metal lo graphic preparation of mmc

22
P.Merle et al. MMC-Assess – Thematic Network 0/20 M M e e t t a a l l l l o o g g r r a a p p h h i i c c Pr r e e p p a a r r a a t t i i o o n n  o o f f M M e e t t a a l l M M a a t t r r i i x x C C o o m m p p o o s s i i t t e e s s  MMC -Assess Thematic Net wo rk    V   o    l   u   m   e    3 P.Merle et al .

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8/3/2019 Metal Lo Graphic Preparation of MMC

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P.Merle et al. MMC-Assess – Thematic Network 

0/20 

MM ee ttaa ll lloo gg rraa pp hh iicc Prree pp aa rraa tt iioo nn  oo ff MM ee ttaa ll MM aa tt rr iixx CC oo mm pp oo ssii ttee ss MMC -Asse ss The ma tic Netwo rk 

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P .Mer le e t a l .

8/3/2019 Metal Lo Graphic Preparation of MMC

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C O N T E N T  

AA6061/ Al2O3 /10-22p...................................................................................................2 

A359/SiC/22p ..................................................................................................................2 

AA2XXX / SiC / 25p .......................................................................................................4 

AlSi7/SiC/(50+16)p-bimodal .........................................................................................5 

Dispal...............................................................................................................................6 

AA 357 / C-KC139 /UD or laminates...........................................................................8 

AA1099 / Al2O3 Nextel 610 / 50f-UD..........................................................................9 

AlZn6Mg / Al2O3 Altex/UD50f .................................................................................10 

Carbon fiber reinforced magnesium alloys ..............................................................11 

Magnesium/ C-T300 /50f-UD......................................................................................12 

Micrographs of C/Mg-composites with Al-content in the magnesium matrixand without...................................................................................................................13 

Micrographs of C/Mg-composites with Al2O3 particles as spacers.....................14 

Cu-C (SFRM)// vol. 44% ..............................................................................................15 

Cu-C (CFRM)// vol 40, 50,60% ...................................................................................15 

Stainless Steel AISI 316 / 10-20 Vol.% Al2O3 ...........................................................16 

Stainless Duplex Steel (UNS 31803) + 30 w.% Cr3C2 ..............................................17 

Titan-alloys / continuous SiC fibre ............................................................................19 

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AA6061/ Al2O3 /10-22p

A359/SiC/22p

T1,T4 or T6 condition.

POLISHING CONDITIONS

• Automatic polishing. MECAPOL P320 machine with rotating polishing disk +PERE rotating

specimen holder

• Polishing cloths and diamond pastes PRESI (http://www.presi.com)

Table 1:Polishing stages of AA6061/ Al2O3 /10-22p and A359/SiC/22p

Stage

N°Support Abrasive

Force*

(daN)

Disc

Rotating

speed (rpm)

Specimen

Rotating speed

(rpm)

Time

(min)Lubricant

1 paper SiC P400 6 150 100 1 water

2 paper SiC P800 6 150 100 1 water

3 paper SiC 1200 6 150 100 1 water

4

Polishin

g cloth

RAM

diamond

paste 6?m

LD33

1spray/45

sec

6 150 100 5

GH

(2drop /

5s)

5

Polishin

g cloth

RAM

diamond

paste 3?m

LD33

1spray/45

sec

6 150 100

1

+

30”

GH

(2drop /

5s)

6

Polishin

g cloth

SUPRA

Suspensio

n SPM

1/3 SPM+

2/3 H2O

1drop/sec

6 150 100 3 ///

* Pressure of 0,15 MPa for typical 32 mm diameter polish 

Fig.1:AA6061/ Al 2O3 /10p (Duralcan W6A10A)

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Fig.2: AA6061/ Al 2O3 /22p (Duralcan W6D22A)

Fig.3: A359/SiC/22p (Duralcan F3S.20S)

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AA2XXX / SiC / 25p

POLISHING CONDITIONS

• Manual polishing with rotating disk (? 300mm)• All grinding and polishing products purchased from Struers (http://www.struers.com)

Table 2:Polishing stages of AA2XXX / SiC / 25p

Stage N° Support AbrasiveDisc Rotating

speed (rpm)

Time

(min)Lubricant

1 paper SiC 180 300 1 water

2 paper SiC 320 300 1 water

3 paper SiC 500 300 1 water   G  r   i  n   d   i  n  g

4 paper SiC 1200 300 2 water

1

Polishing

cloth

DP-Plan

diamond paste

6?m SYNXI150 2-3

DP-Blue

(DEPIF)

(1drop / 3s)

