TN-12 Principles and Practice for Metallography

Microsoft Word - TN-12 Principles and Practice for Metallography 10 Polishing

5. Report
.
3.
Copyright(C)2005 R&B Inc. Al right reserved 3 www.radnb.co.kr
I.
Metallography .

.
.
1.
. ,
polishing .
.
.
2.
.
, , ,
.
.
.
3.
.
.
. (Deformation,
Scratch, Pull-out, , Smearing, Relief, Edge rounding, )
.
4.

.
. grinding grinding polishing
.
II. Metallography
1.
Metallography
. ,
, , ( ) .
R&D
.
2.
Metallography
. Metallography
‘Science’‘Art’
.
Metallurgist, Metallographer, Technician
. Metallurgist
Metallography .
Metallographer
. Technician
. .
3. Metallography
,
, ,
.
4. Metallography lab.
: .

. sample
.
:
. vibrating scriber
, mounting sample tag mounting .
, .
Report form .
- : , , , ,
- : , , , ,
- : , , ,
- : , Grain size, , , ,
: Metallography .
- Macro, Microhardness test, Inclusion rate, Grain size , Image analysis -
.
5. Report
, , nega. Film .
6.
:
. .
7.
, , , , , .
8.
E-7 Standard Terminology Relating to Metallography
E-45 Standard Practice for Determining the Inclusion Content of Steel
E-112 Standard Test Methods for Determining Average Grain Size
E-340 Macroetching Metals and Alloys
E-381 Standard Method of Macrotech Testing Steel Bars, Billets, Blooms, and Forgings
E-384 Test for Microhardness of Materials
E-407 Microetching Metals and Alloys
E-562 Recommended Practice for Determining Volume Fraction by Systematic Point Count
E-588 Recommended Practice for Detection of Large Inclusions in Bearing Quality Steel by the Ultrasonic
Method
E-768 Standard Practice for Preparing and Evaluating Specimens for Automatic Inclusion Analysis of Steel
E-807 Standard Practice for Metallographic Laboratory Evaluation
E-883 Standard Guide for Reflected-Light Photomicrography
III.
1.
Metallography .
Lapping, Grinding, Polishing 3
.
Lapping
rolling chip
.
. Ceramic
.
Grinding

. Polishing grinding .
Polishing
grinding scratch
.
.
.
(Sectioning or cutting) : Abrasive cutter, diamond cutter
. .
Rough grinding : Belt surface disc grinder
.
Mounting : .
Fine grinding : sand paper rotating disc .
P #1000 ( #600, USA) sand paper .
lapping machine
.
Polishing : (#1000 sand paper) polishing cloth
polishing .
sand paper, Polishing cloth
Etching : Polishing .
.
Photographing : .
2. (Sectioning and cutting)
abrasive cutoff machine, band saw,
diamond saw . ,

