e

s = e c

the square of the electromechanical coupling 2

constant (usually referred to as kt) ,

V D = - ~ EDe electron drift velocity in the presence of a

D e field, EDe '

W = c

wD

=

and v = s

ale

the conductivity and diffusion frequencies,2° and

v the longitudinal velocity of sound at constant s

field. Wc ' wD and Vs are related to the

physical constants as follows :

y2 ID s e

(clp) 1~

where a , De and p are the conductivity, diffusion constant for electrons, and mass

density respectively.

7

The solution to this quartic yields four allowed waves characterized by the

wave vectors k., i = l, 2, 3, 4 ; or alternatively z., i = l, 2, 3, 4. In 1 1

general, z. is a complex number causing k. to be complex of the form (101 1 v. - i a.) 1 1 1 1

where v. is the phase velocity of this porticular wave and a. an attenuation constant 1 1

associated with the space propagation of the wave. ( a. being positive for a wave at-1

tenuated as it advances in the positive x-axis direction).

For a finite piezoelectric film of thickness L and driven byan a c field

E , all four waves will be present. Following the derivation given in Reference 21, one o

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ends up with expressions for the velocity, stress and electric field along the trans-

ducer * :

e E 0 [ Q. (ik-x)J v = ......- . exp

p Vs 1 1 2.4

T = e E . [ - 1 - Q. z. exp ( i k. x) ] 0 1 1 1

2.5

E = E . [ 1 + Q. (z. - 1 / z. ) . exp ( i k. x) ] 0 1 1 1 1

2.6

where ( pVs

) is the mechanical characteristic impedance of the piezoelectric material

and Q., i = l, 2, 3, 4 a set of amplitude ratios that depend on boundary conditions. 1

The time dependence exp ( - i Ct.) t) is implicit in the above equations. The voltage across

the transducer faces is then directly calculated :

E dx = EL o

[l-iQ. Ct.)o (i-l)'{exp(ik.L)-l}J 1 11 Ct.) 1 1

while the current flowing is given by

= E A E (Ct.) - i Ct.)) which con be rewritten o c

2.7

* The convention that repeated subscripts represents summation is used in the

rest d this work.

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Ca) - i Ca)

= Ca) (EA)'E L • [_c __ J o L 0 Ca)

2.8 o

where A is the "acoustic beam cross-sectional area (defined by the top metal electrode)

and Ca) the angular frequency at which the length, L, is a half wavelength. o

For both machine computation and mathematical manipulation, it is useful

at this point to introduce the concept of normalization - while keeping the seme notations

for the normalized values:

v = Q. exp ( i k. x) 2.9 1 1

T = - 1 - Q. z. exp ( i k. x ) 2.10 1 1 1

E = 1 + Q. (z. - 1 / z. ) exp (i k. x) 2.11 1 1 1 1

Ca) 2

. { exp ( i kj L) 1} V 1 . Q 0 - 1 ) 2.12 = - 1 .- ( z. -11I'c.J 1

= (Ca) - i Ca) / c.J 2.13 c 0

It is now clear that Q. is a set of normalized velocities while z. is the corresponding set 1 1

of normalized mechanical impedances.

The normalizing electrical and mechanical impedances are

the magnitude of the transducer clamped reactance at f - and o

[ 1 ] 1

Ca) ( E A) o L

Z op

the piezoelectric material mechanical characteristic impedance. These normal izing factors

are functions only of the piezoelectric material and the geometry of the transducer .

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2.3 The Mu 1 tilayer Structvre Problem

Referring to Figure 2.2 (a), showing a structure of N fi Ims on the top

of a delay rod of mechanical impedance ZDR' and with the free face loaded byan

impedance Z A (usuaHy set to zero) ; for each fi lm (n) we know the length, Ln'

sound velocity, v , and the mechanical characteristic impedance, Z sn on

The piezo-

electric layer is one of these films, e.g. number p •

PIEZOELECTRIC LAYER

.....,..---'-~ - - - - - ....... --,.-------4

2 P N DELAY ROD

ZON ZDR ZA Zol Z02 - - - Z op

~ ~ ~ 1+- ~ z zl z2 z z

p+l 0 P -1

(a)

(b)

FIGURE 2.2. (a) MULTILAYER STRUCTURE

(b) EQUIVALENT 3 - PORT.

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1 1

A basic and justifiable assumption is that the acoustic loss in the coupling

layers is small and may be neglected.17

The boundary conditions which must be satisfied

at each interface are the continuity of stress and velocity in both media. Therefore, as

shown in Figure 2.2 (b), the acoustic impedances ZL and ZR which are the actual loads

on the "Ieft" and "right" of the transducer can be obtained by applying the principle of

travelling waves in lossless media .19 Defining 9 n

= wL

n v

sn of the n th film, we obtain

ZL = Z P - 1

with zp _ 1 defined by the recursive relation:

z = Z n on

z 1 + i Z tan 9 n- on n

Z + i z 1 tan 9 on n- n

where n = 1,2, .... , p-1

and

Similarly,

ZR = zp + 1

with

z defined by the recursive relation p + 1

the angular or radian length

2.14

2.14 (a)

2.15

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z n+1

+ iZ tan 9 Z

on n z = i z 1 tan 9 n on Z +

on n+ n .2.15 (a)

where n = N, N - 1, ..... p + 1

and zN+1 - ZOR·

For a computational interpretation, the reader is referred to the computer listing -

Appendix 1. Equations 2.14 and 2.15, effectively reduce the multilayer structure to

the conventional single layer transducer loaded on each surface as shown in Figure 2.2.

2.4 Acoustic Power Generation

and

ln this case, the mechanical boundary conditions become :

T (0) =

T (L ) =

ZL • v (0 )

-Z ·v(L) R

Substituting for v and T from Equations 2.9 and 2. 10 we obtain

and

1 + Q. (z. - ZR) . exp ( i k. L) = 0 1 1 1

( = 1, 2, 3, 4 and the summoti on conventi on i s understood).

2.16

2.17

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Two additional boundary conditions are required to obtain the four amplitude ratios Q .• 1

We examine the following possible Hreasonable tt boundary conditions: the plane wave

component of either the spa ce charge, the current density or the electric fie Id is made to

vanish at both ends of the transducer. Such choices may be thought of as defining an

ideal metallic contact.25

(a) Setting the current density equal to zero:

2 Q. (1 + s - z.) / z. = 0

1 1 1

2.18 (a)

Q. (1 + s - l) . exp (i k. L) / z. = 0 1 1 1 1

(b) Setting the space charge equal to zero:

2 2 Q. (1 +s -z.)/z. = 0

1 1 1

2.18(b)

2 exp (i k. L) / i 0 Q. (1 + s - z. ) =

1 1 1 1

(c) Setting the electric field equal ta zero

2 = 0 Q. (1 - z.) / z. 1 1 1

2.18 (c)

Q. 2

• exp (i k. L) / z. 0 (1 - z.) = 1 1 1 1

Only one pair ~ Equations 2~18 is required for the solution. While they 011 seem reasCYloble,

computations show negligible differences between the results obtained using sets a and b,

while the electric field assumptions yield slightly different results as will be shown later.

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2.4 .. 1 Input hnpedëmce and Transducer Loss

Now that the boundary conditions are formulated, Equations 2. 16 to 2. 18

can be solved for the amplitude ratios Q. and by bock substitution into Equations 2.9 , 1

2.10 and 2.12, v, T and V are defined. The electrical input impedance of the trans-

ducer will then be 11" :'

z = V /1 e

Up to this point, only the lIintrinsic transducer· has been considered. In

practi ce 1 the contact to the top e lectrode may i ncl ude a series resistance, r , wh i ch may c

not be negligible compared to the input impedance .24 If the transducer is driven from a

source of internai impedance Z , the electrical port "mismatch loss·26 is: s

L ( E) = 4 Re [Z + r ] . Re [Z ]

e c s

Z + r e c

The voltage across the extrinsic terminais of the transducer is

VI = V + 1 r c

Therefore, the electrical and mechanical pa.vers are given by :

P ( E) = 1 / 2 • R e (VI • 1 * )

"

+ Since the time dependence ci the plane waves is assumed exp ( - i w t), the elec­

trical impedances will be Z (- i w), i.e., a positive reactonce is a Copacitive

Load.

2.19

2.20

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and

P ( M) = 1 /2 Re (- T R • vR*) 2.21

ln Equation 2.21 TRond vR

are the stress and velocity at the r. h. s. of the transducer.

P (M) is therefore the mechanical power intensity fed to ZR and delivered through the

lossless coupling films to the delay rode The power absorbed by ZL (in case Re (ZA):j 0)

is radiated at the free face of the device and presents a loss factor.

The actual "generation" conversion efficiency is :

11(G)= 5 p (M)

P ( E )

The term 5 /1f appearing in this equation is due to the normalizing factors carried along

the derivation.

2.22

The transducer loss defined as the ratio of the net power delivered to the load to the avai lable

power from the generator, is then :

TL (G) = L(E)' 11(G) 2.23

2.5 Acoustic Power Detection

ln this case, the generator - the deloy rod - suppl ies the transducer with

the mechanical power through the coupling films. The conversion to electrical power parallels

in 011 respects the acoustic power generation presented in the previous section. However,

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since the acoustoelectric interactions due to drifted carriers are being taken into account,

the transducer 1055 in this case will differ from that obtained above.

To solve for this case we look again for the proper boundary conditions.

Those given in Equations 2.16 and 2.18 still apply, while the one given in Equation 2.17

is no longer applicable. Instead, one can state the condition on the voltage at the intrinsic

terminais as :

V= -1 (Z +r) 5 c

or fr~ 2.12

la) i Q. ~ ( z~ - 1) . [exp (i k. L) - 1 ] = 1 + 1 (Z + r )

Inla) 1 1 5 C 2.24

Again, 50lving Equations 2.16, 2.18 and 2.24, and bock substituting into Equations 2.9

and 2.10, v and Tare obtained. The mechanical input impedance, mismatch 1055, volt-

age output, conversion efficiency and detection transducer 1055 are respectively :

=

L (M) =

VI =

17(0) =

TR

/ v R

4 Re [Z M] . Re [ZR]

1 ZM + ZR 12

-IZ

.. 5

5

P (E ) P (M)

2.25

2.26

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and

TL(D) = L(M)· 11(D) 2.27

where P ( E) and P ( M) are obta i ned by proper substi tuti on in Equations 2.20 and

2.21 .

2.6 The Non-conducting Case

ln the case of a high resistivity piezoelectric thin film or at frequencies

much ,higher than thec6ncNotlvifyJre.que,I'I,CY, one. .. con n'egj~c:t the ,conduction and diffusion

of the carries in the material. Equation 2.3 reduces in such a case to a quadratic giving :

z. 1

= :: (1 + s) 1/2 = l, 2

These roots correspond to the piezoe lectric stiffened conditions. The set Q. also re­l

duces to a set d two amplitude ratios Ql and Q2. Equations 2.16 and 2.17 are

now sufficient in themselves for the complete solution and no additional boundary condi-

tions are needed. Further, the conditions for reciprocity are satisfied and the solution for

either the acoustic power generation or detection is sufficient.

2.7 Computer Program

A computer program has heeA .... rif*en-Gnd used to solve for the transducer

loss at any given frequency. This program is able to handle the different boundary condi-

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18

tions given in Equations 2.18, as weil as different conditions for the input impedance tuning

which can be either "conjugate match ", ··series tuned", "shunt tuned" or "untunedll .22

The conjugate match case is when the source impedance is the conjugate

of the extrinsic input impedance of the transducer at each frequency. This can be achieved

b b • b h f • h'" 27 F • 1 • of • Y stu tunlng or y t e use 0 an active matc Ing circUit. rom a prachca pOint Vlew,

the conjugate match is only possible in an experimental set up.

ln the series tuned case, the source impedance has a reactive element

selected to tune out the input reactance of the transducer at a predefined frequency. The

real part of the source impedance is a fixed value. (e.g. the characteristic impedance of

the r f coupling lines).

The shunt tuning is similar to the series tuning but with the reactive element

connected in shunt with the transducer input. In the untuned case, the transducer is directly

connected to a source of a fixed impedance, usually the characteristic impedance of the

circuit.

The computer listing included in Appendix 1 shows the main features of this

program which displays the frequency response of the given transducer in different ranges of

other variables.

2.8 Computed Results

To illustrate the effect of the different conditions discussed above, the loss

of a multilayer transducer with zinc-oxide as the piezoelectric material, (k = 0.28), has t

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19

been computed over the frequency range 0.5 - 3 GHz. The results obtained are

shown in Figures 2.3 to 2.11.

Solutions using the various boundary conditions discussed in Secti on 2.4.1,

ore shown in Figure 2.3. The space charge and cur.re.ntdensity assumptions yield practically

the sa me transducer loss. The assumption of zero plane wave components for the e lectri c

field at the boundaries, yields results with negligible differences over most of the frequency

bond. However, the validity of this assumption is in doubt, especially since calculations

predict "transducer gain" and "bonds of instability" which ore facts associated with high

carriers drift velocities,22 whereas the drift velocity is zero in these calculations.

ln Figure 2.4, the 2-wave solution - neglecting the conductivity -

is shown together with the frequency responses of a high conductivity and a low conductivity

zinc-oxide film. The structure of the transducer is similor to that shown in Figure 2.3. The

results indicate that the simplifying assumption of infinite resistivity con be used when the

zinc-oxide film resistivity is greater thon a few K ohm.m-l (f < 0.5 x 106

Hz). c

The effect of the contact resistance is shown in Figure 2.5. The

computed input impedonce of the "intrinsic" transducer is typically [0.14 + i 14.5J ohm

at 1.0 GHz, and [0.20 + i 7.5J ohm at 2.0 GHz. The small value of the real part

explains why the conjugately matched transducer is considerably affected bya contact re-

sistance of the order of a few tenths ohm, while in the untuned transducer, the additional

loss is minor and con be neglected for 011 practical calculations.