2

Polishing

cloth DP-

MOL

diamond paste

3?m SYNTE150 2-3

DP-Blue

(DEPIF)

(1drop / 3s)   P  o   l   i  s   h   i  n  g

3

Polishing

cloth OP-

Chem

OP-S

Suspension150 3-4 ///

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AlSi7/SiC/(50+16)p-bimodal

POLISHING CONDITIONS

• Polishing and grinding by Planopol-3 with Pedemax-2 (STRUERS)

Table 3:Polishing stages of AlSi7/SiC/(50+16)p-bimodal

Stage

Nr. Support 

Abrasi

vePressure

Disc Rotating

Speed

(rpm)

Specimen

Rotating

Speed

Time

(min)Lubricant

1Diamond

disc

Piano

220F=170N 150 110

to

plainWater

2 Largo-disc 15µm F=170N 150 110 8-10min

Diamond-suspension

3

Polishing

Cloth

PAN

15µm F=170N 150 1105-6

min

Diamond-

suspension

4

Polishing

Cloth

DUR

6µm F=170N 150 110 6minDiamond-

suspension

5

Polishing

Cloth

MOL

3µm F=170N 150 110 6minDiamond-

suspension

6

Polishing

Cloth

OP-CHEM

OPS or

OPUF=65N 150 110 2min

100ml OPS

+1ml H2O2 

+1ml

Ammoniak

Fig.4: AlSi7/SiC/(50+16)p-bimodal

FOR MORE INFORMATION

Heidemarie Knoblich, [email protected]

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Dispal

DISPAL M1xx (M = reactive milling); AA1085 + submicron Al4C3/Al2O3 

DIS PAL M2xx (M = reactive milling); AlSi(12-20) + submicron Al4C3/Al2O3

DISPAL A2xx (A = RS-powder by spraying); AlSi(12-40) + further alloying elements

DIS PAL S2xx (S = spray compaction); AlSi(12-40) + further alloying elementsDISPAL S7xx (S = spray compaction); AlZn(6-15) + further alloying elements

POLISHING CONDITIONS 

• Automatic polishing with RotoPol-31 + RotoForce-4 top (rotating polishing disk (? 200 or

300 mm) and rotating specimen holder of ? 100mm)

• Polishing cloths: Struers (http://www.struers.de)

• Diamond pastes Wirtz-Bühler (http://www.buehlerltd.com), Fig.1

Table 4:Polishing stages of Dispal

Stage N° Support Abrasive

Disc Rotat

ing speed

(rpm)

Force*

[N]

Time

[min] Lubricant

1 SiC 80 120  0.25 water

2 SiC 220  90  0.25 water

3 SiC 800  90  0.25 water

4 SiC 1200 90  0.25 water   G  r   i  n   d   i  n  g

5

SiC-Paper

on MD-

Fuga

SiC 2400

150 

90 0.25

1 Polishingcloth

MD-DAC

diamond paste 6µm 

90  5 Struers blue

2

Polishing

cloth MD-MOL

diamond paste 3

µm 60  5

Struers

red 

3

Polishing

cloth MD-MOL

diamond paste 1

µm 60  5

Struers

red    P  o   l   i  s   h   i  n  g

4Polishing

cloth MD-NAP 

Mastermet-

Polish suspension

Fa. Wirtz Buehler(SiO2; 0,06 µm) 

150 

60 2

* Pressure of 0,15 MPa for typical 32 mm diameter polish

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Fig.5:DISPAL S250 (AlSi20Fe5Ni2, spray compacted and extruded, LT)

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AA 357 / C-KC139 /UD or laminates

POLISHING CONDITIONS

• Cutting under water using a diamond cut-off wheel.• Polishing with rotating (? 230mm) polishing plate. Polishing cloths and diamond pastes :

PRESI (http://www.presi.com)

STRUERS (http://www.struers.com),

LAM PLAN (http://www.lamplan.fr),

TRIEFUS France (28011 CHARTRES CEDEX, Tel : 02-37-24-40-40)

Table 5:Polishing stages of AA 357 / C-KC139 /UD or laminates

Stage

N°Support Abrasive Supplier

Disc Rotating

speed (rpm)

Time

(min)Lubricant

1 paper SiC 320 PRESI 250 1-2 water

2 paper SiC 600 PRESI 250 1-2 water

3 paper SiC 1200 PRESI 250 1-2 water

4 Flocked

cloth PSF

(TRIEFUS)

diamond

paste

6?m

LAM

PLAN

250-300 1-3 alcohol

5 Woven

cloth 432

(LAM

PLAN)

diamond

paste

3?m

LAM

PLAN

250-300 1-3 alcohol

6 Flocked

cloth TF-R(PRESI)

