Buehlers

Guide to

Materials
Preparation
The Science Behind Materials
Preparation and Analysis TM

Introduction

Sir Henry Clifton Sorby

Anything approaching to
a burnished (smeared)
surface of polished
scratches is fatal to good
results.
Scientist - Sheffield, England
Father of Petrography
and Metallography
Understood Effect of
Abrasion on Microstructure

Introduction

Structure Organization of Matter

Macro - seen with the unaided eye (or hand lens)

Micro seen with a light microscope
Ultra seen with the transmission electron microscope

Crystal Structure
atomic configurations,
locations and defects
seen by x-ray diffraction
and by TEM
BCC

FCC

Introduction

Why is Microstructure Important?

Microstructure influences properties and behavior develop
structure/property data
Composition and processing influence microstructure monitor
process conformance
Undesired microstructures do cause product failures diagnose
failures (prevent future failures)

Introduction

Preparation Requirements: See

the True Microstructure
Remove cutting, grinding and
polishing related deformation
Avoid thermal damage
Avoid edge rounding
Minimize relief and smearing
Produce scratch-free surfaces

Introduction

Preparation Sequence
Each Step Must be Performed Properly

Sampling
Sectioning
Mounting (if needed)
Grinding
Polishing
Etching (if needed)

Sampling

Sampling
Specimens selected must be representative
of the material to be examined
Driven by the type of the investigation
Quality Control
Failure Analysis
Research and Development

Sampling

Designating Sampling Planes

1. Longitudinal planar section parallel to
the rolled surface
2. Transverse section
3. Longitudinal section perpendicular to the
rolled surface
g
lin
l
Ro

ct
ri e
d

n
io

Sampling

Microstructures Can Look

Different on Different
Planes in Wrought Alloys!

20 m

Transverse

20 m

Longitudinal

Note the difference in graphite shape in AISI O6 Graphitic

Tool Steel as a function of the sampling plane (4% picral)

Sectioning

Sectioning
Sample a large component or part by removing a
suitably-sized specimen from the larger mass at
the desired location and orientation
Sectioning plane should be as near to the desired
location as possible
Aggressive cutting methods will produce
excessive damage that must be removed

Sectioning

100 m

Examples of damage (arrows) from sectioning. Left: cut

surface in CP Ti (mod. Wecks reagent) on a plane
perpendicular to the cut; Right: residual sectioning damage in
the plane-of-polish of a CP Ti specimen (Krolls reagent).

Sectioning

Heat-affected zone (left) and melting at the surface (right,

arrows) due to abrasive sectioning A2 tool steel without a
coolant (nital etch). The cut surface was Ni plated after
cutting perpendicular to the first cut (using coolant).

Sectioning

Sectioning Machines

Sectioning

Sectioning Parameters
Equipment (abrasive cut-off, precision saw)
Blade, Wheel (SiC, Al2O3, CBN, diamond)
Operating Variables:

Load
Speed
Feed Rate
Contact Area

Coolant
Note: Delicate materials may require encapsulation

Sectioning

Abrasive Wheel Selection

SiC wheel - nonferrous materials
Al2O3 wheel- ferrous materials
Hard bond wheel - cut soft material
Soft bond wheel - cut hard material

Sectioning

Cut-off Wheel Selection

Application

Bond

Abrasive

Tool Steels, Carburized Steels, 60 HRC

Rubber resin

Al2O3

Hard Steel, ~50 HRC

Rubber resin

Al2O3

Medium Hard Steel, 35-50 HRC

Rubber resin

Al2O3

Soft or Annealed Steel, 20-35 HRC, 46-90

HRB

Rubber

Al2O3

Medium Hard Nonferrous Materials:

Uranium, Titanium, Zirconium (Refractory
Metals)

Rubber

SiC

Soft Nonferrous Materials: Aluminum, Brass,

etc.