. .
.
,
.
.
, fracturing, sawing, abrasive wheel cutting .
– .
Fracturing – .
Sawing – hacksaw
.
Abrasive cutting – ‘Abrasive wet cutting’.
abrasive() binder cutting wheel
()
wheel
.
. Wheel
wheel . factor abrasive
size size sample damage . abrasive
wheel ceramic
bakelite binder diamond wheel .
Wheel wheel .
Diamond wheel
diamond CBN wheel .
binder abrasive particle . wheel
cutoff wheel diamond wheel.
Wheel metal core resin metal bond wheel
loading dressing low high speed saw
. high concentration diamond wheel
, low concentration diamond wheel . high speed
saw ,
, circuit board diamond saw . Diamond saw
200RPM wheel wheel
0.2~0.4mm 3~6″ . wheel
diamond CBN wheel binder .
metal binder bakelite ( ) binder .
.
Metallic binder ceramic bakelite binder
sintered carbide . CBN wheel bakelite binder
.
Diamond cutting machine Diamond wheel & cutting oil
1. Diamond wheel
(RPM) (gf) Wheel (Grid/Con.)
Soft/brittle <300 <100 Fine/low
B-composite Very brittle 500 250 Fine/low
Ceramic fiber Very brittle 1000 500 Fine/low
Brittle 1000 500 Fine/low
Friable/brittle >1500 >500 Fine/low
Alumina Hard/tough >1500 >500 Medium / low
Zirconia Hard/tough >3500 >800 Medium/low
Metal matrix - >3500 >500 Medium/high
- Medium/high
Abrasive wheel
abrasive cutoff wheel bakelite bonded silicon carbide
bakelite binder aluminium oxide(alumina) .
SiC alumina wheel wheel
. wheel diamond wheel .
alumina wheel , , ,
CBN wheel .
Alumina wheel resin rubber bond type resin bond wheel dry cutting
rubber bond wheel wet cutting . rubber bond wheel
hood .
Wheel wheel hard wheel
soft wheel . Soft wheel rubber
bond ,
hard wheel
.
wheel .
2. Oxide Wheel
Wheel
Soft non-ferrous SiC/ Rolled rubber
Hard non-ferrous Alumina/ Rubber resin
HRC 45 Soft ferrous Alumina/ Rubber resin
HRC 45 Hard ferrous Alumina/ Rubber resin
Super alloys High Ni-Cr alloys SiC/ Rolled rubber
Abrasive cutting machine abrasive wheel
.
Water-soluble oil coolant
, .
Coolant wheel cutting . coolant
hose cutting .
Wheel
. wheel
.
abrasive particle
abrasive particle .
Cutting speed, load, diamond concentration, diamond size, bonding material, cutting fluid
.
- Speed : 50~5000RPM
- Load : 10~1000 gf ( Ceramic , , )
- Diamond concentration ( Low and high)
ceramic low
high concentration .
- Bond material
- Cutting fluid
Oil base blade metal .
Water base ceramic porous cutting .
.
wheel . Wheel
clamping . wheel
wheel wheel
.
Wheel wheel wheel
. wheel 1mm wheel 0.2mm
0.55mm. Weller
.
Abrasive cutoff wheel Spark erosion Diamond saw
Electrolytic Copper 250 85 50
Carbon steel 125 50 25
Austenitic stainless steel 85 50 30
Titanium 150 75 45
3. Mounting
grinding polishing
mounting . Mounting .
, ,
.
.
Mounting hot compression mounting cold mounting .
. Hot mounting
mounting press , cold mounting castable
. Mounting grease
.
polishing polishing .
mold mounting .
. Mounting
Hot compression mounting
mounting press
.
.
mold
.
phenolic , acrylic , epoxy .
phenolic . Diallyl phthalates epoxy resins
mounting . acrylic
.
.
mounting .
4. Compression Mounting
Phenolic Acrylic Epoxy Diallyl Phthalates

(g/cc) 1.4 0.95 1.75-2.05 1.7-1.9
,,
0.006 - 0.002 0.001-0.003

Molding 150-165C 120-140C - 143-177C 160-177C
Molding 3050-4000psi - ~3000psi ~3500psi
Curing 90-120 sec. 120-240 sec 90-120 sec. 90-120 sec.
HRM 113 HRM105 HRM103
Cold mounting
Hot mounting
mold
. 150
hot compression mounting .
ceramic . Cold mounting
curing microwave
. .
.
Epoxy
Cold mounting
curing . epoxy .
Acrylic
curing . .
acrylic .
Polyester
Cold mounting .
5. Cold mounting
Epoxy Acrylic Polyester resin

28 28 38
HRM 56.8+/-7.7 HRM 71.9+/-3.1 HRM 89+/-2.3
mounting , mounting
, , . Hot mounting mounting
. cold mounting series
. mounting press mounting
. Mounting mold (Release agent)
. mold 3mm
.
cold mounting vacuum impregnation .
cold mounting resin
Vacuum impregnation
, coating vacuum impregnation
mounting .
.
. Mounting trouble shooting
Mounting .
1) Thermosetting mounting defect
: edge
: mold
: Mold .
Edge shrinkage
: plastic
: Molding mold .
Circumferencial Split
: Molding
: Powder powder pressing .
Burst
:
:
: Curing .
Unfused
: molding pressure curing
: molding pressure curing .

: , curing cooling
:
mold
Bulging
:
: curing .
Void
:
: , ,
: , ,
Mounting ram
: , , ,
: mounting process .
crack
: .
2) Cold mounting defect
:
: Oven cure , resin hardner
: Air cure , oven cure , resin/ hardner .
Bubbles
: Resin hardner agitating
: .
Soft mount
: Resin- hardner
: .
4. Grinding/Polishing
.
Metallography know-how
. polishing
. Grinding/polishing
.

.
.