The effect of adding a passive tuning element to the source impedonce

is demonstrated in Figure 2.6, which shows that a series inductance that tunes out the capaci-

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TRANSDUCER Au Zno Au LOSS (db) 0.15 1.5 0.15

30

25 UNTUNED

20

15

10 CONJUGATE MATCH

5

0.6 0.8 1 .0 1.5 2.0

20

SAPPHIRE D. R.

-SPACE CHARGE AND

CURRENT DENSITY

-- - ELECTRIC FIELD

r = 0.2 .n. e

f = 0.5 MHz e

3.0

FREQUENCY (GHz)

FIGURE 2.3. EFFECT OF APPLYING THE DIFFERENT BOUNDARY CONDITIONS.

TRANSDUCER LOSS (db) 30

25

20

FIGURE 2.4.

r = 0.2.n. e

f = 0.5 GHz ·e

= 0.5 MHz

= 0.0

=

~JUGATE +-- f 0.5 GHz

e MATCH

0.5 MHz

~ = = 0.0

0.6 0.8 1.0 1.5 2.0 3.0

FREQUENCY (GHz)

CONJUGATE MATCHED AND UNTUNED RESPONSES FOR A HIGH CONDUCTIVITY 1 LOW CONDUCTIVITY AND NON CON DUCTING PIEZOELECTRIC FILM.

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TRANSDUCER LOSS (db)30

25

20

15

10

5

0.6 0.8 1 .0

f = 0.5 MHz c

CONJUGATE MATCH

1.5 2.0

1 .0 ohm

1.0

0.2

0.0

· 3.0

FREQUENCY (GHz)

21

FIGURE 2.5. CONJUGATE fv'IATCHED.·AND· UNTUNED RESPONSES

TRANSDUCE LOSS (db)30

25

20

15

10

5

FOR DIFFERENT CONTACT RESISTANCES.

f = 0.5 MHz c

'--- SHUNT TUNED AT 1.0 GHz

'-- SHUNT TUNED AT 2.0 GHz

r-CONJUGATE MATCH

~~ __ ~~~ ______ L-__ ~==~~_

0.6 0.8 1.0 1.5 2.0 3.0 FREQUENCY (GHz)

FIGURE 2.6. FREQUENCY RESPONSE UNDER DIFFERENT TUNING CONDITIONS.

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22

tive part. of the input impedance at say 1 GHz, is actually ineffective. This is again

explained by the small input impedance compared to the 500hm characteristic impedance

of the source.

On the other hand, shunt tuning introduces considerable changes highly

dependent on the tuning frequency. Computations - show that shunting the transducer

by an inductance of 2.3 n H increases the input resistance at 1.0 GHz ta 1500 ohms

whi le 0.6 n H wi Il cause it to tune at 2.0 GHz with a tuned input resistance of 280 ohms.

The change of frequency response by shunt tuning con be used advantageously

in "response shoping'! by properly choosing the tuning frequency. Other factors that can be

used for frequency. respon.seshaping: are the :electrode niaterial's :andthicknesses. A thinner top

electrode - as it represents less mass loading on the free face of the transducer - gives a

frequency response with a broader bandwidth and lower transducer loss as shawn in Figure

2.7.

ln Figure 2.8, we see the effect of varying the material of the electrodes.

ln general, an acoustically Ilight" material ~ower Zo) yields responses of lower loss but

less bandwidth .

Frequency response shoping con also be achieved by additional loyers as

shown in Figures 2.9 and 2.10. Here, the piezoelectric film is separated from the delay

rod by two metallic loyers. Different combinations of materials are tried, and we see that

the combination (gold / aluminum) gives the broadest bandwidth while the (aluminum / gold)

gives the lowest transducer loss.

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TRANSDUCER LOSS (db)

30

25

20

15

10

5

TRANSDUCE LOSS (éJb~

25

20

15

10

5

Au ZnO Au SAPPH IRE

L = 0.2 ~ L 1.5 0.1 D.R.

UNTUNED

0.6 0.8 1.0 1.5 2.0 3.0

FREQUENCY (GHz)

FIGURE 2.7. EFFECT OF TOP ELECTRODE THICKNESS.

X ZnO

0.1 1.5

UNTUNED

0.6 0.8 1.0 1.5

X

0.1

2.0

SAPPHIRE

D.R.

Zo

Au 65.5

Ag 40.0

A 1 18.4

3.0 FREQUENCY (GHz)

FIGURE 2.8. EFFECT OF DIFFERENT ELECTRODE MATERIAL.

23

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TRANSDUCER LOSS (db)

30

25

UNTUNED

0.6 0.8 1.0 1.5

Au ZnO X y SAP PH IRE

0.1 1.5 0.15 0.15 D.R.

2.0

Agi Au

Agi AI

3.0

FREQUENCY (GHz)

FIGURE 2.9. SHAPING OF THE FREQUENCY RESPONSE.

UNTUNED Au 1 AI

........ ~_ 3 db B. W ____ ., __ ~

Ail Au

0.6 0.8 1 .0 1.5 2.0 3.0 4.0

FIGURE 2.10.

FREQUENCY (GHz)

SHAPING OF THE FREQUENCY RESPONSE.

24

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25

The broad bandwidth obtained using a gold-aluminum "transformer ll

instead of a single gold coupling layer is better visualized by looking at the intrinsic input

impedance of the transducer in the two cases. This is shown in Figure 2.11 where we see

INPUT RESISTANCE (ohm) 0.5

0.4

0.3

0.2

0.1

0.6

F 1 GU RE 2. 11 .

INPUT CAPACITANCE - CONSTANT ~ 11.1 PF

Au, ZnO, AuJ

0.8 1.0 1.5 2.0 3.0

FREQUENCY (GHz)

INPUT IMPEDANCE OF MUlTiLAYER TRANSDUCERS.

that the addition of an aluminum layer causes the real part of the input impedance, as a

function of frequency, to have a double peak, resulting in a broader bandwidth.

At the present time, no general conclusions can be made about these

computed results. Further studies should be directed to a "design" program that con

synthesize a multilayer transducer, given a prescribed frequency response .

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26

CHAPTER III

R F SPUTTERING OF ZINC-OXIDE TRÂNSDUCERS

3. 1 Introducti on

As defined by Davidse and Moissel,28 the term "sputtering" refers to

the ejection of atorns from a material through the impact of ions or atoms. The bombarding

particles are usually ionized particles of an inert 90S (e .g. argon), accelerated by an elec­

tric field appl ied between two electrodes.

ln 0 C diode sputtering, the target is the cathode while the substrate is

at the anode. AOC glow discharge is clearly applicable to the sputtering of conducting

materials only. A high - frequency potential, applied to a metal electrode behind the tar­

get con be used for R F sputtering non-conducting (or poorly conducting) materials.

Further, it is found that R F glow discharge con be sta:-ted and maintained at a mu ch lower

pressure thon that necessary for 0 C discharge. In bath 0 C and R F sputtering processes,

the ionization of the working 90S is enhanced by the accelerated free electrons and charged

particles that happen to he between the electrodes.

Triode sputtering differs in that the main ionizing perticles are electrons

provided bya hot filament and accelerated by an anode positioned so that these electrons

travel in a direction normal to the sputtering beam. A magnetic field is applied to make

these electrons spiral, thus increasing their ionizing ability.

If the 90S used as a sputtering medium contains reactive elements, film

growth is influenced. This property may oc tua Il y be advantageous in sorne appl ications,

particularly in sputtering metal oxides, which are found to deposit with an excess of the

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27

metal element if sputtered in a pure inert 90S. This process is known as IIreactive

sputtering". For a more detaited description of the different processes, see Holland. 29

3.2 Sputtering of Zinc Oxide

From the above discussion, it is clear that RF sputtering has the advantage

of operating at a lower pressure, normally in the microns range. This low operating pres-

sure, considerably increases the mean free peth of the sputtered pertides which implies that

they con reach the substrate white they still have a high kinetic energy, hence giving better

adhesion ~ Also, diode sputtering is advantageous since the apparatus needed is less com-

plex thon that required for triode sputtering. Thirdly, since the material under considera-

tion is a metal oxide, it is mandatory to use reactive sputtering in an oxygen-rich medium.

To summarize, RF diode reactive sputtering is a simple and promising pro-

cess for the fabriaction of high quality zinc-oxide thin films.

3.3 Factors Affecting the Fabrication of Zn 0 Transducers

Uniformity of crystal structure, stoichiometry, orientation of the crystall ites

and good adhesion of the film to the substrate are necessary to obtain reliable and reproduc-

ible transducers.

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28

The rate of deposition and the energy of the sputtered atoms at the moment

they strike the substrate (hereafter referred to as "deposition energy") widely affect the

above-mentioned conditions. The deposition rate and deposition energy are, in turn,

complicated functions of the different factors controlling the sputtering process, such as the

target and substrate positions, shapes and sizes, the substrate temperature, the input power

and the sputtering gas composition. To better understand how each factor affects the pro­

duction of zinc-oxide thin films, they are grouped into the following categories:

3.3.1

Factors pertaining to the sputtering station.

Factors pertaining to the substrate.

Independent factors.

Factors Pertaining to the Sputtering Station

(a) Residual Gases in the Vacuum Cham ber

Even a small uncontrolled amount of a reactive element in the 90S present

in the chamber during sputtering may produce contaminants in the deposited film. Reducing

the amount of unwanted perticles before admitting the sputtering 90S into the chomber, ne­

cessitates the use of a leak-free, non-out9Ossing system, preferably equipped with a 1 iquid

nitrogen cooled baffle. An optically dense baffle mounted directly above the diffusion

pump is used to prevent the oil vopor from backstreaming into the chamber. Also liquid

nitrogen cooling gives the added capability of trapping the condensables and thus reducing

the system pressure.

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29

(b) Target and Substrate Shapes, Positions and Sizes

The geometry of the electrodes between which the discharge takes place

is primarily responsible for the uniformity of the thickness of the deposited film~' 31,32

For the plane parallel disk configuration shown in Figure 3.1, the de-

position intensity distribution at different radial locations on the receiver plane is given

30 by :

= A [ 1 2 2

. H + R - 1 ]

[ 1 - 2 ( R2 _ H2) + (R2 + H2 ) 2 ] 1 ï2

where is the intensity of the deposit, and A a constant depending on the other factors

also H h spacing between the 2 plates

= - = Target radius r

R ri radial location of receiver element

= -= r Target radius

A diagrammatic interpretation of the above equation is shown in Figure 3.2. It is clear that

for best uniformity of distribution, the substrate should be positioned at the centre of the re-

ceiver plane while its lateral dimensions in this plane should be small compared to the radius

of the electrode. The distance between the two electrodes, h, should be kept to a mini-

mum. Decreasing this distance has also the effect of increasing the energy of deposition,

since the average number of collisions a sputtered particle suffers, is reduced. However,

the interelectrode distance can not be decreased below a certain 1 imit determined by the RF

matching network. This constraint is due to the extreme difficulty in tuning the power supply

when h is small. Bock shielding of the target electrode is also another aspect of the tuning

limitations, since the distance between the shield and the electrode is constrained to be

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H

R

h r

ri

r

1· S RECEIVER PLANE

C:;f=====I--===r;:::·1 =~~ ( SUBSTRATE)

h

t I-r --+1 , '-TARGET PLANE

FIGURE 3.1. PLANE PARALLEL DISC CONFIGURATION.

RELATIVE 1.00 INTENSITY

H = 0.1

0.95

0.3

0.90

0.85

0.80

r O. l 0.2 0.3 0.4 0.5 0.6 R

RELATIVE RADIAL LOCATION

FIGURE 3.2. RELATIVE INTENSITY OF DEPOSITION OVER

THE RECEIVER PLANE (REFERENCE 30).

30

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31

within the tldark space" so that the sputtering plasma is confined to the unshielded

28 face. In our case, both for interelectrode distance and bock shield position, we found

that the values provided by the manufacturers allow an easy matching. (lnterelectrode

distance = 2 cm and bock shield at 0.5 cm from the electrode).

3.3.2 Factors Pertaining to the Substrate

(a) Type and Surface Preparation of the Substrate

Typical delay media are selected from single crystals of quartz, yttrium

iron garnet (YIG) , yttrium aluminum garnet (Y AG), and sapphire. The latter is usually

preferred because the crystals are chemically inert, easily cleaned, have good thermal and

f b .. l' . d Il . . 4 a rJcatlon qua Itles, an exce ent acoustlc propertles.

For use as a delay line in the microwave bands, the sapphire crystal shoù"ld

have an optically polished surface. This surface must be c1eaned prior to the deposition of

the transducer. The cleaning procedure must be efficient enough not to leave traces of the

cleaning substances on the substrate.

(!J) Metal Underlayer (s) Used

ln Chapter Il, the importance of a metallic underlayer was discussed. In

addition to the electrical and acoustical properties required, the bock electrode materiol

should provide a good hast for the zinc-axide depasit. Selt and Floria 4

experimented with

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32

different materials and their best results were obtained with sil ver • Gold is extensive Iy

used as a bock electrode for zinc-oxide transducers on c-axis oriented sapphire delay rods

because it is easy to deposit and provide a good base material for epitaxial growth of zinc-

oxide and simi lar wurtzite structures.

(c) Substrate Temperature

The substrate temperature is one of the critical porameters in fi lm growth,

inf1uencing the sticking coefficient, nucleation conditions and the degree of epitaxy

obtainedll

,33 (Figure 3.3). Hussain34

and de Klerk6

remarked that the stoichiometry

of CdS and ZnO deposits depends on substrate temperature.

The effect of substrate temperature on the deposition rate is large. In

RF sputtering, the rate of deposition is found to decrease os the temperature rises, while in

DC • h' 1 •. 13 sputtenng t e Inverse re atlon IS true. The dependence of deposition rate on tem-

perature points out the importance of a uniform, stable, substrate temperature.