Rubber

SiC

Metal

Diamond

Very Hard, Brittle Fracture Materials:

Carbides, Ceramics, Minerals

Sectioning

Precision Saws

Precision positioning
Small kerf loss
Diamond blades, thin abrasive wheels
Applications
Delicate components
Ceramics, Carbides, Nitrides
Biomaterials

Sectioning

Wafering Blade Selection

Application

Blade

Plastics, polymer, rubber

30 HC diamond

Aggressive sectioning: ferrous and nonferrous materials

including titanium alloys

20 HC diamond

General use: ferrous and nonferrous alloys, copper, aluminum,

composites, thermal spray coatings, pc boards

15 HC diamond

Hard/tough materials: Boron nitride, Silicon nitride

20 LC diamond

Hard/brittle materials: structural ceramics, glass, electronic

substrates, alumina, zirconia, concrete

15 LC diamond

Lower hardness/low density ceramics, electronic packages,

packaged integrated circuits, GaAs, AlN

10 LC diamond

Soft, friable ceramics, electronic packages, un-mounted silicon

chips, carbon composites, CaF2, MgF2

5 LC diamond

Carbon steels, high alloy steels, cobalt alloys, nickel-based

superalloys, and lead alloys

Cubic boron nitride

Mounting of Specimens

Why Mount Specimens?

Protect edges during preparation process
Protect delicate samples
Increase life of polishing surfaces
Uniformity of shape and size for automation
Simplify specimen identification

Mounting of Specimens

To Maximize Edge Preservation

Select the best mounting compound EpoMet resin
Use a press that cools under pressure
Plate edge with a protective metal EdgeMet Kit
Add a filler material to cast resins Flat Edge Filler
Use nappless polishing surfaces

Mounting of Specimens

Mounting Methods

Mechanical Clamps
Thermosetting Resins
Thermoplastic Resins
Cast (Cold) Resins
Vacuum Impregnation for Porous
Specimens

Introduction

Hot Mounting Presses

Mounting of Specimens

Hot Mounting Resins

Thermosetting Resins
PhenoCure (phenolic)
EpoMet
Diallyl Phthalate

Thermoplastic Resins
TransOptic

Conductive Resins
ProbeMet (Cu-Filled)
KonductoMet (C-Filled)

Mounting of Specimens

Selecting a Hot Mounting Compound

Phenolic (PhenoCure)

Acrylics (TransOptic)

Lowest Price
High Shrinkage
Poor Edge Retention
Poor Resistance to Hot Etchants

Epoxy (EpoMet)

Superb Edge Retention

Low Shrinkage
Resistant to Heat and Chemicals
Abrasion Rate Matches Metals

Transparent
Long Curing Cycle
High Shrinkage
Defect Prone
Low Chemical Resistance
Poor Heat Resistance

Mounting of Specimens

Edge Retention

PhenoCure mounting compound

Improperly carburized 8620 alloy
(arrow points to gap) 500 X

EpoMet mounting compound

borided 42CrMo4 alloy steel
1000 X

Mounting of Specimens

Good edge retention in salt-bath nitrided 1215 carbon steel mounted in a) Epomet
resin and b) electroless N-plated with the EdgeMet kit and mounted in Epomet resin
(poor image contrast, however, between plating and nitride layer). These specimens,
and the next two, were prepared in the same holder revealing variations in edge
retention due to the mounting materials used. (nital etch). The arrows point to the
iron nitride surface layer. The needle-like particles are nitrides.

Mounting of Specimens

Poor edge retention in salt-bath nitrided 1215 carbon steel mounted

with b) phenolic resin; and c) methyl methacrylate resin and all
prepared in the same holder (with previous specimens) revealing a
lack of edge retention (nital etch). The arrows point to the iron
nitride surface layer. The needle-like particles are nitrides.

Mounting of Specimens

Shrinkage gaps between resin and specimen, as shown above, can

leadge to edge rounding (note the rounding revealed using Nomarski
DIC at left), bleed out after washing (left) or after etching (right, M2
high speed steel etched with Vilellas reagent).

Mounting of Specimens

Bleed out from a shrinkage gap between two sheet specimens of

L605 Co-based alloys etched with 15 mL HCl 10 mL acetic acid
10 mL HNO3, 200x.