.
Grinding
Grinding paper wet grinding . Wet
grinding
.
Grinding 45-90 . grinding
scratch polishing
scratch .
.
. Grinding SiC, emery, alumina , diamond, boron carbide
.
SiC , .
Aluminium oxide SiC ,
, .
grinding machine
60mesh 120,
240, 320, 400, 600mesh sand paper .
grit size
, band saw
grinding grit grit # 60 #120 , abrasive
cutter 120-240 grit, wire saw
diamond saw 320-400 grit
grinding .
SiC emery . dry grinding
wet grinding kerosene
.
Emery aluminium oxide iron oxide SiC alumina ,
SiC
, SiC .
Polishing
600grit (P1000) grinding , scratch , .
Polishing coarse fine coarse (rough) polishing 30~1 micron
fine polishing 1 micron .
Rough polishing 1 low nap nap
cloth , fine polishing low-medium, high nap cloth . Polishing
grinding . polishing
. damage
edge rounding, relief .

.
Metallography polishing
polishing cloth
.
polishing factor
comet tail, pull out, edge rounding
. polishing (Polishing
cloth ) . wheel
. . grinding sand paper
90 . sand paper
.
.
(Abrasive)
Diamond powder rough grinding oxide
polishing diamond .
2.5~3 polishing cloth
nap cloth .
(Grid/Grain size)
.
polishing
.
(Lubricant)
, ,
.
, smearing .
smearing ,
polishing .
abrasive
. . polishing cloth
.
cloth polishing .
scratch .

. .

grinding fine grinding
150RPM . holder
. .
polisher holder holder . grinding
holder disc
grinding . head disc
. head disc
. grinding inclusion
. grinding
,
.
. coating
. coating
coating coating
.

.
. 10psi (
30mm 4~5kgf ) 5
. .
, mounting .
mounting
. grinding
. ceramics,
minerals and composites CMP
nodular cast iron grinding inclusion
.

. relief edge rounding
.
.
Planer Grinding
Course grinding rough grinding
. polishing
.
silicon .
7. Planer Grinding
Grinding
120 or 240 grit SiC paper 800 1000grit
(silicon, alumina, barium titanate, plastic PCB's )
. Coating . 400 600 grit SiC 15 micron diamond lapping film .
. Ceramic
diamond lapping film .
Ceramics
15 30 micron diamond
metal mesh cloth .

Plastics SiC sand paper .
composite lapping film relief
.
European (P-grade) Standard grit Median diameter (Microns)
60 60 250
80 80 180
100 100 150
120 120 106
150 150 90
180 180 75
220 220 63
P240 240 58.5
Rough Polishing
planar grinding fine polishing .
rough polishing inclusion .
. 9 ~1micron diamond
. Polycrystalline diamond cutting edge
low napped cloth polycrystalline diamond
rough polishing .
9. Rough polishing
Polishing
6 , 1 diamond , nap cloth .
Ceramics Nap cloth polycrystalline diamond colloidal silica . CMP
Polymer composites Diamond lapping film
Nap polishing pads polycrystalline diamond colloidal silica

Plastics 800 1000 grit SiC abrasive paper
Plasma spray
Diamond lapping films nap polishing pad diamond
colloidal
Fine (Final) polishing
.
.
Polishing
Nap polishing pad colloidal alumina, silica . 30
Ceramics Nap polishing pads 1 um polycrystalline diamond colloidal silica
colloidal silica Polymer composites Fine abrasive diamond lapping films nap polishing pad
Nap polishing pad polycrystalline diamond colloidal silica
Diamond lapping films nap polishing pad
Plastics Alumina nap polishing pad
Plasma spray Diamond lapping film, nap polishing pad alumina colloidal silica
. Polishing cloth
Polishing cloth abrasive wool, cotton,
silk rayon .
plain back PSA () PSA polyester
. Slurry PSA back .
Metal mesh cloth
lapping/polishing
polyester cloth
Nylon cloth . Nap polishing
Non-textile cloth
polishing cloth non-woven type
break-in .
Nap cloth glass .
Polymer cloth
cloth polishing nap cloth .
High napped cloth
Micro polishing cloth
polishing cloth cotton rayon
nap 100% cotton 0.02”~0.03” rayon flock , rayon flock
cotton base 10% rayon 90% cotton . plastic, polishing
oxide powder diamond powder . 0.04” .
Super micro polishing cloth
Micro polishing cloth nap cloth polishing wool
glass, fiber optic, final polishing . oxide diamond
.
Acetate base cloth
Acetate polishing cloth cloth nap flock
.
loading glazing . , Al .
. Polishing
Alumina fine polishing 1, 0.3, 0.05 micron
suspension powder polishing . gamma alpha . Gamma
alpha (mohs 9.0) . (mohs 8.0). Gamma alumina cubic crystal
alpha alumina hexagonal . Fine polishing alumina
colloidal silica . Alumina
polishing . Alumina gamma (mohs
8) alpha (mohs 9, 2000 HV) phase fine polishing
SiC . cutting
metallographic application . Jell
alpha alumina calcining gamma alumina
. calcined 0.05 gamma alumina
5 . polishing
aluminum, tin, lead, copper and soft steels
scratch . alpha alumina (<0.5 )
final polishing . Jell alpha alumina suspension scratching,
cutting , , , suspensions . alumina suspension
trouble shooting