3.3.3 Independent Factors

(a) Sputtering Gas Composition

Zinc-oxide films grown by reactive sputtering are found to have varying

degrees of deviation from stoichiometry, depending on the percentage of oxygen in the

sputtering 90s. This fact is assumed to result From the chemisorption of oxygen both at the

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DEPOSITION 10 RATE (AO

/ H) o

/

*

* 1 * * 1 * * * "1:

* * * "1<- * X

*

*

o Moderately Oriented

* Highly Oriented

X Epitaxial

*

*

100 200 300 400 500 600

SUBSTRATE TEMPERATURE (oC)

33

FIGURE 3.3. EFFECT OF DEPOSITION RATE AND SUBSTRATE TEMPERATURE ON

STRUCTURE OF ZnO FILMS ON SAPPHIRE SUBSTRATES (REFERENCE 11).

substrate and at the target. The oxygen collected at the substrate is bel ieved to come

from four sources :

Oxygen originally contained in the target and sputtered

as otoms.

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Atomic oxygen formed in the discharge •

Molecular dissociation upon impact with the surface.

Absorption of energetic oxygeri which penetrates the

lattice.

34

At the target, the surface layer of sorbed oxygen - originating from the sputtering gas -

reduces the sputtering yield significantly.

(b) Input Power

As the input power (or the electrode potential in OC sputtering) in­

creases, two effects contribute to the increase of the rate of deposition :

the increased number of ionized particles in the sputtering

gas ; and

the higher velocities these ionized particles reach before

bombarding the target.

The application of an axial magnetic field confines the plasma between the electrodes and

causes the electrons to spiral, increasing their ionizing abi! ity, thus increasing the rate of

deposition. An important side effect to the appl ication of a magnetic field is that it pro­

vides a more stable glow, allowing for easier tuning and matching to the RF source.

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35

SPUTTERING YIELD (Atom / ion)

0.5 -- - - --------

0.4

0.3

0.2

0.1

1

2 5 10 20 50 100 200

PRESSURE (millitorr)

FIGURE 3.4. SPUTTERING YIELD OF NICKEL IN ARGON (REFERENCE 36).

MEAN FREE PATH (cm)

PRESSURE (Torr)

FIGURE 3.5. MEAN FREE PATH IN ARGON.

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36

(c) Chamber Pressure

As shown in Figure 3.4, the sputtering yield is nearly independent of

the gas pressure in the ronge 1 - 15 millitorr, which is used for RF sputtering, while

it decreases rapidly at higher pressures. This is explained by the balanced action of the

extra ionization available at on increased pressure, and on the other hand, the decrease

of the mean free pat.h at this pressure. (i.e. the increase in the average number of

collisions). Figure 3.5.

(d) Post-deposition Treatment of the Deposited Film

The effects of post-deposition heat treatment on the stoichiometry and

35 texture of vacuum deposits is not yet weIl studied. Desrumaux et al., found that

"bocking" a CdS evaporated film at 4000

C in CdS powder, compensates for the ex­

cess of cadmium and improves the texture quality. For zinc-oxide, Rozgonyi and Polito10

suggest that a stoichiometric balance con be maintained "bya post-deposition treatment".

ln the present work, we have tried heating the zinc oxide films in vacuo and in on oxygen

rich atmosphere . The results of these experiments ore given in Chapter VI .

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4.1 Introduction

CHAPTER IV

TRANSDUCER FABRICATION

37

The various parameters affecting thin film transducer fabrication have been

discussed briefly in Chapter III. The present chapter is concerned with the experimental

set-up for the fabrication of the transducers. The first part covers the description of the

vacuum system and the instruments and accessories used. In the second part, additional

important data are obtained frorn sorne preliminary experiments related to the sputtering

station. Finally, the fabrication procedure is presented.

4.2

4.2.1

Experimental Sputtering Facility

Main Vacuum System

The station used for the preparation of the transducers is an NRC - 3116

vacuum coater with a 6 inch oil diffusion pump and a liquid nitrogen cooled trap, as de­

picted in Figure 4.1. The vacuum chamber -18 inch diameter - is equipped with a feed

through ring, three fixed water cooled electrodes and one movable grounded electrode . The

movable electrode can be rotated about a vertical axis to bring it - horizontally parai lei to

and vertically above - any of the fixed electrodes. Its vertical position is also adjustable

so that the spacing of the two plates can be changed. The fixed e lectrodes have a diameter

of 5 inches and are used as target holders, whi le the movable one carries the substrate holder

and heater, a thermocouple to measure the substrate temperature, and the thickness monitor

crystal.

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2 x GAS 1 N LET====::()():===t F. T. R.

~--~------~--~ A . F • • L-----"""

A.R. V. T C 1

R. V. C.B.

TC2

M.P. D.P.

F. V.

38

"fMAGNETS

3 x ELECTRICAL POWER INLET

FIGURE 4.1. SCHEMATIC DIAGRAM OF THE VACUUM SYSTEM.

LEGEND

A.F.

A.R.V.

B.V.

C. B.

D. P.

F.E.

F.T.R.

F.V.

Air Filter.

Air Release Valve.

Baffle Valve.

Cryo Baffle.

Diffusion Pump.

Fixed Electrode.

Feed Through Ring.

Foreline Valve.

I.G.

M.P.

N.V.

P.G.

R.E.

R.V.

T .C.

Ion Gouge.

Mechanical Pump.

Needle Valve.

Pirani Gouge.

Rotating Electrode.

Roughning Valve.

Thermocouple Gouge.

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39

Two coils, ring shaped, carrying currents of up to 10 amperes provide an

axial magnetic field between the electrodes of up to 100 gauss.

A Pirani gauge (CVC, GP - 210 C) provides an accurate reading of the

chamber pressure in the range 1 - 50 millitorr, which is the useful range for sputtering.

An ionization gouge and two thermocouples (NRC 720) monitor the chamber and fore-

1 i ne pressures from atmospheri c to 10-8

torr. (See Fi gure 4. 1) •

4.2.2 Instrumentation

(a) Substrate Heating and Temperature Control

The substrate heater is essentially a stainless steel block heated by a

Nichrome wire element. The substrate (sapphire delay rod) is fixed by holding it under

a slight mechanical pressure between two aluminum grips as shown in Figure 4.2. The

holder is designed so that the surface of the delay rod facing the target is emerging out of

the electrode plane, thus preventing any masking or shadowing effects.

To ensure good heat transfer, the sapphire crystal is wrapped in on indium

tinned copper shim.3

A chromel-alumel thermocouple is in contact with one of the side

faces of the substrate. This sensor is connected to a "Thermovolt" control 1er capable of

a temperature control of better thon :: 5 Oc in the ronge 50 to 500 oC. The control 1er

switches the current to the heater on and off. This current which can be adjusted up to 5

amperes is usually set at about 4 amperes.

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40

HEATING WIRES THERMOCOUPLE

STAINLESS STEEL BLOCK

ALUMINUM GRI P

COPPER SHIM

SU BSTRATE

FIGURE 4.2. SUBSTRATE HEATER.

(b) Holder with Mask

To deposit the top electrodes, another holder is used. This is shown in

Figure 4.3 and consists of a block of aluminum in which two circular holes 0.5 mm dia-

meter and spaced 3 mm apart are drilled counter-sunk to minimize shadowing effects.

Two transducers are thus produced in each run under the some conditions, allowing for a

quick check on the re liabil ity of the results. Four centering screws enable positioning the

crystal to obtain the two transducers at nearly symmetrical places on its surface.

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41

SU BSTRATE

r 4 x CENTERING SCREWS

ELECTRODE

(j 0.5 mm, COUNTER SUNK

FIGURE 4.3. HOlDER WITH MASKS.

(c) Film Thickness Monitor

A Slocn DTM - 3 frequency meter relates the thickness of the deposit

build-up on an osci lIating quartz crystal, to the change in frequency.36

where

T

T

Af

p

A f =

5.63 P

= thickness of the deposit in microns,

=

=

reading of the rneter in KHz,

3 mass density of the deposit material in 9 / cm ,

5 63 . .. f d .. . KH 3 / • = sensltlvlty or mass etermlllotlon, III z. cm g. ~

During sputtering, two kinds of difficulties are encountered. First, the sensor head being

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42

sensitive to high temperatures, has to be thermally isolated from the heated electrode.

This introduces a source of error in thickness monitoring since the rate of deposition is a

function of temperature. The temperature dependent error is estimated during sorne pre­

liminaryexperiments (see Section 4.3.3) and is accounted for in the rest of the work •.

Secondly, the interference between the RF sputtering fields and the crystal oscillator make

it impossible to read the instrument during sputtering. To overcorne this difficulty, the

sputtering is started with the thickness monitor crystal in the field of deposition and the in­

strument adjusted for null indication. After 30 minutes, the RF ·source is switched off

to enable a measurement of the thickness. The rate of deposition is thus calculated and

the sputtering is continued under the same initial conditions for the time required to obtain

the proper thickness.

(d) DC and RF Power Sources

A DC high voltage power supply (NRC 1901) as weil as an RF one

(CVC Plasmavac Type AST 300) are avai lable .

A Bayly IW3 - 15A RF wattmeter is used to measure both forward and

reflected RF powers. Due to the high VSWR on the cable connecting the tuning network

to the electrodes, the power meter is inserted in the line connecting the RF power amplifier

to the tuning network, which is shown in Figure 4.4. Losses in the tuning network and cables

are assumed negligible, cornpared to the power fed to the discharge .

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43

POWER METER

~ ,..-_____ TO VACUUM

RF

OSCILLATOR

POWER

AMPLIFIER

TUNING

NETWORK

CHAMBER

HIGHVSWR

FIGURE 4.4. R F POWER SUPPLY AND POWER METER.

4.3 Preliminary Experiments

Before proceeding with the main experiments, sorne preliminary tests were

necessary to establish the procedure to be followed in producing the transducers.

The various experiments done in this study are:

1. Evaluation of the metallic film deposition techniques.

2. Measurement of the temperature rise of an unheated substrate

as the sputteri ng process deve 1 ops.

3. Obtaining calibration charts for the rate of deposition of zinc-

oxide versus the net RF power input for different substrate

temperatures and 90S cornposi ti ons.

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44

4.3.1 Metallic Films

The objective of this experiment is to establish the procedure for deposit­

ing the gold metal electrodes. Since gold does not adhere weil to sapphire, an intermediate

layer of chromium is used.

(a) Chromium Deposition

A chromium film is formed on the face of a partially masked sapphire rod.

The conditions for sputtering are as follows :

Target : 5 inch diameter pure chromium disk.

Intere lectrode distance : 2 cm.

Working gas : pure argon at a pressure of 7 mill itorr.

Power supply: 150W RF.

Time of deposition: 5 minutes.

After removing the sample from the vacuum system, the film thickness is measured using a

Watson-Bornet interference microscope objective having a vertical resolution better than

1 /10 fringe with a green light source, (Thallium X = 535O~). The chromium layer

is found to be about 1000 i. thick, i.e., the rate of deposition is about 200 A / min.

(b) Gold Deposition

A gold film is deposited on a sopphire crystal on the top of a chromiun

loyer prepared os in (0) above. The gold target is a 2 inch diameter gold disk. Pure

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45

argon at a pressure of 40 mill itorr is used as the working gas for DC sputtering at

2.5 KV and 2 cm interelectrode distance. After 5 minutes of sputtering, the sample

is removed from the cham ber and the thickness of the gold deposit is measured. About o

1470 A of gold is detected, i.e., the rate of deposition ~ 300 °A / min. A high re-

solution diffraction picture of this gold film showed that it is polycrystalline with the

(220) planes preferably oriented parallel to the substrate surface.

(c) Gold Top Electrodes

A gold layer is deposited as in (b) through a 0.5 mm mask. Micros-

copic inspection showed that the film has a convex shape which is due to the shadowing o

effect of the mask. It has a thickness of 1160 A at its centre corresponding to a rate of o

230 A / min, compared to 3000

A / min obtained in the unmasked case.

4.3.2 Temperature Rise Due to Sputtering

The substrate temperature was recorded during the deposition of a zinc

oxide layer on a sapphire rod, once using an input RF power of 200 w, and another time

with 125 watts. The results are in Figure 4.5, which show that the rate of temperature

rise is highly dependent on the input power. This experiment also tells us that in order to

maintain a fixed substrate tempe rature , we have either to heat the specimen to a temperature

level above that which it would have reached if unreated, or, to cool it at a certain rate

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TEMPERATURE (oC) 1

100

80

60

40

20

P = 200 W·

30 60

p = 8 ~ , O2

= 10 %

t END OF SPUTTERING

r P = 125 W

90 120 150 180

TlME (min)

FIGURE 4.5. TEMPERATURE RISE DUE TO SPUTTERING.

balancing the rate of heating due to sputtering. A practical experimental set-up is to

46

have a cooled electrode (e .g. water cooled) with a controlled heating element 50 that

the adjustment of the flow of the cooling substance together with the heating current allows

us to operate at any temperature we wish. In our vacuum system, described in Section

4.2.1, a water cooled "movable" electrode presented a technical difficulty, and 50 we

were limited to operate at temperatures higher thon 150 Oc .

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47

4.3.3 Effect of RF Power on Deposition Rate

Glass microscope slides are used as substrates in this set of experiments. o 0 .-

First, a 150 A thick chromium layer, followed bya 1500 A gold film, is deposited on the

glass substrate. Then, without breaking the vacuum, the substrate is moved to a masked

section of the electrode having a hole of 10 mm diameter, through which zinc-oxide is

sputtered for 30 minutes. This arrangement makes it possible to obtain 4 test samp les at

different power levels on one slide in each run.

The thickness of the zinc-oxide loyers is measured using the film thickness

monitor, (Section 4.2.2 (c)) , and 0150 - after breaking the vacuum - using the inter-

ferometric method. A comparison of the two readings gives the correction factor for the

thickness monitor calibration, thus compensating for the error due to temperature rise.