Diamon

d paste0.25 ?m

LAM

PLAN

250-300 1-3 alcohol

Cleaning with alcohol in an ultrasonic bath and drying after stages 3, 4, 5, 6

Fig.6:AA 357 / C-KC139 /UD or laminates

FOR MORE INFORMATIONS

[email protected] 

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AA1099 / Al2O3 Nextel 610 / 50f-UD

POLISHING CONDITIONS

• Automatic polishing with rotating polishing disk ( ? 200mm) and rotating specimen holder(? 100mm)

• Grinding, polishing cloths and diamond pastes of

Table 6:Polishing stages of AA1099 / Al2O3 Nextel 610 / 50f-UD

Stage

N°Support Abrasive

Pres-

sure

(bar)

Disc

Rotation

(rpm)

Specimen

Rotation

(rpm)

Time

(min)Lubricant

1 SiC 320 1 flat

2 SiC 600 1 1

3 SiC 12001

14

Paper1 

Dia-

mond

disc 2

SiC 4000 1

PIANO

1202

0.6 1 150110

2

water

5Polishing

cloth

RAM 1

LARGO

disc 2

diamond paste

6?m DESY 1

9µm 20.6 150 110 3-5

PM 1

(1drop / 3s)

suspension 2

6Polishing cloth

RAM 1

DAC 2

diamond paste 3?m

DESY 1 0.6 150 1103-5

PM 1

(1drop / 3s)

suspension 2

7

Polishing cloth

SUPRA1

MD-Chem 2

Suspension

25%SPM 1 

+75%H2O;

OPS or OPU 2

0.6 150 110 1-2

As above 1 or

100ml OPS 2 

+1ml H2O

+1ml NH3 

8 1Polishing cloth

HS 1As above 1 0.4 150 110 1 water

1 PRESI (http://www.presi.com), 2 STRUERS (http://www.struers.de)

Fig.7:AA1099 / Al2O3 Nextel 610 / 50f-UD

FOR MORE INFORMATION:

1 [email protected]; 2 [email protected]

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AlZn6Mg / Al2O3 Altex/UD50f

POLISHING CONDITIONS

• Automatic polishing with rotating polishing disk (? 300mm) and rotating specimen holder(? 160mm)

• Polishing cloths: Struers (http://www.struers.de)

• Diamond pastes Wirtz-Bühler (http://www.buehlerltd.com), Fig.1

Table 8:Polishing stages of AlZn6Mg / Al2O3 Altex/UD50f

Stage

Support Abrasive Pressure

(bar)

Disc Rotating

speed (rpm)

Specimen

Rotating speed

(rpm)

Time

(min)

Lubricant

1 paper SiC 180 1 - 5 300 150 until

flat

water

2 Largo °

Honey-

comb

disc

diamond

suspensi

on 9?m

1 - 5 300 150 3 Dialub sw

3 Texmet

W *

diamond

suspensi

on 3?m

1 - 5 150 150 3 Dialub sw

4 Polishin

g cloth F

*

Masterm

et II *

1 - 5 150 150 2.1 water

FOR MORE INFORMATIONS

[email protected]

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Carbon f iber reinforced magnesium alloys

• Fiber: Tenax HTA 5331, Toray T300J, Toray T800H, Torray T1000

Fiber coating: TiN and uncoated

• Matrix: cp-Mg, AM20, AM50, AZ91

POLISHING CONDITIONS

• Manuel polishing with a very low pressure

• The same preparation conditions like mentioned in the table below are used for the

combination of all fiber matrix types listed above:

Table 9:Polishing stages of Carbon fiber reinforced magnesium alloys

Stage

No Support Abrasive Pressure

Disc Rotating

speed (rpm)

Time

(min)Lubricant

1 Paper SiC 320 Low 300 1 Ethanol

2 Paper SiC 500 Low 300 1 Ethanol

3 Paper SiC 800 Low 300 1 Ethanol

4 Paper SiC 1200 Low 300 1 Ethanol

5 Paper SiC 2400 Low 300 1 Ethanol

6 Paper SiC 4000 Low 300 1 Ethanol

7 Polishing

Cloth

MOL*

Dp

suspen-

sion 3

µm

(Samte*)

Low 300 5-10 Struers Lubricant red*

+ blue*

* Products of Struers (www.struers.de)

Comment : In the case of Al2O3 particles as spacers for producing graded carbon fibre

reinforced magnesium alloys, the metallographic preparation stays the same

FOR MORE INFORMATIONS

[email protected]