Suspending
100% cotton alcohol
polishing 10-15
relief Over polishing Final polishing
final polishing time
Scratches polishing pad pad
2
polishing pad guide-line polishing pad
Diamond cubic
grinding .
polycrystalline diamond rough polishing . Rough polishing
, 1micron alumina
diamond . Rough polishing diamond
scratch, , , , , ,
.
. Diamond aerosol paste
.
Polishing cloth diamond
, grinding diamond .
Polishing debris polishing .
Polycrystalline diamond synthetic natural mono-crystalline diamond
. cutting , , , blocky shaped,
hexagonal micro-crystallites, , mono-crystalline diamond 300%
.

Diamond Diamond suspension
Coarse scratches Pad polishing pad
Polishing pad softer polishing pad polishing pad guide-line
Diamond compound, diamond suspension polishing lubricant
Silica colloidal suspension final polishing diamond
scratch . polishing polishing agent
cloth . scratch
. SiC silica carbon .
hexagonal-rhombohedral 2,500 Hv.
edge cutting grinding . SiC cutting
. SiC 60grit 1,200grit size
abrasive grinding paper . Colloidal silica
final polishing chemical mechanical polishing (CMP)
fine , zeta potential .
polishing . Colloidal silica
polishing suspension. , ceramics, composites soft metals chemical
mechanical polishing (CMP) . 0.05 0.07
alkaline pH 9.5 . pH colloidal silica
suspension . Polishing diamond
mechanical . colloidal silica chemical mechanical polishing
ceramics minerals
. polishing 10-15
. colloidal silica .
12. Colloidal silica trouble shooting

10-15 pad
polishing
pH polishing suspension
scratching Silica cloth filtering colloidal silica filtering
magnesium oxide polishing
polishing . final polishing slurry
powder carbonates scratch
. polishing cloth cleaning 2%
HCl . .
iron oxide 3 micron rough polishing
chromic oxide 1, 0.05micron rough final polishing .
Cerium oxide 1 micron soft metal, , copper final polishing
. 6micron diamond polishing
.
13. Polishing
Alloy Condition Melting point (°C) Hardness ( Hv) Polishing rate
(/min)
Tin Annealed 231 9 9
Cadmium Annealed 321 22 14
Lead Annealed 327 5 7
Zinc Annealed 421 50 12
Magnesium Annealed 650 40 16
Aluminum alloy Heat treated 580-650 105 13
Aluminum alloy Annealed 580-610 40 8
Aluminum Annealed 660 25 9
Brass(40%Zn) Annealed 900-905 155 15
Brass(30%Zn) Annealed 915-955 95 14
Silver Annealed 960 30 12
Copper Annealed 1083 45 11
Austenitic steel (18%Ni-8%Cr)
Annealed 1400-1425 170 3
B.S 970:En2A steel
. Polishing
Grinding , Mayburg
polishing micron diamond paste .
grinding grit , , polishing rate
.
Case 1 : grinding polishing ,
polishing
T : polishing
f : polishing
a : Polishing rate
S0 : grinding (micron )
Sf : polishing (micron )
, 2 polishing , 1micron polishing , polishing
. ( steel , grinding grit : 600grit=30micron) f : polishing = 2, a : polishing rate =
1.2
Sf : polishing = 1
T = 2(1/1.2)(30/1)1/2 = 9.1min
polishing 4.5 .
Case 2 : grinding polishing , polishing
polishing grade
fmin = polishing Sf : polishing
- Polishing grade
)1/f
S2=(S0 x Sf 2 )1/f
S2 = polishing S0 : grinding
Sf : polishing f : polishing
- Polishing
fmin = polishing a : polishing rate, e = 2.72
grinding 600 grit (30) , polishing 1micron diamond
polishing ( steel , grinding grit : 600grit=30micron) .
fmin = ln(S0/Sf)
Sf : polishing = 1
fmin = ln (30/1) = 3.4 grade
3 polishing . polishing .
S1=(302 x 1 )1/3 = 9.4 micron polishing 9 micron
S2=(S0 x Sf 2 )1/f = 3.1 micron polishing 3 micron
T = (3 x 2.72 / 1.2) = 6.8min .
3 polishing , 9, 3, 1micron polishing 2 26