The rate of deposition calculated from the measured thickness is plotted

in Figures 4.6, 4.7 and 4.8, against the net RF input power. In Figure 4.6, we see

that within the accuracy of the actual measurement, the relation is linear and independent

of pressure. However, Figure 4.7 shows that at high input powers, the relation deviates

from linearity and is affected by the substrate temperature. The sputtering gas composition

is argon : oxygen = 50 : 50. In Figure 4.8, similor calibration chorts ore obtained

for the gas composition 90 : 10 .

The important conclusion drawn from these experiments is that a stable

temperature and a good control of the input power are necessary to maintain a fixed rate

of depositi on throughout the sputtering operation.

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RATE 100 48 (Ao/min) PRESSURE

9 0

80 * 9.5 * , 10

x 11

60 0 12

+ 15 x

* 18 EXPERIMENTAL 0 ERROR

40

x + 20

*

20 40 60 80 100 120 140 W

FIGURE 4.6. RATE OF DEPOSITION vs. POWER INPUT AT DIFFERENT PRESSURES.

RATE

(A ° /min) 200

350

150 , __ - 300°C

10

50 UNHEATED / /

/ /

./' /

50 100 150 200 250 W

FIGURE 4.7. RATE OF DEPOSITION vs. POWER INPUT AT 50 % O2 .

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RATE

(Ao/min) 200

150

100

50

UNHEATED /

/ /

/ /

50

49

350 Oc

100 . 150 200 250 W

FIGURE 4.8. RATE OF DEPOSITION vs. POWER INPUT AT 10 % 0 . 2

4.4 Transducer Fabrication Procedure

4.4.1 Cleaning Procedure

The sapphire crystal used as a delay rad is cleaned, prier to the deposi-

tions, using the following steps :

{a} Immerse in hot aqua-regia for 2 minutes to remove

previ ous deposits.

(b) Rinse in disti lied water.

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50

(c) Remove organic residues using hot chromic acid.

(d) Rinse in running distilled water.

This method is found satisfactory (see Section 3.3.2 (a», especially if the substrate is dried

and put under vacuum immediately after cleaning.

4.4.2 Deposition of Bock Electrode

After cleaning, the substrate is fixed in the holder described in Section

4.2.2 (a». The vacuum chamber is then pumped down for several hours, usually over­

night. This prolonged period of evacuation has two purposes : to reduce the residual gases

in the chamber to a minimum, a vacuum better than 10-7

torr is achieved, and to allow

for a uniform and stable substrate temperature.

Pure argon is introduced into the chamber through a needle valve whi le

the baffle valve is throttled to allow for a dynamic flow of the 90S. At an equilibrium

pressure of 7 millitorr the RF power supply is switched to the chromium target. After a

few minutes of pre -sputtering, the substrate is brought above the target for 45 seconds.

With an input power of 150 watts, this time gives a chromium thin fi lm of about 150 A 0

The pressure is then raised to 40 mill itorr and using the D. C. power supply at 2.5 KV

the gold bock electrode is formed after a pre-sputtering period of 5 minutes and another

active sputtering period of 5 minutes. The fi lm thus obtained has a thickness of about

1500Ao

.

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51

4.4.3 Deposition of the Zinc-Oxide Film

Following the deposition of the gold e lectrode, the argon is pumped out

for one hour and then the proper Argon-oxygen mixture is admitted through a needle valve

to raise the pressure to the required value. A pre-sputtering of the zinc-oxide target for

15 minutes followed by the deposition of the required film using the RF power supply

terminates this step. Adjustment of the tuning network and the driver current, to obtain

the necessary power to the discharge, is made during the pre-sputtering periode

4.4.4 Deposition of the Top Electrodes

The substrate is allowed to cool for 6 hours before breaking the vacuum

to transfer it to the holder with the masks. (see Section 4.2.2 (b)). Under the same con­

ditions described in Section 4.4.2 above, the gold top electrodes are deposited.

4.4.5 Chemical Etching of Zinc-Oxide

Since the zinc-oxide is deposited over the entire surface of the sapphire

crystal, it is necessary to etch the film at the corners of the delay rod to uncover the

gold bock electrode. This is done using diluted hydrochloric acid followed bya short rinse

in running distilled water.

Referring to Figure 4.2, one can see that gold - as weil as zinc-oxide -

deposit as a narrow' ribbon on the side faces of the substrate. Special care has to be given

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52

to etch zinc-oxide from this area whereas the presence of gold is advantageous insofar as

it provides a good electrical contact to the holder used in the electron microscope,

(Chapter V) , thus providing a leakage path for the space charge build up on the sample

surface.

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53

CHAPTER V

TESTING OF THE TRANSDUCERS

5. 1 !ntroducti on

ln this chapter, the methods used for testing the transducers are described

in detail. The major tests performed on each transducer are:

Determination of the crystallographic structure and orientation

of the zinc-oxide crystallites w ith respect to the substrate .

This gives an indication of how far the transducer is, ho,." the

ideal, c - axis oriented, single crystal one used in theoreti-

cal calculations.

Evaluation of the frequency response - transducer loss versus

frequency - which is the only meaningful representation of

the electrical performance of the transducer.

5.2 Structure Ana Iysi s

Reflection electron diffraction (RED) and X-ray reflectio'1 techr<que)

are used to study the crystal structure of the vacuum deposit,. However; a thin fil"., less

than a few microns thick can only be examined by the RED technique. Thi, i5 due to +he

fact that the interaction of electrons wjth atoms is much stronger. bya factor of rcughly

103

, than the interaction of X-rays. For RED, diffracted beams of intel"sity cQtT1poroble

wi th that of the incident beam can be given by less thon 100 A 0

of crysto l, ..... h 'Ie 0"

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54

X-ray beam must traverse 5 to 10 mi.crons of perfect crystal before a diffracted beam ca~

achieve appreciable amplitude.37

5.2.1 General Formulae Governing RED

RED employs a stream or beam of high energy e lectrons (de Broglie waves)

contained in a vacuum better thon 10-4 torr. In the incident beam , it is assumed that

the electrons (also known as ~ particles) are monoenergetic, hence monochromatic. It

con be easily shown that the wave length , À 1 of such electrons is given by :

À == h

[2m eV(l+ o

where h is Pkmck's constant j m 1 electron rest mass j V 1 the accelerating o

potential ; e 1 electron charge ; and c, the speed of light.

If numerical values are substituted for constants in the above equation,

we get

À == 5.1

or

5.2

Equation 5.2 is accurate within an error of less thon 5 % for 100 KV.

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55

The simple, elegant relation

2 d (hk 1) sin 9 (hk 1) = n À 5.3

known os Bragg1s Law, relates d (hkl) the distance or interplanar spocing between con­

secutive parallel diffracting planes whose Miller indices ore (hkl) and 9 (hkl) the ongle

between the direction of the incident beam and the diffracting planes. 9 is also half the

diffraction angle, i.e., the ongle between the incident beam and the diffracted one. In

the above relation n is on integer giving the order of diffraction.

Applying Bragg1s law to single perfect crystals, gives electron diffraction

patterns consisting of arrays of spots. More often a spot pattern represents the average

pattern for a large number of separate small crystals aligned to have the sorne orientation.

The alignment of the individual single crystals is imperfect not only by

bending or rotations about axes Iying in the plane of the specimen but also by rotations

about on axis perpendicular to this plane. Thus, not only do we get a modification of in­

tensity of the diffracted spots, but the spots ore spread into arcs and ore often also diHused

by the limitation of crystal size in the directions perpendicular to the incident beam ~7

On the photographic plate the radii of the arcs measured from the central

spot formed by the incident beam are given by :

r (hkl) = L ton 2 9 (hkl) 5.4

where L is the cornera length, i.e., the length from the specimen to the photographie

plate.

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56

o For RED, 9 isusuallyverysmall, lessthan 1 , sothatEquations 5.3

and 5.4 con be combined to give :

r (hkl) ~

XL d (hkl)

5.5

line-broadening as mentioned above is due to the limited crystal size, t (hkl) , in the

direction (h k 1) normal to the incident beam. Using Sherrer formula: 38

t (hkl) X 5.6

49 . cos 9 (hkl)

one can estimate the crystal size. However, due to the small values of X and 49, the

estimate is very coarse.

5.2.2 The Zinc-Oxide Structure

The Zincite crystalite, (ZnO), is known as the Wurtzite structure. The

description of the crystal is in terms of two interpenetrating hexagonal lattices as shown in

Figure 5.1 ,

zinc atoms are at positions (0, 0, 0) + h c p trons-

lation, and

oxygenatomsareatpositions (0,0, u) + hcp

translation .

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57

r 110

-! 100

002L

~~ t u + 1/2

Tl/2

b

/ ® ZINC ATOMS

• OXYGEN ATOMS a

FIGURE 5.1. ZINC - OXIDE CRYSTAL.

The ideal value of u for hexagonal closed pack is 0.375 while

39,40 0 measured values are 0.374 and 0.383. The lattice constants at 298 K are:

a = 3.249858 ± 6 A 0

and

c = 5.206619 ± 2 A 0

The c / a ratio is thus 1 .602 compared with the hexagonal closed pack value of

.i 8 /3 = 1 .633 .

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58

For this structure, the only reflections systematically absent are the

( h h 1) for 1 = 2 n + 1 •

5.2.3 Experimental Set-up and Procedure

RED pictures were taken on a Philips EM 300 electron microscope using

an accelerating voltage of 80 KV and a camera length of 353.5 mm. Substituting

these values in Equations 5.1 and 5.5, we get :

À = 0.0416 AO

r (hkl) = 14.75/ d (hkl) 5.7

For convenience, rand d in Equation 5.7 are in millimeters and angstroms respectively.

Table 5.1 gives the values of d and r for different planes of the zinc-oxide structure.

To take a RED picture, the fi lm is first etched by short immersion in

dilute hydrochloric acid to remove any surface contamination. The sapphire crystal is

then introduced into the microscope column via an air-Iock device and diffraction patterns

at several positions on the surface are examined. The results obtained are discussed in

Chapter VI.

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TABLE 5. 1 .

Zn 0 interplanar spacing (d) and radii of semi circles on

the photographie plate (r) based on :

Mi 11er Indices

h k 1

100

002

101

102

110

103

200

ZnO lattice parameters :

a

c

=

=

3.2498 A 0

5.2066 A 0

Electron microscope constants:

y = 80 KV

L = 353.5 mm

Formula d h k 1 d= A

O

a sin 600

2.8142

c /2 2.6033

2 a c sin 600

2.4754

j3a2 +4c2

. 600 a c Sin 1 .9109

)3 a2

+ c2

a /2 1 .6249

0 2 a c sin 60 1.4774

fz,;/ 2 . 27a +4c

a /2 . sin 60 0

1 .4071

XL r =

d

5.23

5.65

5.94

7.70

9.05

9.95

10.45

59

mm

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60

5.3 Evaluation of the Electrical Performance of the Transducer

ln network theory, the transducer gain of a 2 - port is defined as the

ratio-expressed in decibels - of the power dei ivered to the load to that power available

26 from the generator. Referring to Figure 5.2 (a), the ability of a piezoelectric trans-

ducer to convert electrical power to mechanical power (acoustic power generation) is

expressed in terms of the generation transducer 1055 :

P T L (G)

a = - 10 10910 P 5.8

o

where P is the acoustic power delivered to the acoustic medium and P is the elec-a 0

trical power available from the generator.

The inverse function, namely converting mechanical power to electrical

power (acoustic power detection), Figl're 5.2 (b), is expressed as a detection transducer

loss :

T l (D) Pd

= -10 log­P.

1

5.9

where Pd is the power dei ivered to the electrical load and Pi is the acoustical power

;.,cident on the transducer, ail of which is "available".

As discussed in Chapter Il, if there are no drifting carriers in the transducer

uf'1der consideration, then reciprocity holds and the generation and detection transducer

losses are equal.

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----- TRANSDUCER ---~

P. 1

(a) (b)

61

ELECTRICAL LOAD

FIGURE 5.2. PIEZOELECTRIC TRANSDUCER AS (a) GEN ERATOR, (b) DETECTOR.

P o

P ~ o ~ P - - - - - - --, al , ~ Pil -- - - - ----'

~ P ------, 02 1

+ Pi2 - - - - --'

---..,,. Pa3

.... etc.

FIGURE 5.3. PULSE - ECHO DELAY LlNE.

1 ~Pal \

DELAY

L

rMIRROR PLANE

1 1 1

1 Pil

1 1 ROD 1

t

L~

-..P ~

dl

Il

FIGURE 5.4. UNFOLDED DELAY LlNE WITH RESPECT TO THE FIRST ROUND-TRIP.

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62

5.3.1 Ove rai 1 Transducer Loss

ln the pulse echo technique of measurement~1 pulse modulated oscillations

cause the transducer to generate ultrasonic waves that travel in the delay rod, reflect at

the far-end face, and travel bock towards the transducer where they are detected (first

echo). Due to the acoustic impedance mismatch at the transducer-rod interface, a portion

of the mechanical power is repeatedly reflected bock into the delay rod causing higher

order echos as depicted in Figure 5.3.

As far as the first echo is concerned, the single ended delay line with a

reflecting endfac~ can be unfolded about the mirror reflecting plane and therefore re-

presented by the 2 - port network shown in Figure 5.4. An overall - device - transducer

1055 is then defined :

T L (device) 5.10

It is pointed out that the device transducer loss combines the generation and detection

transduce r losses as weil as the delay rod 1055, aDR

, where:

T L (device) = T L (G) + aDR

(1) + T L (D) 5.11

and

aDR

(1) Pil

5.12 = - 10 log-Pal

The subscript (1) in Equations 5.10, 5.11 and 5.12 refers to the first

rou.,d trip of the acoustic pulse .