Mounting of Specimens

Example of good edge retention using Flat-Edge Filler soft

ceramic shot in Epoxicure resin to view the microstructure of
annealed H13 tool steel (4% picral etch).

Rigid Grinding Disk

ApexHercules RGD

Rigid grinding disks not only yield very high removal rates, they produce superb
edge retention and relief control. However, the surface finish is poorer than
cloths produce with the same abrasive. Hence, the following step must restore
the surface finish without degrading flatness.

Mounting of Specimens

Castable Mounting
Cold Mounting
Acrylic Resins
VariDur
SamplKwick

Epoxy Resins

EpoKwick
EpoxiCure
EpoThin
EpoColor
EpoHeat

Mounting of Specimens

Selecting a Castable Resin

Acrylic Resins

Epoxy Resins

Least Expensive

Low Shrinkage

Rapid Cure

Transparent

Poor Edge Retention

Adheres to Specimen

Strong Exothermic Reaction

Solvent Resistant

High Shrinkage

Moderate to slow cure

Strong Odor

Will Flow into Cracks and

Voids (under vacuum)

Mounting of Specimens

Vacuum Infiltration
Goal: To infiltrate open voids
or cracks with mounting media
Reason: Maintain true void
shape and size, avoid pull outs
causing artifacts, etc.
Application: Pour resin
mixture under vacuum (25
vacuum).

Mounting of Specimens

Castable Resin Processing Factors

Specimens must be cleaned and dried

Do not use products beyond their shelf life
Mix resin and hardener by specified weights
Resin and hardener must be mixed carefully
Large epoxy volumes generate high heat
To reduce exotherm, use conductive mold
Large specimen size increases cure time

Semi-Automatic Systems

Grinding / Polishing

PowerPro Series

Very Powerful
Z-Axis Removal Control
Under-Bowl Cooling
Two Head Speeds
Two Head Directions
Fully Programmable
3000, 4000 and 5000 Models

Grinding

Initial Grinding Step

Goals
Remove the damage resulting from sectioning
Establish a planar surface
Reach a specific plane close to a desired
area/feature

Extent of sectioning damage determines the

selection of the initial abrasive size

Grinding

Subsequent Steps
Remove damage from previous step(s)
Decreasing abrasive size
Depth of damage decreases
Removal rate decreases

Depth of damage is greater for soft

materials than hard materials

Polishing

Final Polishing
Remove any remaining damage or smear
Produce a lustrous, scratch-free surface
Maintain edge retention
Yield the true structure with sharpness and good
contrast

Colloidal (Amorphous) Silica

MasterPrep Sol-Gel Alumina

Alumina suspensions are redefined by sol-gel MasterPrep alumina

(0.05-m particle size). Unlike calcined alumina suspensions,
MasterPrep suspensions are totally free of agglomerates. It markedly
outperforms all other alumina abrasives and has none of the problems
associated with colloidal silica.

Polishing

Examples of poor (a) relief

control and (b) good relief
control around voids in a braze
(glyceregia etch) and comet
tails at nitrides in H13 tool steel
(Nomarski DIC, as polished),
shown above.

Polishing

10 m

Examples of embedded abrasives: Left, SiC from grinding

embedded in a weld in 6061-T6 aluminum (0.5% HF etch); Right, 3m diamond embedded in a steel specimen (unetched).

Polishing

After 1-m Diamond Polish

SiC
Embedded
in Lead
and its
removal

100 m
After 0.05-m Al2O3 5 min

100 m
After 0.05-m Al2O3 3 min
After Colloidal Silica, Vibratory Polish, Pollacks Reagent

Polishing

Example of a poorly dried steel specimen (Nomarski DIC).