. Polishing
Coarse polishing relief formation nap , low nap medium nap cloth 6micon
diamond paste .
2 6 1micron diamond 3
1micron diamond paste polishing .
hand polishing comet tailing polishing
,
.
.
, spray gun .
Gun .
.
1 diamond polishing 2 fine polishing
, 0.3 0.05 micron alumina slurriy final polishing .
2 diamond polishing 0.05 micron alumina polishing final polishing .
final polishing .
Polishing
. alumina
.
.
.
. polishing
.
.
. 2 mount cavity holder crevice
tap
water . air .
.
final polishing . polishing
. colloidal silica alumina
polishing pad , , holder polishing 10-15
. . Pad
.
. trouble shooting .
14. trouble shooting

Alumina

Colloidal silica polishing polishing 10- 15 .
spot polishing
pit soluble
mount crack
oven
. polishing
15. Carbon composites
/
6 diamond on medium-nap pad 3-5 psi 3-5 minutes
1 diamond on medium-nap pad 3-5 psi 2-5 minutes
0.05 alumina on nap pad 3-5 psi 30-60 seconds
16. Silicon carbide fibers in a silicon nitride (5% Mullite) matrix
Cutting : fiber fine grit diamond blade
/
30 diamond on a metal mesh cloth 10-12 psi 5-10 minutes
6 diamond on a CERMESH pad Colloidal silica 10-12 psi 5-10 minutes
1 diamond on POLYPAD pad Colloidal silica 10-12 psi 5-10 minutes
Colloidal silica 10-12 psi 2-5 minutes
17. Boron-Graphite composites
/
18. Cast iron
/
320 grit SiC paper 400 grit SiC paper 600 grit SiC paper 800 grit SiC paper 1200 grit SiC paper
Water Water Water Water Water
5 psi 5 psi 5 psi 5 psi 5 psi
1 minute 1 minute 1 minute 1 minute 1 minute
3 diamond on POLYPAD pad 5 psi 3-5 minutes 1 diamond on TEXPAN pad 5 psi 3 minutes
0.05 alumina on napless pad 5 psi 15-20 seconds
19. 1095 Carbon steel (Pearlite and martensite phases)
/
120 grit SiC paper 240 grit SiC paper 320 grit SiC paper 400 grit SiC paper 600 grit SiC paper
Water Water Water Water Water
5-10 psi 5-10 psi 5-10 psi 5-10 psi 5-10 psi
1-3minutes 1 minute 1 minute 1 minute 1 minute
9 diamond on napless pad 5-10 psi 3-5 minutes
3 diamond on napless pad 5-10 psi 3 minutes
0.05 alumina on napped pad 5 psi 15-20seconds
20. Stainless steel
/
320 grit SiC paper 400 grit SiC paper 600 grit SiC paper
Water Water Water
6 diamond on napless pad 5 psi 3 minutes
1 diamond on napless pad Colloidal silica 5 psi 2 minutes
0.05 alumina on napped pad 5 psi 30seconds
21. Aluminum Aluminum
/
Paraffin wax water Paraffin wax water
Water
0.05 alumina on napped pad 5 psi 30seconds
22. Alumina Cutting : Fine grit diamond blade
/
6 diamond on napless pad Colloidal silica 10-12 psi 5-10minutes
1 diamond on napless pad Colloidal silica 10-12 psi 5 minutes
23. Zinc Zinc
/
Water Water Water
3 diamond on napless pad 5 psi 3minutes
1 diamond on napless pad 5 psi 90seconds
0.05 alumina on napped pad 5 psi 1minutes
. Trouble shooting
polishing .
1. Scratch ()
grinding/polishing . scratch
scratch ( scratch )
.

polishing cloth

a) b)
a) After PG scratches from PG are still visible Mag: 200x , After diamond polishing,
b) Scratches from FG still remain. The very deep scratch from PG Mag: 200x
2. Deformation ()
.
. line
fine polishing
. .