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63

5.3.2 De lay Rod Losses

For the nth round trip, the delay rod loss is :

p. a

DR (n) = - 10 log pin

an

This term is made up of several factors which are summarized as follows :

(a) Delay Rod Attenuation : 01

For c - axis oriented sapphire, the attenuation is 0.18 db / cm at

1 GHz, and varies as the square of the frequency ~2 Therefore we can write :

= - 0.18 L f2 x 10-16 db

5.13

5.14

where f is the frequency in Hz, and L the length of the round trip - twice the length

of the delay rod - in meters.

(b) Diffraction Loss : 02

Diffraction loss is a more complicated function of frequency, top elec­

trode geometry, rod material and length ~3

ln Figure 5.5, the diffraction loss in c - axis oriented sapphire is plotted

against a normalized trip length. In Figure 5.6, the diffraction Joss of the first, second

and third round trips is plotted against frequency. The deJay rod length is taken to be

12 .5 mm and the top e Jectrode diameter 0.5 mm.

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RELATIVE LOSS ( db)

4

2

2 4 6

SAPPHIRE, C - AXIS

b = 0.16

64

8 10 L/(02/ X)

FIGURE 5.5. DIFFRACTION ATTENUATION IN SAPPHIRE (REFERENCE 43).

O2

(n )

(db) 2

LOSS

(db)

2

=: 12.7 mm.

o = 0.5 mm.

n = 1

0.5 0.6 0.8 1.0 1.2 1.6 2.0

FREQUENCY ( GHz)

FIGURE 5.6. DIFFRACTION LOSS PER ROUND TRIP.

0.5 0.6 0.8 1.0 1.2 1.6

FREQUENCY (GHz)

FIGURE 5.7. DELAY ROD LOSSES.

2.0

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65

(c) Other losses : 03

These are caused by imperfect reflection at the free face of the delay

rOO, non parallelism of the 2 faces and small deviations in the crystallographic orienta­

tion. In general

5.15

a3

can be made negligible by properly choosing and machining the delay rod. The at­

tenuation and diffraction losses are known and can be incorporated in the calculations.

Figure 5.7 is a plot of 01 ' a2

(1) and aDR

(1) for the first echo

in the de lay rOO described above .

5.3.3 Delay ROO Holder

ln Chapter Il, calculations have shown the importance of an effective

low loss contact to the metal electrOOes. The delay line holder used for transducer loss

measurements was specially designed to meet this requirement. As shown in Figure 5.8,

the holder is a type N male connector (lnitially a He~lett Packard 420 A crystal de­

tector holder) to which a gold plated, spring loaded "POGO" contact is soldered.

Four centering screws enable accurate positioning of the delay rOO so that the top elec­

trOOe of the transducer to be tested faces the spring loaded contact, while the delay rOO

is pressed from the other side by a spring loaded plastic piston. Short-circuit impedance

measurements showed that the parasitic contact resistance to a thin gold foil is less than

0.4 ohm.

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66

DELAY ROD

4 CENTERING SCREWS

TYPE N CONNECTOR

FIGURE 5.8. DELAY ROD HOlDER.

5.3.4 Conjugate Motched Tronsducer loss

The circuit of Figure 5.9 is the basic circuit used to measure the con-

. h d d 1 l, 2 , 35, 41 lugate matc e trans ucer oss.

G is a pulse modulated UHF generator,

H a Hybridge with insertion loss Hab between

ports a and b,

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67

M a "lossless" match ing network - e. g., Double Stub Tuner,

A a variable calibrated attenuator,

S an RF coaxial switch,

R a heterodyne receiver and amplifier. x

The method of measurement consists in adjusting the attenuator A until the power received

at switch position 2 is equal to the power detected from the first echo at switch position 1.

Therefore :

A Po = H24 P dl 5.16

where P is the power available from the generator after splitting equally in arms 2 and o

3 of the Hybridge. Equation 5.16 converted into decibels, together with Equation 5.10

gives the device loss :

T L (device) = A - H24

5.17

SÏ!1ce the Hybridge is operated with ail ports terminated in the characteristic impedance,

H24

is a known constant (6 db for the "Alford" Hybridges).

At this point, it is recalled that the generation and detection transducer

losses are equal since no acoustic amplification effects are involved. Therefore, using

Equati ons 5. 11 and 5. 17

T L (G) = T L (D) = A - 6 - a

DR (1)

2 5.18

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G

--+ P

o

3

H

2 4

A

DELAY ROD

1 1 1 1 1 1

1 P 1

1 0 TRIGGER 1 L ______________ .. ______ --1

68

FIGURE 5.9. CIRCUIT USED FOR TUNED TRANSDUCER LOSS MEASUREMENT.

G

v o

2 S N

e

A

1

1

Pd1 1 +- DELAY 1

-- ROD 1 1 5 P

1 e 0 1 1 1 TRIGGER L_~_L _________ ~------.J

FIGURE 5.10. CIRCUIT USED FOR UNTUNED TRANSDUCER LOSS MEASUREMENT.

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69

which is simply called the transducer loss, TL, and is plotted against the frequency to

give the frequency response of the transducer under test.

The use of a matching network (M) in this circuit is necessary to balance

the two arms of the Hybridge. Careful tuning to minimize the voltage standing wave ratio

seen by arm 2 of the Hybridge is carried out at each frequency. The transducer loss

obtained under such conditions is the conjugate matched transducer 1055.

ln a high resistivity (Iossless) transducer, the "intrinsic" conversion

efficiency is 100 %, so that the conjugate matched transducer loss is exclusively due to

the contact resistance and the matching network loss so far assumed negligible. The effect

of these parasitics is discussed in Chapter Il.

5.3.5 Untuned Transducer Loss

ln order to measure the untuned transducer loss the circuit of Figure 5.9

is modified, namely the matching circuit is removed and the Hybridge is replaced byan

electronic switch (S) as shown in Figure 5.10. The drive of the electronic switch is e

obtained From a pulse gene rator , Figure 5.11, synchronized with the pulse modulator of

the UHF source. The duration and delay of the driving pulse are adjusted 50 that it over-

laps the incident UHF burst providing the necessary isolation of the receiver.

Let S be the insertion loss of the switch (lncluding the 3 db pad). e

Therefore equating the pa.vers at terminais 1 and 2 of the manual switch S:

5.19

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PULSE GENERATOR GR 1340

EXTERNAL

DRIVER

2 SWITCH

NO 1 1 NC L ______ J

TRIGGER 3 db PAD

70

D C POWER SUPPLY

FIGURE 5.11. DETAILED BLOCK DIAGRAM OF THE ELECTRONIC

SWITCH USED IN FIGURE 5.10 .

Converting 5.19 into decibels and combining with Equations 5.10 and 5.11, noting

that the incident power on the transducer is S P , we get e 0

T L ==

A - 2 S e - a DR (1)

2

which is the untuned transducer loss.

5.20

Typical frequency responses obtained using the above circuits are shown

and discussed in the following chapter.

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71

CHAPTER VI

EXPERIMENTAL RESULTS

6.1 Introduction

A large number of zinc-oxide transducers were produced and tested in

accordance with the method of fabricati on outl ined in Chapter IV, and the testing pro-

cedures detai led in Chapter V.

ln order to investigate the effect of the different parameters affecting the

preparation of the transducers, the objective originally was to produce a set of samples

having 011 deposition parameters fixed - except one. However, as mentioned earlier, it

was found that preselecting the sputtering power does not allow a close control on the de-

position rate. This is due to the steepness of the rate-power relationship which was found

in the experiments described in Chapter IV and shown in Figures 4.7 and 4.8. It was

therefore decided to study the effect of varying each of the parameters, with the deposition

rate as another indepenCiient variable. The results obtained are thus presented as two dimen-

sional families of curves. An example is given in Figure 6.1 which shows a family of

constant temperature - minimum loss versus rate curves.

6.2 Temperature and Deposition Rate

1 •• Il h ba· f . d· 1.2 h f· of . n.tla y, on t e SIS 0 prevlous stu les, t e Irst set expenments

were performed using a sputtering gas of 50 : 50 - oxygen : argon - composition, while

the pressure was fixed at 8 millitorr. The distance between the electrodes was 2 cm.

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72

A number of depositions (19 samples) were made at various rates and o

temperatures covering the ranges 40 - 200 A / min and 200 - 400 oC, respectively.

The results for these transducers are shown in Table 6. 1 ~

ln Figure 6.1, a plot of the minimum transducer loss (conjugately matched)

against the rate of deposition, with the temperature as a parametric variable, is shown.

For a certain fixed temperature, say 300 oC, the transducer loss is seen to decrease with

the increasing deposition rate. However, this relationship has a discontinuity at a certain

rate (hereafter called the critical rate) which seems to have very little correlation with

MIN TL 02 = 50 %

TEMPERATURE (db)

o 200 Oc 30 c 250 Oc

6 3OQoC

20 / 350 Oc x 400 Oc

10

50 100 150 200 RATE ( A 0 / MIN)

FIGURE 6.1. MINIMUM TRANSDUCER LOSS vs. RATE OF

DEPOSITION AT 50 % OXYGEN.

* Tables 6.1 to 6.7 are shawn at the end of the chapter.

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73

the temperature. RED studies showed that the transducers produced below the critical rate

have in general weil ordered structures, with the c - axis oriented perpendicular to the

substrate surface, within :1: 200

as shown in Figure 6.2, for sample number 10. The

transducers fabricated at higher rates are polycrystalline with the (100) planes preferably

oriented parallel to the substrate surface as in RED picture for semple number 12 as shown

in Figure 6.3 (a). The latter, however, contain sufficient correctly oriented crystal lites

(c - axis normal) to be piezoelectrically active. A further increase in the deposition

rate apparently increases the percentage of correctly oriented crystal lites as shown in

Figure 6.3 (b), thus improving the transducer action.

ln general, the crystal structure was uniform throughout each sample and

no preferred orientation in the plane of the substrate surface was noticed. The randomness

is readily verified by checking that the pattern is completely independent of incident elec­

tron beam directi on.

ln Figure 6.4, another representation of the results discussed above is

used. Here, the constant transducer-Ioss contours are drawn in the rate-temperature plane

with the experimental points shown by small circ les •

The frequency responses of some typical samples are shown in Figure 6.5.

The different responses are better expressed in terms of the 3 d b bandwidth as a percent­

age of the central frequency (% B.W.) , which is drawn in Figure 6.6 against the rate

of deposition, and is found to be independent of the substrate temperature. It is also noted

that the minimum % B.W. occurs at - or about - the critical rate.

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FIGURE 6.2. RED PICTURE OF

Zno FILM No. 10

(002)

FIGURE 6.3. RED PICTURES OF

(a) SAMPLE No. 12

(100)

~) SAMPLE No. 14

(100, 002)

74

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FIGURE 6.2. RED PICTURE OF

ZnO FILM No. 10

(002)

FIGURE 6.3. RED PICTURES OF

(0) SAMPLE No. 12

(l00)

lb) SAMPLE No. 14

(l 00 , 002î

74

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TL 30

( db)

20

10

0.5 0.6 0.8 1.0 1.2 1.6 2.0

FREQUENCY (GHz)

FIGURE 6.5. TYPICAL FREQUENCY RESPONSES FOR SAMPLES

PRODUCED AT 50 % OXYGEN.

%BW 100

o

o 50

o

.50 100 150 200 RATE (A

0 / MIN)

FIGURE 6.6. BANDWIDTH vs. RATE OF DEPOSITION

AT 50 % OXYGEN.

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77

ln Figure 6.7, in spite of the small number of experimental points, we

see that the loss-rate re lationship at different pressures has the sorne general trend as was

shown earl ier •

MIN TL

(db) 30

20

10

12

8

50 100

~ 15 .... 12

~1O

150

FIGURE 6.7. EFFECT OF PRESSURE.

8

PRESSURE

6 10 m ili itorr

° 12

X 15

200 RATE (Ao/MIN)

A specially interesting somple is number 27 which showed shear mode

excitation near the quarter wavelength frequency. Figure 6.8 is an os ci 1 logram for the

echo pulses showing the shear mode superimposed on the longitudinal mode. RED picture

for this somple is shown in Figure 6.9. A c1ear (110) trace indicates that these planes

are stacked poralle 1 to the substrate surface.

Another interesting RED picture, Figure 6.10, is that obtained for

semple 20, which shows a very high orientation of the zinc-oxide film.

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FIGURE 6.8. DETECTED ECHOES

SHOWING SHEAR AND

LONGITUDINAL WAVES.

Upper trace at 1 GHz.

Lower trace at 1.2 GHz.

(Vertical 17 db / cm,

Horizontal 2 ~ sec / cm.)

FIGURE 6.9. RED PICTURE OF

SAMPLE No. 27

(110, 002)

FIGURE 6.10. RED PICTURE OF

SAMPLE No. 20

(002, HIGH

ORIENTATION)

78

fl1ll II l

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79

6.4 Effect of the Gas Composition

Table 6.3 summarizes the conditions and results obtained for 11 samples

fabricated at different gas compositions : 5, 10 and 20 % oxygen respectively with the

complementary balance of argon. The minimum transducer loss is plotted versus the rate

of deposition in Figure 6.11, which again shows the same type of relationship as above.

MIN. Tl ( db) 30 OXYGEN

50 X 5%

0 10 20

20 A

20

~ 10 AR A 10 ~ 10

50 100 150 200 RATE (A

o / MIN)

FIGURE 6.11. EFFECT OF THE GAS COMPOSITION.

ln addition, an attempt was made to deterniine the stoichiornetry of the samples produced in

this set of experiments. Visual microscopic inspection showed that the films produced in

5 % oxygen are - without exception - dark grey, characteristic ci excess zinc in the

deposit. Those produced at 10 and 20 % oxygen are transparent while the films obtained

in the previous set of experirnents at 50 % oxygen content were yellowish.

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80

Methods of analytical chemistry 47 failed to give a stoichiometry index

for these films because the quantity of material available was too small (about 0.2 mg).

X-ray fluorescense also failed as a stoichiometry indicator because of the oxygen light

atomic weight compared to the zinc, (0 = 16, Zn = 65.38).