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Magnesium/ C-T300 /50f-UD

POLISHING CONDITIONS

• Automatic polishing. MECAPOL P320 machine with rotating polishing disk +PERE rotatingspecimen holder

• Polishing cloths and diamond pastes PRESI (http://www.presi.com)

Table 10:Polishing stages of Magnesium/ C-T300 /50f-UD

Stage

Support Abrasive Force*

(daN)

Disc Rotating

speed (rpm)

Specimen

Rotating speed

(rpm)

Time

(min)

Lubricant

1 paper SiC P240 6 150 100 2 EXXSOL

D80

2 paper SiC P600 6 150 100 2 EXXSOLD80

3 paper SiC 1200 6 150 100 2 EXXSOL

D80

4 Polishin

g cloth

RAM

diamond

paste

6?m

PM

6 150 100 5 EXXSOL

D80 (1drop

/ 2s)

5 Polishin

g cloth

RAM

diamond

paste

3?m

LD33

6 150 100 3 EXXSOL

D80 (1drop

/ 2s)

** Pressure of 0,15 MPa for typical 32 mm diameter polish 

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Micrographs of C/Mg-composites with Al-content in the

magnesium matrix and without

The two SEM micrographs show composites with a Tenax HTA 5331 carbon fibre (similar to

Toray T300J) as reinforcement and two different magnesium matrix alloys. On the left picture

micrograph you see the fibres in a pure magnesium matrix (cp-Mg). On the right micrograph

the fibers are infiltrated in a magnesium matrix with an aluminum content of 5% (AM50). To

make the fiber/matrix-interface better visible the matrix has been e tched for 15 seconds with 2%

HNO3. On the right picture micrograph plate shape Al2MgC2 precipitates can be seen at the

fiber/matrix-interface.

Fig.7: Tenax HTA5331/cp-Mg (SEM) Tenax HTA5331/AM50 (SEM)

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Micrographs of C/Mg-composites with Al2O3 particles as spacers

The two SEM micrographes show composites with a pure magnesium matrix (cp-Mg) andToray T300J fibres as reinforcement. The Al2O3 particles are used as spacers to get a graded

fibre volume fraction. On the left micrograph on the bottom there are no Al2O3 particles and

the composite has a fiber volume fraction of about 60%. Only on top of this micrograph a few

Al2O3 particles (white) are visible. One the right micrograph the fiber volume fraction is about

30% and a lot of Al2O3 are visible in white color.

Fig.7: T300J/cp-Mg composite with a very low content of Al2O3 particles on top of the

micrograph (SEM)

Fig.8: T300J/cp-Mg composite with high content lot of Al2O3 particles (SEM)

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Cu-C (SFRM)// vol. 44%

Cu-C (CFRM)// vol 40, 50,60%

POLISHING CONDITIONS

• Polishing and grinding by hand. The time for grinding depends on the surface morphology

which was determined by a visual control of the surface.

Table 10:Polishing stages of Cu-C (SFRM)// vol. 44% and u-C (CFRM)// vol 40, 50,60%

Stage

N°Support

Abrasi

ve

Pressure

(bar)

Disc Rotating

speed (rpm)

Specimen

Rotating speed

(rpm)

Time

(min)Lubricant

1 paper SiC 320 - ~750 - dep. water

2 paper SiC

1200

- ~750 - dep. water

3 paper SiC

2400

- ~750 - dep. water

4 paper SiC

4000

- ~750 - dep. water

5 Polishing

with felts

and/or

1µm

- ~750 - dep. alcohol

Fig.9: Cu-C-SFRM (x-y-direction) Cu-C-SFRM (z-direction)

100 µm 

100 µm 

FOR MORE INFORMATIONS

[email protected]

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Stainless Steel AISI 316 / 10-20 Vol.% Al2O3

POLISHING CONDITIONS

• Manual polishing with rotating polishing disk (? 250mm in stages 1-5 and ? 200mm instages 6-8). Duration of each stage - polishing until apparent scratches from the previous

stage has been disappeared (Table 1. and Fig. 1.).

• Abrasive papers: Buehler (http://www.buehlerltd.com/)

• Polishing cloths and diamond pastes: Struers (http://www.struers.com/)

Table 11:Polishing stages of the AISI 316 + 20 Vol.% Al 2O3 PRM MMC.