Grinding/polishing
a) b)
a) Short deformation lines, restricted to single grains. Mag: 100x DIC b) Well defined, sharp deformation lines Mag: 200x, DIC
3. Smearing
smearing .
, polishing cloth ,
, .
a) b)
a) Smearing on soft, ductile steel. Mag: 15x, DIC b) Smearing on soft, ductile steel. Mag: 25x, DIC

. Polishing cloth (nap )
polishing cloth .
smearing .
4. Edge rounding ( )
.
coating
. .
mounting
polishing
nap polishing cloth
a) b)
a) Due to a gap between resin and sample the edge is rounded. Stainless steel. Mag: 500x, Etchant: Beraha I
b) Good edge retention, Stainless steel. Mag: 500x, Etchant: Beraha I
5. Relief
2 . phase
polishing polishing cloth .
polishing (nap ) polishing cloth
.
B4C fibers Mag. 200x, Same as figure a) but without relief Mag. 200x
6. Pull out
grain particle cavity .
particle inclusion carbide
.
Pull out .
Cutting mounting
.
Grinding .
step grinding, polishing
step
Polishing cloth napless type cloth .
cloth polishing
pull –out .
Mag: 500x
metallography .
.
8. Embedded abrasive
grinding polishing .
.
polishing cloth

a) b)
a) Aluminium, with 3 diamond, Mag: 500x
b) Same as above, after final Most of the diamonds are still left in the sample. Mag: 500x
9. Lapping track
Lapping track .
. disc cloth
.
cloth cloth
. 10%
.
Zink alloy: Mag: 200x Lapping track after final polishing. Mag: 500x
10. Staining
etching
.
mounting
.
.

.
Staining of sample due to gap between resin and sample. Mag: 20x
11. Comet tails
.
polishing

.
Comet tails Mag: 20x,
. Etching and Photographing
1. (Etching)
Etching grain , . Etching
, ,
molten salt , , plasma .

.

.
.
.
Tint etching
Tint color . Tint
copper copper alloy .
tint .
(Molten salt etching)
.
grain size grain
boundary . .
(Thermal etching)
. grain boundary grain

grain boundary groove . grain
boundary .
, silicon nitride SiO2
.
27.

Kellers etchant
10-30
15
Kallings reagent
50 ml 50 ml
Marble's reagent Distilled water
~
Picral Ethanol Picric acid
Vilella's reagent Glycerol
Nitric acid HCl
~
28.

Wro. Stainless steel NH4OH 6 volts DC , 30-60
Aus. stainless steels
5-60 Carbides sigma phase
Copper alloy 5-14% H3PO4
Water 1-4 volts DC
Titanium
35 ml perchloric ac.
5-10 °C, 10-40
2 grams potassium hydroxide
30-60 mA/cm2 2-30
Stainless steel cathode 5-10 volts DC 15-20 ,

Pt SS cathode 3-6 volts DC
5-60
15 parts Nitric acid 40 parts glycerol
SS cathode 2-4 volts DC, 0.5
A/dm2 5-15
SS cathode 6 volts DC,
29. Tint