The electrical resistivity was then taken as a relatively more precise esti­

mate of the stoichiometry than the color of the film. The samples produced at 10 % oxygen

had generally a high resistivity of about 15 K ohm. m. Those fabricated in the 20 % and

50 % oxygen atmospheres were also highly resistive. However, an erratic, unexpected

drift in their resistivity was noticed and could not be explained. The few samples made at

5 % oxygen showed lower resistivity (about 200 ohm. m) which is due to excess rne ta Il ic

(Zn) atoms in the deposited fi lm.

6.5 Rate - Temperature Survey at 10 % Oxygen

At this point, it was felt that the 10 % oxygen - 90 % Argon 90S com­

position gives the best ZnO films with regard to their stoichiometric structure. Therefore

a rate - temperature survey similar to that done for the 50 - 50 gas composition was rele­

vant. Table 6.4 and Figures 6.12, 6.13 and 6.14, show the results obtained end are

in ail respects similar to Table 6.1 and Figures 6.1, 6.4 and 6.6. The comparison

shows that lowe ... transducer losses and wider bandwidths can be achieved using the 10 %

oxygen atmosphere without being critically sensitive to the deposition rate - i.e. the R F

power input. Figure 6.15 is the frequency responses of typical transducers in this set.

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MIN TL

(db) 30

20

10

50 100 150

81

TEMPERA TURE

o 200 Oc o 250 Oc Il 300 Oc / 350 Oc

200

RATE (Ao

/ MIN)

FIGURE 6.12. MINIMUM TRANSDUCER LOSS vs RATE OF

RATE 200

(Ao

/ MIN)

150

100

50

DEPOSITION AT 10 % OXYGEN.

o

200 250 300

PREDOMINANT ORIENTATION

002

100, 002

350 400 TEMPERATURE (oC)

FIGURE 6.13. CONSTANT TRANSDUCER LOSS CONTOURS

AT 10 % OXYGEN.

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%BW

100

50

50 100 150

82

o

200 RATE (AO

/ MIN)

FIGURE 6.14. BANDWIDTH vs RATE OF DEPOSITION AT 10 % OXYGEN.

TL

( db)30

20

10

0.5 0.6 0.8 1.0 1.2 1.6 2.0

FREQUENCY (GHz)

FIGURE 6.15. TYPICAL FREQUENCY RESPONSES FOR SAMPLES

PRODUCED AT 10 % OXYGEN.

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FIGURE 6.16. RED PICTURES OF

(a) SAMPLE No. 34

(002, EPITAXIAL)

(b) SAMPLE No. 46

(002, HIGH ORIENTATION)

(c) SAMPLE No. 48

(100, 002)

83

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FIGURE 6.16. RED PICTURES OF

(a) SAMPLE No. 34

(002, EPITAXIAL)

(b) SAMPLE No. 46

(002, HIGH ORIENTA TlON)

(e) SAMPLE No. 48

(l 00, 002)

83

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84

Epitaxial growth is noticed in RED pictures of samples made at 300 Oc and below the

critical rate (120 A 0

/ min in this case). Figure 6.16 •

6.6 Crystal Size and C - Axis Spread

The microcrystallite size was estimated from line broading (see Chapter V)

o to be about 200 A. An attempt was made to correlate the crystal size and the c - axis

spread about the film normal with respect to : transducer loss, rate of deposition and / or

temperature. Apparently there is no direct relation between these variables. However,

if we only look at samples with pol ycrysta Il ine structure, having a c - axis spread of

about :1: 200

the apparent crystal size seems to decrease slightly with increased rate of

deposition as shown in Figures 6.17 and 6.18. These conclusions are very tentative since

the error in crystal size measurement might be very large (:1: 100 A 0) .

6.7 Input Impedance

The input impedance of sorne samples have been measured at 2 MHz

using a high frequency bridge. In Table, 6.5, the measured C and R, as weil as the

calculated values for the input capacitance are listed. The resistivity of each film is de-

duced from the measured input resistance.

A comparison between the calculated and measured capacitances shows

that the latter are 2 to 3 times higher than the former. This suggests that the electrode

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C-AXIS SPREAD

:1: 9° 30

20

10

50

0

a â

x

0

[)

!J. 0

/

!J.

!J.

100

85

TEMPERATURE

° 200 Oc o 250 Oc Il 300°C / a

!J. 1 350 Oc )( 4OQoC

0 / /

150 200

RATE (Ao / MIN)

FIGURE 6.17. C-AXIS SPREAD vs RATE OF DEPOSITION.

CRYSTAL SIZE

AO 400

300

200

100

o 0

~--H- Il 0

o l,a-~L- 0 A A-

o o

50 100 150 200

RATE (Ao /MIN)

FIGURE 6.18. CRYSTAL SIZE vs RATE OF DEPOSITION.

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86

material (gold) diffuse (or is imbedded during sputtering) in the ZnO film to decrease

the effective length of the transducer and / or increase the effective area. It is to be

noted that the high substrate temperature and the process of depositing the top electrode

(sputtering, evaporation, ••• ) play a role as far as this effect is concerned.

6.8 Effective Coupling Constant and Contact Resistance

A technique commonly used for the evaluation of the electrical performance

of the transducer is to fit the computed frequency response to the experimental points by

adjusting an effective electromechanical coupling constant, Keff

' according to some best

fit criterion. (Keff

~ Kt' where Kt is the coupling constant of an oriented single

crystal of the piezoelectric material, Kt = 0.28 for ZnO).

ln Chapter ", the theory for the calculation of the transducer loss was

discussed and it was shown that the conjugate matched responses are highly sensitive to cir­

cuit losses, while untuned responses mainly depend on the intrinsic transducer. This fact

makes it possible to evaluate both Keff

and the contact resistance r c by fitting computed

curves using a least squares criterion for both the tuned and untuned measured experimental

points. This has been carried out and results in Figure 6.19 for samples numbers 34 and

39. Here it can be seen that the circuit losses can adequately be modelled by a contact

resistance of about 1.0 - 2.0 ohm. The results obtained for these samples as weil as

other samples are summarized in Table 6.6. The effective coupling constant ranges from

0.04 to 0.25 : 0.01 and is higher for a transducer having a weil oriented structure.

The highest value of Keff

= 0.25 obtained for sample number 34, is approximately 10 %

belaN the value for bulk znO.

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TL

(db)

TL

(db)

30

20

10

0.5

30

20

10

0.5

o untuned

Il tuned

A

0.6 0.8 1 .0

(a)

0 untuned

A tuned

0.6 0.8 1.0

(b)

87

SAMPLE 34

= 0.25

r = 1.7 ohm c

o

1.2 1.6 2.0

FREQUENCY (GHz)

SAMPLE 39

Keff = 0.17

r = 1.0 c

0

1.2 1.6 2.0

FREQUENCY (GHz)

FIGURE 6.19. COMPUTED CURVES FITTED TO EXPERIMENTAL POINTS.

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88

This method of fitting curves for both tuned and untuned measurement:;

provides us with a better model for the extrinsic transducer and proves to be more accurate

than the methods used hereto.9,24

6.9 Post-Deposition Treatment

The effect of heat treating a sample to compensate for its stoichiometric

deficiency is studied.

Semple number 8, originally prepared in 50 % oxygen, showed an

improvement in the frequency response after baking for six hours at 300 Oc in a vacuum

better than 10-6 torr, Figure 6.20. The same treatment tried with samplenumber 35

prepared in a 10 % oxygen showed negligible differences.

TL (db) 30 SAMPLE 8

ORIGINAL~

AFTER HEAT TREATMENT

0.5 0.6 0.8 1.0 1.2 1.6 2.0

FREQUENCY (GHz)

FIGURE 6.20. POST-DEPOSITION HEAT TREATMENT.

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89

A third sample (number 31) was heated for 6 hours at 300 Oc in an

atmosphere of 8 microns pressure of oxygen : argon - 20 : 80. The 90S was then

slowly pumped out white the sample was left to cool before breaking the vacuum. Neither

the frequency response, nor the microstructure, showed observable changes.

These three tests, affirms the conclusion that heating the zinc-oxide film

in vacuo causes the desorption of the chemically absorbed oxygen,44 thus causing the

compound to approach its stoichiometric composition.

6.10 Adhesion

Good adhesion of the different films to one another and to their substrate

is an important factor that affects the transducer performance. Methods of measuring ad-

hesion are quite a few : "Scotch tape" method and abrasion testing have been criticized

elsewhere.45

The scratch method consists of drawing a rounded steel point across the film

surface while a vertical load applied to the stylus is gradua Il y increased until a critical

value is reached at which the film is stripped cleanly from the substrate leaving a clear chan­

nel. The critical load is taken as a measure of the adhesion. A more recent publication 46

adds sorne observations and comments to this method and concludes :

n The stylus method does, however, appecr capable of

providing a comparison of the adhesions of otherwise

identical film - substrate combinations. n

For a qualitative comparison of our specimens, an apparatus similar to the one sketched in

Reference 46 was specially constructed. Severa 1 specimens were tested and it was found

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90

that the adhesion failure always occur at a load of about 10 grams. Microscopic inspec­

tion showed that the failure is in the gold - chromium - sapphire bond. It is therefore

conc\uded - with reservation - that the adhesion of ZnO to gold is of a better quality

than that of gold to sepphire. The reservation here is referring to the fact that the pro­

cesses of measuring adhesion have been developed and analysed only for the case of a single

film - i.e. the y have not yet been proven to work for multilayered structures.

6.11 Reliability and Reproducibility

Reliability of the results is readily verified throughout the work by checking

that the two transducers produced simultaneously on the same substrate have similar responses

and structures. Few semples showed differences of any significance and whenever this

happened microscopic inspection showed black lloases" in the gold top electrode of one of

the transducers, probably due to a foreign particle trapped on the substrate surface while

transferring it to the masked holder.

A check for reproducibil ity that was a Iso carried out, is the fabri cation of

complete transducers under exactly the seme conditions as previous ones. Conditions for

semples 11 and 34 were imitated to produce semples 11 Rand 34R. The critical control

of the rate of deposition reflects on the results obtained, while the reproducibility is con­

firmed as shown in Table 6.7, where it can be seen that semples produced under the seme

conditions have the seme structure and almost the seme electrical performance.

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91

TABLE 6.1 *.

O2 =50%, P = 8 mil li torr

N° T . P VSWR L R TL % B.W . Structure Oc Watts ~ A °lmin db

200 155 1.6 1.4 87 33 002

2 200 180 1.4 1.6 118 16 32 002

3 200 200 1.6 1.6 138 30.5 33 100, 002

4 200 210 1.4 1.5 170 11.5 61 100, 002

5 250 180 1.3 1.1 83 18 79 002

6 250 200 1.4 1.3 106 10 54 002

7 250 210 1.3 1.6 129 28 17 100, 002

8 250 220 1.3 1.8 200 15 60 100, 002

9 300 130 1.2 1.2 45 23 80 002

10 300 175 1.3 1.4 72 18.5 73 002

11 300 200 1.2 1.6 107 12 47 002

12 300 210 1.4 2.0 112 23 22 100, 002

13 300 215 1.2 1.6 136 20 30 100, 002

14 300 225 1.3 1.6 179 13 65 100, 002

15 350 200 1.4 1.6 105 20 46 002

16 350 225 1.5 1.5 144 9.5 42 002, 100

17 350 230 1.2 1.4 149 19.5 40 100, 002

18 400 250 1.2 1.3 85 25 33 002

19 400 280 1.4 1.3 174 20 65 002, 100

* ln this and ail subsequent tables O2

is the percentage oxygen in the sputtering gas ;

p, the pressure in millitorr i T, the substrate temperature in Oc ; P, the net R F input

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92

power in watts ; VSWR, the voltage standing wave ratio j l, the ZnO film thickness

in microns j R, the rate of deposition in A 0

/ min ; T l, the minimum tuned transducer

loss in db j B.W., the 3 db bandwidth of the transducer loss in terms of percentage

from the central frequency. The number sets appearing under "structure '1 are the Mi 11er

indices of the planes preferably oriented porallel to the substrate surface. If 2 sets are

given the first one is the more dominant orientation. Additional letters: h. o. and

e p. stand for : high orientation and epitaxial respectively.

TABLE 6.2.

O2 = 50 % , T = 300 Oc

N° p P VWSR L R T.l % B.W. Structure

20 10 175 1.2 1.3 80 15 60 002 h .0.

21 10 200 1.3 1.6 120 13.5 32 100, 002

22 10 220 1.2 1.7 155 8.5 29 100, 002

23 12 125 1.2 1.6 40 17 002

24 12 170 1.2 1.5 77 11 40 002, 100

25 12 200 1.2 1.8 104 22.5 35 100, 002

26 12 220 1.4 1.5 150 16 58 100, 002

27 15 190 1.2 1.6 106 22 41 11 0, 002

28 15 220 1.6 1.2 134 17 61 100, 002

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93

TABLE 6.3.

p = 8 mi Il itorr, T = 300°c

N° O2 P VSWR L R T .L. --% B. W. Structure

29 5 100 1.2 1.5 60 10.5 43 002

30 5 130 1.2 1.6 77 20 43 100, 002

_~.1 5 150 1.3 1.5 116 20 36 100, 002

32 5 200 1.3 1.8 144 18 36 100, 002

33 10 100 1.2 1.3 55 9 002 e p •

34 10 150 1.2 1.5 77 6.5 47 002 ep.

35 10 175 1.3 1.5 120 13 47 100, 002

36 10 200 1.4 1.6 160 8.5 75 100, 002

37 20 100 1.2 1.2 55 11 83 002 h. O.