Stage

No.Support Abrasive

Disc Rotating

speed (rpm)Lubricant

1 paper SiC 60 300 water2 paper SiC 320 300 water

3 paper SiC 400 300 water

4 paper SiC 600 300 water

5 paper SiC 2400 300 water

6polishing cloth

DP-Moldiamond paste 3? m 70 etanol + glycerin

7polishing cloth

DP-Napdiamond paste 1? m 70 etanol + glycerin

8polishing cloth

DP-Nap

magnesium oxide

(MgO)70 water

Fig. 10:Polished microstructure of AISI 316 + 20 Vol.% Al2O3 PRM MMC (200x).

FOR MORE INFORMATIONS

[email protected],[email protected]

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Stainless Duplex Steel (UNS 31803) + 30 w.% Cr3C2

POLISHING CONDITIONS

• Manual polishing with rotating polishing disk (? 250mm in stages 1-5 and ? 200mm

in stages 6-8). Duration of each stage - polishing until apparent scratches from the

previous stage has been disappeared, Table 1.

• Polished microstructure, Fig. 1.

• • Abrasive papers: Buehler (http://www.buehlerltd.com/)

• • Polishing cloths and diamond pastes: Struers (http://www.struers.com/)

ETCHING  

Etching solution Aqua regia + glycerin. Etched microstructure, Fig. 2.

Table 12:Polishing stages of composite sample.Stage

No.

Support Abrasive Disc Rotating

speed (rpm)

Lubricant

1 paper SiC 60 300 water

2 paper SiC 320 300 water

3 paper SiC 400 300 water

4 paper SiC 600 300 water

5 paper SiC 2400 300 water

6 polishing cloth

DP-Mol

diamond paste 3?m 70 etanol + glycerin

7 polishing clothDP-Nap diamond paste 1?m 70 etanol + glycerin

8 polishing cloth

DP-Nap

magnesium oxide

(MgO)

70 water

Fig. 11: Polished microstructure of Duplex Stainless Steel+30 w.% Cr3C2 PRM MMC (200x).

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Fig. 12:Polished+etched microstructure of Duplex Stainless Steel+30 w.% Cr3C2 PRM MMC (200x).

FOR MORE INFORMATIONS

[email protected],[email protected]

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Titan-alloys / continuous SiC fibre

CUTTING CONDITIONS

• low speed precision saw• resin bonded diamond wheel, thickness 0.6 mm, diamond grain size ca. 126 µm

POLISHING CONDITIONS

• Automatic polishing device, rotating disk (diameter 300 mm), rotating specimen holder

(diameter 140 mm)

• Polishing cloths: Struers (http://www.struers.de)

• Diamond pastes Wirtz-Bühler (http://www.buehlerltd.com), Fig.1

Table 13:Polishing stages of Titan-alloys / continuous SiC fibre

Stage

No.

Support Abrasive Lubri-

cant

Load

(N)

Disc

Rotating

Speed

(rpm)

Specim

en

Rotatin

g

Speed

(rpm)

Time

(min)

1 diamond

pad

Ni-

 bonded

diamond

grain

size

20 µm

water hand 150 2

2 SiC-paper

SiC 800 water hand 150 1

3 SiC-

paper

SiC 1200 water hand 150 1

4 synthetic

woven

silk

polishin

g

cloth

diamond

grain

size

3 µm

alcoholic

suspensi

on

90 150 140 6

5 synthetic

leather

polishin

g

cloth

SiO2

0,04 µm

colloidal

silica

suspensi

on

pH 9.8

40 150 140 1

ETCHING, ALTERNATING WITH POLISHING, STAGE 5

100 ml water, 15 ml nitric acid (65 %), 10 ml hydrofluoric acid (40 %) for several seconds at

room temperature

MORE INFORMATION

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Fig. 13: cross section of a metal matrix composite Ti (Timetal 834)/ SiC (SCS-6) fibre

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MMC-Assess Publications

Volume 1: Glossary of Terms sp ecific to Metal M atrix Compo sit es

Volume 2: Thermal Treatm ents of A ge-hardenable Metal M atrix Compos ites

Volume 3: Metallographic Preparation of M etal M atrix Compos ites

Volume 4: X-R ay Computed Tomography on M etal Mat rix Composit es

Volume 5: Qualit y control and nondestructiv e tests in metal mat rix composit es

Volum e 6: Machining guidelines of Al/SiC parti culate MM C 

Volume 7: Thermophy sical Properties of M etal M atrix Compos ites

Volume 8: Guidelines for joining of m etal m atrix composit es

Volume 9: Bomding and interface format ion in M etal M atrix Compo sites

Copyright: MMC-Assess Consortium, August 2000Content: P.Merle

Design: P.Prader 

Contact:  Insitut e of M aterials Science and Testing – Vienna Univ ersity of Technology

[email protected]: http://mmc-assess.tuwien.ac.at/