200g CrO3 +20g sodium sulfate + 17ml HCl + 1000mL water
1-5 , 10% aq .NaOH pre- etching 50% aq.HNO3
100ml + 10ml HF , molybdate .
200 ml water + 20ml HNO3 +3g ammonium molybdate
20 – 80ml ethanol
5g ammonium molybdate + 10g sodium thiosulfate+ 20ml ammonia + 200ml water
Al-Si-Cu-Ni cast alloy , 20C 5-8min
Cobalt and alloy a. HCl and water(1:1) Ingredient, b. 0.6-1g potassium metabisulfate Ingredient, c .1-1.5g FeCl3
100ml stock solution ingredient b ingredient c 20C 60-150
Copper and Alloy
Klemm’s I reagent : 50ml sat. aq. sodium thiosulfate 1g potassium metabsulfite
-brass 3min -brass 60min
Klemm’s II reagent : 50ml sat. aq. sodium thiosulfate 5g potassium metabsulfite
-brass 6-8min
Klemm’s III reagent : 50ml sat. aq. sodium thiosulfate 5g potassium metabsulfite
Bronze alloy 305min
Iron and alloy
60-80 ml 35% aq. sodium bisulfite + 40- 20ml water
Beaujard’s and Tordeux’s tint etch. 20C 10-25
Klemm’s I reagent : 50ml sat. aq. sodium thiosulfate 1g potassium metabsulfite
20C 40-100
Klemm’s II reagent : 50ml sat. aq. sodium thiosulfate 5g potassium metabsulfite
20C 30-90
30. Molten Salt

Cr2O3, CeO2, Al2O3 Potassium hydrogen sulfate melt
Pt crucible 3-10
Al2O3, Al2SiO5 Potassium hydrogen fluoride melt
Pt crucible 5-10
Si3N4 Sodium or potassium bicarbonate melt 10
31.

SiC 10-3 torr , 1200°C
UO2 10 torr, 1600 °C, 1
Si3N4 10-5 torr , 1250 °C, 15
2.
32. Al Al

Kellers Etch Distilled water Nitric acid Hydrochloric acid Hydrofluoric acid
190 ml 5 ml 3 ml 2 ml
10-30
Al
25 ml 25 ml 25 ml 1 drop
10-60 Al, Al-Mg
Mg-Si
92 ml 6 ml 2 ml
15 Al-Cu
33. Brass Bronze

Ammonium hydroxide (dilute solutions) Dilute Immersion Attack polishing
Distilled water Ferric chloride Hydrochloric acid
100 ml 5 grams
Brasses, bronzes, aluminum brass, alpha -phases in brass
Ethanol Hydrochloric acid Ferric chloride
100 ml 5-30 grams
or swabbing
34. Cast Iron

Nital Ethanol Nitric acid
100 ml 1-10 ml
35. Cu Cu

Distilled water Ammonium hydroxide ,3% Hydrogen peroxide
25 ml 25 ml
5-25 ml ~ Grain boundaries use less H2O2 Grain contrast use more H2O2
Distilled water Nitric acid
50 ml 50 ml ~ Copper and copper alloys
Distilled water or Ethanol Hydrochloric acid Ferric chloride
100-120 ml 25-50 ml
36.

Nital Ethanol Nitric acid
100 ml 1-10 ml
37.

100 ml 2-4 grams
~
Ethanol Nitric acid Hydrochloric acid Picric acid
80 ml 10 ml 10 ml
1 gram
~
38. Sn Sn

Ethanol or methanol or Distilled water Hydrochloric acid
100 ml
antimony-copper alloys
Distilled water or methanol Hydrochloric acid Ferric chloride
100 ml 5-25 ml
10 grams ~ Sn-Cu
39. Zn Zn

Distilled water or Ethanol Hydrochloric acid
100 ml 1-5 ml Zinc and zinc alloys
Distilled water Sodium Hydroxide
100 ml 10 grams 1~5 Low alloy zinc and pure zinc
Distilled water CrO3 Na2SO4
Swabbing
CERAMICS
40. Oxide ceramics

Thermal etching in air ~ Al2O3, Al2O3-MgO
Molten Salt Potassium hydrogen fluoride melt
5-10, Pt crucible
15 ml 85 ml 5 ~2 boiling Al2O3
Distilled water Sulfuric acid
41. Carbide Ceramics

Molten Salt Sodium or potassium bicarbonate melt
10 , Pt crucible
SiC
10 ml 10 ml
42. Nitride Ceramic

Thermal etching in high purity nitrogen 1600 Si3N
Molten Salt Potassium hydroxide melt
~, Pt crucible
43. Boride Ceramics