38 20 125 1.3 1.7 83 10.5 58 002, 100

39 20 160 1.2 1.4 140 8 87 100, 002

TABLE 6.4.

o = 10 % , p = 8 millitorr 2 NO T P VSWR L R Llo % B.W. Structure

40 200 100 1.2 1.4 56 29 002

41 200 125 1.3 1.5 110 11.5 40 002

42 200 145 1.2 1.5 120 9 58 002

43 200 150 1.4 1.6 140 19 60 100, 002

44 200 160 1.2 1.7 170 9 79 100, 002

45 250 100 1.2 1.2 57 15 78 002

46 250 125 1.2 1.6 n 10.5 72 002

47 250 175 1.2 1.4 150 14 69 100, 002

-id 250 200 1.3 1.5 194 10 85 100, 002

(cont1d) ...•

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94

TABLE 6.4 (cont'd)

o = 2 10 % , p = 8 mill itorr

N° T P VSWR L R LL- % B.W. Structure

49 350 125 1.2 1.8 55 18 72 002

50 350 lSO 1.2 1.6 97 14 60 002

51 350 175 1.2 1.6 120 29 100, 002

52 350 200 1.3 2.0 160 20 33 100, 002

TABLE 6.5

c = input capacitance ( P F) R = input Resistance ( K ohm) p = resistivity ( K ohm. m)

N° L C cale. C R P meas.

11 1.6 9.6 23 130 15.9

12 2.0 7.7 18 210 20.6

29 1.5 10.2 26 2 0.2

34 1.5 10.2 28 125 16.4

35 1.5 10.2 30 120 15.7

38 1.7 9.1 22 165 19.0

42 1.5 10.2 31 140 18.3

46 1.6 9.6 21 150 18.4

50 1.6 9.6 24 130 15.9

51 1.6 9.6 22 115 14.2

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95

TABLE 6.6.

r = contact resistance (ohm) c

Keff

= effective coupling constant

TL TL Keff

r N° TUNED UNTUNED

c STRUCTURE

31 20 31 0.04 1.4 100, 002

34 6.5 15 0.25 1.7 002 e p •

35 13 20.5 0.13 1.3 100, 002

36 8.5 15.5 0.21 1.5 100, 002

39 8 19 0.17 1.0 100, 002

42 9 16.5 0.21 1.6 002

TABLE 6.7.

REPRODUCIBILITY CHECK

N° O2

, p, T, P, VSWR L R t.L. % B.W. STRUCTURE

11 1.6 107 12 47 002 Sorne Conditions

11 R 1.5 100 13 49 002

34 1.5 gJ 6.5 47 002 e p • Sorne Conditions

34R 1.4 90 7 50 002 e p •

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CHAPTER VII

SUMMARY AND CONCLUSIONS

96

A procedure for computing the response of a multilayer transducer has

been described. Results of calculations using this procedure have been presented which

foc us attention on the effects of contact resistance, finite film conductivity, e lectric

tuning and different electrode materials c;>n the transducer performance. The possibility

of achieving very large bandwidths by means of multilayers has also been demonstrated •

. . -further, it has been shown that R F sputtering is a convenient method

for producing well-oriented ZnO transducers having electromechanical coupling constant

within 10 % of the bulk Value. The study of the influence of the deposition parameters

pointed out the fact that the film quality is highly dependent on the deposition rate, hence

the input R F power, the substrate temperature and the gas composition.

For a fixed temperature and gas composition, the results have shown that

a critical rate exists above which the crystallites of the ZnO film deposited on Z-oriented

sapphire have the c-axis Iying in the plane of the substrate surface, randomly oriented,

thus causing the transducer action to deteriorate • For a wide range of temperatures and

gas compositions, the critical rate is found to lie between 100 and 130 A 0

/ min, while

the best transducers are obtained at a rate just below the critical rate. Transducers having

tuned transducer loss as low as 6.5 db and bandwidths of about 0.6 GHz are reproducible

in an oxygen rich atmosphere (10 : 90 - O2

: A), on heated substrates (300 oC) .

It has also been shown that transducers having very wide bandwidths and

reasonably low transducer 1055 can be fabricated by properly selecting the deposition para-

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97

meters. Such a performance was achieved in sample number 48 which had a bandwidth

of 1.2 GHz and a minimum transducer loss of 10 db.

Measurement of the input impedance showed that the resistivity of the

Zno film is about 15 - 20 K ohm.m for good transducers. The e lectromechanical

coupling coefficient, as weil as the circuit losses, were estimated by fitting calculated

frequency responses to both the tuned and untuned experimental points. Values of Keff

of from 0.04 to 0.25 were obtained while the circuit losses were modelled by an ex­

trinsic contact resistance of about 1 - 2 ohm.

Although the transducers described here are canparable in performance

with those previously reported~,9, 16 sorne improvement in the vacuum station and the

measurement techniques are suggested.

To minimize circuit losses, soldered - or welded - leads should

be used instead of spring loaded contacts.

A tighter cootrol should be provided on the rate of deposition, sputter­

ing gas mixture and rate of gas flow to facilitate the optimization of the transducer

performance, since these parameters affect the crystal orientation and stoichiometry of

the zinc-oxide fi lm.

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APPENDIX 1

COMPUTER LISTING

98

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OOOl

000. DilO 1 000 .. Oll'>' OuOI> 000 1

C THIS PROGRAM CALCULATES THE TRANSDUCER LOSS C OF A MULTILAYER SEMICONDUCTING PIE10ELECTRIC C TRANSDUCER. C MKS SYSTEM OF UNITS 15 USED. ACOuSTICAL IMPEDANCES t ARE IN 10 •• ' KG/CM.M.SECI UNITS. C C THE FOLLOWING 15 A LIST OF INPUT YARIABLES 1 C C yARIABLE MIANING c------------------------------.... -... -------------------. ___ ._ C N NUMBER OF LAYERS C 1DR DELAY ROD MECH. IMPEDANCE C lA FRIE FACE IMPEDANCE C AREA AREA OF TOP ELICTRODE C F1 TUNING FREQUENCY C 155 SOURCE IMPIDANCE CEPS PIRMITIYITY OF TRANSDUCER MATERIAL C FO DIFFUSION FREQUENCY C P INDICATES TYPE OF THE LAYER C ' .' FOR THE PIEZOELECTRIC LAYER C ILANK FOR OTHER FILMS C MAT MATERIAL OF THE FILM C IF FILM MECH. IMPEDANCI t L FILM LENGTH C VS SOUND VELOCITY C F FREQUENCY C K ELECTROMECHANICAL COUPLING CONSTANT C R SERIES CONTACT RESISTANCE C FC CONDUCTIVITY FREQUENCY C VR DRIFT VELOCITY/SOUND VELOCITY C MICF NO. OF 80UNOARY CONDITION CASES C BC BOUNDARY CONDITIONS 1 C '5.CHARGE',IEL.FIELD' AND/OR 'CUR,OEN,' C MSIF NO. OF SOURCE IMPEO. CASES C SI TYPE OF SOURCE IMPEDANCE TUNING C 'CO' FOR CONJUGATE MATCH C 'UN' FOR UNTUNED C 'SH' FOR SHUNT TUNED C 'SE' FOR SERIES TUNED C C FOR ~,A,F,FC t VR AOOITIONAL ~ETTERS I,F tS C STAND FOR INITIAL, FINAL AND STEP RESPECTIVELY. , C ••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••• C

CUHMON ,BLK1/L,VS,ZF,ZA,ZOR,N,IP ~ ,BLKZ/FC,FD,FO,5,SS,R,RN,YR,ZFIP,ALPHA,LAMDA i IBLK)/1E,ZS,ZSO,BT,XT,F,F1,IS

DOuBLE PRECISION MAT,BOCOI31,BC')1 DIMENSION 51M141,S1141 olMENSION ZLRI501,ZRRI501,WRI'01 DIMENSION MAlI201,ZFIZ01,VSIZOI,L,ZOI COMPLEx ZE,ZR,ZRR.i~,lLR,ZS,ZSS,zso LJGICAL COND

0008 0009 0010

0011 0012 0013 0014 0015 0016 0017 00111 0019 0020 0021 0022 0023 0024

0025 0026 0027 0028 0029

0030 0031 0032 0033 00310

0035 0036 0037 0038 0039 0040

0041 DOlo'

0043 001010 0045

C

REAL DATA DATA

L,KI,KF,KS PIE10/1 .'I,SIH/'CO"IUN','SH','SE'I BOCO/IS,CHARGEI,IEL,FIELDI,ICUR,DEN.I/

C •••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••• ' C C READ INPUT DATA

C

C

C

READ,5,lOI N,lDR,ZA READC',3DI AREA,F1,lSS READC',301 EPS,FD DO 1 J a1,N READ15'201 P,HATIJI,lFIJI,LIJI,YSIJI IFIP.EQ.PIE10I IPaJ CONTINUE READC5,301 FI,FF,FS READ15,301 KI,KF,KS READ15,301 RJ,RF,RS READ15,301 FCJ,FCF,FCS READI5,3DI YRJ,YRF,YRS READ15,401 HBCF,eC READ(5,501 HSIF,SI

MFCPel.+(FCF-FCII/FCS MYRFal.+CVRF-YRII/VRS MKFa 1.+(KF-KII/KS MRFa 1.+(RF-RII/RS MFFa 1.+IFF-FII/FS

FO= O.5.VSIIPI/L(IPI RNaLIIPI/(6.Z8318.FO.EPS.AREAI RS"RS/RN RI"RI/R~~ ZFIPaZF(IPI

C •••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••• e C C CALCULATION OF ZL AND ZR

FaFI-FS

C

C

C

00 ,. Jal,HFF GO TO 3

2 WRITE(6,100I F 3 F.F+FS

w • 6.28)18.F

CALL ZLZR (W,ZL,ZR,IDI IFCID.EQ.11 GO TO 2

ZLRIJlaZL ZRRIJlaZR

4 WRIJlaW

C ••••••••••••••••••••••••••••••••••••••••••••••••• C C TRANSDUCER LOSS CALCULATION

00 00

Page 107: STRUCTURE AND PROPERTIES OF SPUTTERED ZnO TRANSDUCERSdigitool.library.mcgill.ca/thesisfile47721.pdf · STRUCTURE AND PROPERTIES OF SPUTTERED ZnO TRANSDUCERS ... Basic Equations The

00 .. 6 00 .. , OO"d 0\1"'. OO~O OO~I OO'~ OO~J OO~ .. OO~> OO~b 00' 1 00~6 OO~Q

OObCi OObl OOb, O()bJ OOb" OOb; 00b6 OObl 00b8 OOb'l ~OlO

00 Il OOU 001.1 001'0 007~ OU7b 001 ; 00111 007'1

0010 00111 OJllt OOUJ Oull .. OOIl~ 00110 0081 00811 0\)8'1

OO?I) OOQI OllQl 009) 009 .. OU'I)

C

t

NOTE TH! PROPER NESTING OF 'DO' LooPS FC- PCI DO 666 HFC-l,MFCF CoND - IFCfFOI .GT. 1.OE-Ob IFICoND' GD To , MSCP1-1 MVRF1-l GD To 6

, MICF1·M8CI' MVRF1·MVRF

b CONTINUE DO '" Mlt.l,MBCFl IFI.NoT.CoNDI GD TO 44 ALPHA-l. LA'1DA-l DO 11 1-1,' IFIBCIMSC'.EQ.SOCoII" GD To 122.,).44',1

11 CONTINUE 22 LAHDA·2

GD To lolo 3) ALPHhO. Iolt CONTINUE

VR- VRI DO 444 HVR-l,kVRFl DO J'3 I1SI.l,MSIF DO " 1 -1.1t IFISIIMSI,.EQ.SIMCI" 15.1

H CONTINUE AI( r _1(1 DO 222 HI(-l.MI(F S· ... KT.AKT ,;5-1.+5 "-RI DO 111 '1R-1.MRF RR-R.RN

C SELECT TUNING & WRITE "EADING OF PAGE lFIIS.LT." GD To 66

(.

W • 6.2nlUFl CALL lllR IW.ZL.lR.lD' CALL TLOSSIW,ZL,lR,CoND,l)

bb CALL SOURCECZSS,RN' IFICoNO, WRITEC6,90, BCIM8C,.VR,FC WRITEI6,60, lDR,lA,AREA,RR,AKT 00 11 J-l,N

77 WRITEI6,70, J,HATCJ),ZFIJ),LIJI,VSIJ) wR 1 TE 1 6,101

00 Il Hr.1,MFF W .WIIIH") ZL • ZL Il r '1 F ) ZRoZRIIP1FI CALL TLUSStW,ZL,ZR.CoND,21

Il CO~TINUl

0096 0097 0098 0099 0100 0101

0102 0103 0104 0105 OlOb 0107 0108

0109 0110

0111

0112

0113

C 111 R.R+RS 222 AKT-AKT+KS 333 CONTINUE 441t VR.VR+VRS '" CONTINUE 666 FC.FC+FtS

C C •••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••• C

STOP 10 FORMAT 115,lFIO.4' lO FORMAT IAl,AB,FIO.4,EIO.4,FIO.4' 30 FORMAT IIE10.4' 40 FoRMATI14,4X,4ABI 50 FoRMATI14,4X,4IAl,6X" 60 FoRMATI31X,'DELAY RoD IMPED •• ',FIO.2,

alOX,'FREE FACE IMPEO. -',FlO.2/'lX, a 'TOP ELECTRODE AREA .' ,E10.4,BX, a 'CONTACT RESISTANCE .',FI0.4/31X , a 'KT .',F10.) 1140X,' LAVER 1, a'MATERIALI,4X,'ZF',7X,'L IMICRoN,I,4X,'VS'/1

70 FoRMATC40X,I),lX,AB,F10.2, 6PF13.4,OPF12.ll 80 FoRMATI' 'III' FREQ GHZ',lOX,'TLG CDBI','X,IEL.M.L.I"X,

i 'ELECTRJCAL INPUT JMPEO.',llX,'TLO 10BI'"X,'MC.M.L.I, a ,x,'MECHANJCAL INPUT IHPED.'/I

90 FoRMATI)lX,IBoUNOARV CONDITIONS :',AB l'lX, a 'VO/VS ·',F10.2,21X,'FC .',El'.4'

100 FDRHATI' .WARNING. ZL OR ZR TENDS To " a'lNFINJTV AT ',-9PFlO.2,' GHZ'II 13X, a'CALCULATloNS AT THIS FREQ. ARE DELETED',

END

-OPTIONS IN EfFECT. JO.EBCDIC,SOURCE,NoLI5T,NoDECK,LoAD,NOMAP -OPTIONS IN EFFECT. NAME - HAIN , LINECNT • 56 -5TATI5TICS. SOURCE STATEHENT5 • 113,PRoGRAM SIZE • 4690 .51ATI5TIC5. NO DIAGNOSTICS GENERATED

-o o

Page 108: STRUCTURE AND PROPERTIES OF SPUTTERED ZnO TRANSDUCERSdigitool.library.mcgill.ca/thesisfile47721.pdf · STRUCTURE AND PROPERTIES OF SPUTTERED ZnO TRANSDUCERS ... Basic Equations The

000.

0(10'

OOOJ 00010 000; 0001, 0001 OOOd OOO'i 0010 Dili.

Oul~ OulJ 001,. OOI~ 001t.. 001' OUIII 001'1 OOlll Où" OOlL OOB OO~" OO/.'

Oll/t. 0017 OOll! OOi'l 001(, OJ11 OUJi OOH OiJH OoB OJ1C1 00].' 0,1)0 00)'1 Oll~'J OO~I

01)" t

0010) 00 ... OU .. ,

SUBROUTINE TLOSSIW,lL,ZR,CDND,ID) C SUIROUTINE TLOSS CAlCUlATES THE TRANSOUCER LOSS. C JT CALLS RonT le CINV 1 C ROOT SalVES COMPlEX POLVNOMIAlS C IC 15 THE HAX. NO OF ITERATIONS C CI~V SOlVES SYSTEMS OF COMPlEX EQUATIONS C DELTA 15 THE DETERHINENT OF THE COEFFICIENTS MATRIX

C

C

COHHON IllKZ/FC,FD,FO,S,SS,R,RN,VR,ZFIP,AlPHA,LAHOA i IllKJ/ZE,ZS,ZSO,BT,XT,F,Fl,IS

COMPlEX AI,),ZI4),OI4"BI4,51,BBI4,",EPI41,ENI4) CDHPLEX C,Cl,C2,C],DEtTA,T,Vl,VO,Vl,CU COMPLEX lE,ZOE,ZH,ZOH,ZR,ZRR,Zl,ZlR,ZS,ZSO lOGICAl CoNO F-W/b.ZIJ18 "'-Z Llll-CMPLXISQRTISSI,O.OI lIZ"-l(1) IFe.NOT.CONDI GD To 100

~-4 AI11-CHPlxI1.,FC/FI AIZI-CHPLxl-VR,O.OI A(ll-CHPLXI-SS,IF/FO-FC/FII AI41-CHPLXISS*VR,0.01 AI,,-CHPLxIO.O,-SS*F/FO) C -AIZI/12.*AI111 Cl·CSORrIC*C-SS-AllI/AII» Llll--C·CI 1141--C-Cl IC·ZOO CAll ROUT Il,5,4,1,0.0001 ,ICI BI4,"·CHPlXI0.0,0.01 813,"_CHPlXIO.0,0.01

100 H-~+l BI2,HI-'HPlX(-1.,0.1 B(l,HI-CHPlXI-l.,O.1 ~ -CHPl~(O.O,O.'*W/Fol Cl-CHPl(O.O,Z.·FO/WI CU·CHPlX(FC/FO,-F/FOI 00 10' 1-1,N CZ-CEXpeC/Z(111 IFI.NOT.CJNOI GO To 102 Cl-Ill.·S*AlPHAI-ZII)*ZII)I/IIII)·.LAHOA) IFIVR) 102,10Z,101

101 EP' II-C"PLXI 1.0,0.01 ENIII-l.le2 GO To 10)

10Z ENII hC,'1PLl(1 1.0,0.0) ePIII-C2

10) BI lilI-CIl II-ZRltEPe Il SI~,I)·IZI1)+Zl)*ENII) BB 1 1, 1 1 • O.llI 1 1 * Ill) -1 • ) • ' EPI 1 ) -EN 1 1 ) ) IF, .NOT .CONO) CO TO 105'

004b 0041 Ou48 004 .. 00)0 0051 00), 0053 0054 0055 OOSb 0057 OO)B 0059 OObO OObl

OObl

00b3 00b4 OOb5 OObo 00b7 OObB 00b9 0070 Don OOH

Don 0074 0075 0070

·0'077 007b 007'i OOB", 0081 OOBl OOBJ OOB ..

00B5 OOSCI 0\187 OOBt! Oull9 0090 009\ 0091. 0093 0'J9"

C

C

C

t

c

SI], 1 )-C1*EPII) B14, 1 ) -C l*EN Il )

10' CONTINUE DO lOb J-l,H DO lOb I-Z,N

lOb BBIl,J)-BII,JI CALL CINV 1 B,N,H,OELTA,O.lE-ZOI IFICABSIDELTA).lT. 1.E-301 RETURN VL·CO.O,O.OI vllli 1.,0.01 00 107 1-l,N QII )-BI l,HI Vl-VL+Olll*EPCII

107 vl=V1-C3*OII)*IZlll*ZIII-l.I*IEPII,-ENIIII T--VL*ZR ZE-V1/CU+R

IFIID .EQ.l) RETURN

IFIREAllZEl1 109,109,8 B VO.CU*ze

PE-REAlIVO*CoNJCCCUII PH-REAlI-T*CONJCIVLI) ETAG-PH/PE.S/3.14159 CALL TUNE CHLE-4. t REALIZSI.REALIZEI/REALIIZS+ZEI*CONJGIZS+ZEII n-CHLE.ETAC IFITL.LT.l.OE-lOI Tl.l.OE-lO TlC--10.*ALOG10ITLI

BBel,H)-l.+CU*IZSO+RI CALL CINV IBB,N,H,DELTA,O.lE-ZO) IFeCABSIDELTAI.LT. I.E-30) RETURN Vl·IO.O,O.OI T -1-1.,0.01 DO 108 l-l,N OIII.BBe l'MI VL-Vl+QIll*EPIII T ~T-OIII*ZII)*EPIII

108 CONTINUE ZM=T/Vl IF(REALIZMI) 109,109,9

9 CMLHa4 •• REALIZMI.REALIZRI/REALleZM+ZRI.CONJCIZH+ZRII VO·-CU.lSO PE-REALIVO·CONJGICUII PH=REALI-T.CONJCIVLII ET~O· PE/PH*3.14159/S n~CHlH·ETAO IF(TL.LT.l.OE-101 TL-l.OE-lO TLO--10.*AlOG10ITL) ZOE-lE.RN 10M_ZM*lFIP

... o ...

Page 109: STRUCTURE AND PROPERTIES OF SPUTTERED ZnO TRANSDUCERSdigitool.library.mcgill.ca/thesisfile47721.pdf · STRUCTURE AND PROPERTIES OF SPUTTERED ZnO TRANSDUCERS ... Basic Equations The

C III' lTE OUTPUT 009~ IIRITEI6,101 F,TLG,CHLE,ZDE,TLO,CMLH,ZOM OJ9~ RETURN 0097 109 IIRITEI6,201 F o"''Ie RETURN OO'l~ 10 FORMATe' ',-9PF7.3,6X, OP2F1Z.4'2E15,5,6X,2F1Z.4,Z~15.51 OIOU 20 FURMATe' ',-9PF7.3,' UNSTABLE'I 0101 ENO

·I)~'IONS IN EFFECT' 10,EBCOIC,SOURCE,NOLIST,NOOECK,LOAO,NOMAP -opriONS IN EFFEtT' NAHE - TLOSS , LINEtNT - 56 .~T~TI~TICS' SOURCE STATEMENTS - 101,PROGRAM SIZE - 5120 ·S1ATISTICS* NO UIAGNOSTICS GENERATEO

0001

0002 0003 0004 0005 0006 0007 0008 0009 0010 0011 0012 0013 0014 0015 0016

0017 0018 0019 OOZO OOZl 00Z2 0023 00Z4 OOZ5 0026 0027 0028 00Z9 0030 0031

SU8ROUTINE ZLZRIW,ZL,ZR,IOI C SUBROUTINE ZLZR CALCULATES ZL ANO ZR AT W, C ID 15 AN INTERNAL INDICATOR TO PREVENT OVERFLOW. C

C

COHHON IBLK1/L,VS,lF,ZA,ZOR,N,IP DIMENSION ZFCZO),VSI201,LI20) CoMPLEX ZL,ZR,DEN REAL L 10-0 n-cl"O.O)*ZA IFIJP.EQ,1) GOTo 3 JP1-IP-1 00 2 J-1,IP1 CS-COSIW*LCJ)/VSCJ)) SN-SINCW*L(II/VS(I)) OEN-ZFCJI·CS+ZL*SN*CO.,1,) IFICABSCDEN).LT,1,E-30) GO TO 6

Z ZL-ZFCJI*'ZL*CS.ZFCII*SN*CO.,l.I)/OeN :. ZL-ZL/ZFC IP)

ZR-Cl.,O.O)*ZOR JFIJP,EQ,N) GO TO , JP1-N-IP DO 4 II-l,IP1 J-N-II.1 CS-COSCW*L(II/VS(J)) SN-SINCW*L(II/VS(I)) OEN-ZFCII*CS.ZR*SN*IO"l.1 IFCCA8SCDEN),LT,l,E-30) GO TO 6

• ZR-ZFCI)*CZR*CS.ZFCI)*SN*CO.,l.))/DIN , ZR-ZR/ZFIIP)

RETURN 6 10-1

RETURN END

-OPTIONS IN EFFECT* .IO,EBCOJC,SOURCE,NOLIST,NOOECK,LOAD,NOHAP 'OPTIONS IN EFFECT- NAME - ZLZR , LINECNT • '6 _5TATI5TIC5* SOURCE STATEHENTS • 31,PROGRAM 51ZE - 1670 -STATI5TIC5* NO DIAGNOSTICS GINERATEO

-o ...,

Page 110: STRUCTURE AND PROPERTIES OF SPUTTERED ZnO TRANSDUCERSdigitool.library.mcgill.ca/thesisfile47721.pdf · STRUCTURE AND PROPERTIES OF SPUTTERED ZnO TRANSDUCERS ... Basic Equations The

0001

0002 000) 0001t 000' 000& 0007 00011 0009 0010 0011 0012 Oou 0014 OOU DOIt> 0017 00111 0019 0020

0021

0012

0023

SUIRaUTINE SOURCE IISS,RNI C SUI~OUTINE saUlCE CALCULATES TUNING ILEMENT AND. C MRITES PlDPER HEADING OF PAGE

- C eOMMON IILKI/IE,IS,ZSO,IT.XT,F,F1,IS COMPLIX II,ZS,Y,lSS,lSO lS.ZSS/RN GO Ta 111,11",,441 ,IS

11 MRITII&,lOOI RITURM

Il WRITII&.2001 ISS RITURN J, Y·l./ZE IT·-AIMAGIYI I·IT/RN WRITII&.IOOI 155,Fl,1 RITURM

44 xT.-AIMAGIZII X·XT.RN WRITII&.4001 ZSS,Fl.X RITURN

100 FORMATI'l',IOX, 'CONJUGATE MATCH TRANSOUCER LOSS'I 100 FO~MATI'l',IOX"UNTUNIO TRANSDUCIR LOSS'I

a J1X.'SOURCE IMPeDANCI .',2F11,4' 100 FO~MATI'l',IOX,'SHUNT TUNID T~ANSDUCIR LOSS'I

a J1X,'SOURCE IMPIDANCE .',2F12,41 a Jlx,'TUNING FRIQ. ·',11S,4,'X, a 'TUNING suseEPTANCE .',E1S.41

400 FORMATI'1',JOX,'SERI15 TUNED T.ANSDUCIR LOSS" a J1X.'SOURCE IMPIDANCI .',IFll,41 a J1X,'TUNING FRIQ •• ',llS,4.,X, a 'TUNING REACTANCI .',115.41

END

-OPTIONS IN !FFICT* ID.EICDIC,SOURCE,NOLIST,NODICK,LOAO,NDMAP *OPTIONS IN IPFleT* NAME. SOURCE • LINICNT • 5& *STATISTles. SOURCI STATIMINTS • II,PROGRA" SIZI • 1072 -STATISTles* NO DIAGNOSTICS GINERATID

0001

OOOl 0003 0004 OOO~ 000t> 0007 0008 0009 0010 0011 0012 0013 0014 0015 DOIt> 0017 0018 0019 0020 OOZI 0022 Don OOZ ..

5USROUTINE TUNE e SUIROUTINE TUNE CALCULATES THE 'TUNEDI INPUT C IMPEDANCE OF THE TRAN5DUCER. C

COMMON 18LK"IE,lS,lSO,8T,~T,F,Fl,IS COMPLEX lE.1S,150,Y GO Ta 111,22"3,441,15

11 U-CONJGCZEI 22 UO-U

RElURN 3J IFIBTI 1.1.2

1 &-eUF/Fl GO TO ,

2 a-aUFl/F ) Y-l.llE+IO.,l.'*&

ZE-l./Y Y-l.11S+10.,1.I*B UO-l./V RETURN

44 IFIXTI 'u4,' 4 X-XUF/Fl

GO TO 6 , XaXUFl/F 6 ZE-ZE+IO.,l.I*X

Z50-Z5+10.,1.I*X RETURN END

-OP1ION5 IN EFFECT. IO.EBCDIC,50URCE,NOLI5T.NODECK,LOAO.NOHAP -OPTIONS IN EFFECT. NAHE - TUNE • LINECNT - '6 .SIATISTICS* SOURCE STATEHENTS - 24.PROGRAM SIZE _ -ST4TISTICS. Na DIAGNOSTICS GENERATED

9&6

-o w

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104

REFERENCES

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