Latic acid Nitric acid Hydrofluoric acid
30 ml 10 ml 10 ml
~
3.
.
level . macrostructure, microstructure, ultra-microstructure level
. , ,
. processing step .
Bright field illumination
Bright field(B.F) illumination . B.F.
illumination , ,
. (, ,
)
.
polishing brightfield .
, graphite, nitrides, carbonitride, baride
. , polishing
. differential
interference contrast illumination (DIC) .
bright field illumination .
Polarized light
Cubic cross (polarizer analyzer 90 )
. cubic
. beryllium, cadmium, magnesium, alpha-titanium, uranium,
zinc or zirconium .
analyzer polarizer Polaroid filter .
prism polarizer .
crossed-polarized light
polishing . cubic
second cubic .
nodular graphite
. Cubic tint etched
.
Differential interference contrast (DIC)
Brightfield
differential interference contrast (DIC) brightfield .
. DIC
contrast .
Darkfield illumination
. copper
copper . copper sulfide
brightfield . Darkfield DIC brightfield
. Darkfield DIC brightfield
. Darkfield roughness, cracks, pits
.
Optical interferometry
.
.
splitter . 3
. shift
PZT phase shifting (PSI) vertical scanning (VSI)
. PSI VSI PSI z-
. VSI scan .
Atomic force microscopy (AFM)
AFM . AFM
, .
4.

.
graphite .
micro shrinkage cavity .
graphite ,
image analysis graphite , , nodule
.

.
color tint-etching .
.
#120 sand paper, 300rpm, 1.5 kgf ( 2.35m/sec, 200 dia. Wheel ),
#240 sand paper, 300rpm, 1.5 kgf ( 300mm dia. Wheel 180rpm)
9 diamond paste, napless cloth, 150rpm, 1.5kgf, 3min.
3 diamond paste, napless cloth, 150rpm, 2kgf, 3min.
1 diamond paste, medium nap cloth, 150rpm, 1.5kgf, 2min.
Etching : 4% natal

.
- 4% Nital : ferrite grain boundaries cementite, pearlite
.
- Alkaline sodium picrate (25g NaOH, 2g picric acid, 75 cc ) : 60 to 100°C 30
( 1-3 ) . cementite
ferrite .
- Murakami's reagent (10g KOH, 10g potassium ferricyanide and 100cc ) : 50°C 3
iron phosphide cementite ferrite
.

polishing .
4.3% eutectic point Fe-C CE (Carbon Equivalent Value)
4.3 hypereutectic , hypoeutectic . Fe-C
cementite, Fe, C, Graphite Si graphite graphite
.
V. Replica()
1.
Replica 1970 .
mounting, grinding, polishing
process.
.
replica .
, , ,
, metallurgical research .
replica .
*
* , plant
*
*
* (20 )
* metallography
2.

Replica .
,
. ,
, ,
.

. replica ×50∼×500,
(SEM) ×100∼×10,000 .
Replication
Replica 1974 ISO 3057
(Non-Destructive Testing-Metallographic Replica Techniques of Surface Examination) ,
1987 ASTM ES 12 1990 ASTM E 1351(Standard Practice for
Production and Evaluation of Field Matallographic Replicas) .

, (SEM)
, 1 replica, 2 replica, replica .
1 replica
, Replica .
2 replica
replica
1 replica replica . replica
.
replica
(matrix) replica
replica
.
Replica acetylcellulose film paraffin 0.035mm,
0.08mm . 0.035mm , replica
0.08mm .
acetylcellulose film 1.3, 24, 5%, 100,
, 1 methylacetate .
Replica
replica , , ,
. ,
replica , .
film
, .
Replica
(1) Rough grinding
Grinder 15∼20mm 0.3∼2.0mm ,
. .
(2) Fine grinding
#100, #220, #400, #600, #800, #1000 .
mesh(#) ,
heavy etching .
(3) Polishing
6 , 1 diamond polishing, polishing .
, polishing pit .
, polishing pipe .
(4) Etching
Etching replica . Etching cavity
. Etching , ,
,
. replica over etching polishing
. , cavity light etching
. (SEM) Au coating , cavity
, carbide
. over-etching carbide cavity .
cavity carbide .
(5) Replica
* .
* replica film .
* HAZ (Heat Affected Zone) .
* Replica .
* Replica (Striation)
.
(6) Marking
* Film replica , number, ,
, .
* Replica film , HAZ, , HAZ, marking
(7) Slide glass
Slide glass replica . replica
. .
(8) replica
replica portable polisher grinding polishing sand
paper, polishing cloth, , , replica film, .
OMR-kit, portable microscope

TN-12 Principles and Practice for Metallography

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Transcript of TN-12 Principles and Practice for Metallography