Polishing

Vibratory Polishing
Remove fine scratches
Useful for materials
prone to smearing
Great for difficult to
prepare materials

Grinding / Polishing

Automation Benefits
Increase daily output
Improve consistency
Improve edge
retention, relief
control and overall
flatness

Grinding / Polishing

Preparation Parameters

Abrasive type, size and amount

Working surface (pad, cloth, etc.)
Wheel and head speeds and directions
Head position
Force applied to specimens
Individual force or central force
Lubrication
Time

Grinding / Polishing

Abrasives
Alumina (powders, suspensions)
Diamond (paste, suspensions, aerosols)
(natural or synthetic; monocrystalline or polycrystalline)
Colloidal silica (pH 9.5)
Magnesium oxide (limited use)
Cerium oxide (glass)

Grinding / Polishing

Diamond

Monocrystalline

Polycrystalline

Diamond used for

polishing since 1920s,
but commercial use of
diamond was introduced
in 1949 with natural
virgin diamond as
paste. Later, synthetic
monocrystalline diamond
introduced, and in the
early 1980s, synthetic
polycrystalline diamond
(yields somewhat higher
removal rates and better
surface finish for many
metals).

Grinding / Polishing

Amount of Abrasive

Surface selected
Format size: 8, 10 or 12
Platen rpm
Head rpm

30
.33 ml/min
25
Removal Rate (um/min)

Too little low cutting rate

Too much hydroplaning
Variables

1.83 ml/min
13.83 ml/min

20

15

10

0
Texmet 1000

UltraPol

Hercules H

Parameters: Al specimens, 9m diamond, 150 rpm, 5 lbs/specimen, 8 format

Grinding / Polishing

Comparing SiC and Diamond

Variables
Material type
Material hardness
Working surface
Automation
Pressure
Time

Ultra-Pol, 9um diamond

BuehlerHerculesH, 9um diamond

25
SiC 1200 grit (P2500)
Rem oval Rate (um /m in)

30

20
15
10
5
0
Al (183 HV)

Steel (710 HV)

Grinding / Polishing

MasterPrep Alumina and MasterMet Colloidal Silica

Both are excellent for most metals and non-metals

MasterMet Colloidal Silica

Preferred for refractory metals, polymers, sintered carbides
and aluminum alloys
Unsuitable for precious metals; will etch Mg alloys and stains
pearlitic cast irons; causes etching problems with stainless steels
and Ni-base superalloys when using etchants with Cl- ions

MasterPrep Alumina Suspension

Free from etching, cleaning and staining problems
Sol-gel processing yields agglomeration-free suspension far
better than calcined aluminas

Grinding / Polishing

Surface Comparison
Material Removal (um/min)

30
25
20
15
10
5
0
Microcloth

Texmet 1000

UltraPol

Hercules S

Hercules H

Parameters: Al specimens, 9m diamond, 150 RPM, 5 lbs/specimen

Grinding / Polishing

Wheel and Head: Speed

An increase in speed
usually corresponds
with the following
Increase in removal rates
More loose abrasive
being thrown from the
platen
Difficulty in controlling
flatness when preparing
specimens manually

Removal Rate (um/min)

10
8
6
4
2
0
0

100

200

300

400

500

RPM

Common working range: 150-300 RPM

Parameters: Al specimens, 9m diamond, 5 lb/specimen, Ultra-Pol

Grinding / Polishing

Wheel and Head: Direction

Contra seen as more aggressive
Complementary tends to throw abrasive off the wheel
Most methods use a combination of directions

Contra

Comp

Grinding / Polishing

Wheel and Head: Position

Most common
position specimens
in holder are running
slightly over the edge
of the platen
Prevents non-uniform
grinding of large
specimens (MRD)

Grinding / Polishing

Central or Individual Force

Central Force
Cannot remove any specimens until
preparation is complete
Yields best flatness and edge retention

Individual Force
One or more specimens can be
prepared
Can examine specimens easily during
preparation
Easy to remove etch or repeat last part
of cycle

Grinding / Polishing

Force Selection
5 psi / 35 Mpa

Adjust based on
following criteria
Surface area
Material hardness

Removal Rate (um/min)

Starting point
10
9
8
7
6
5
4
0

10

15

20

Load (lb)

Effect of Increasing Force

Parameters: Al specimens, 9m diamond, 150 RPM, UltraPol

Grinding / Polishing

Increasing the Removal Rate

Modifying a Procedure one Variable at a Time

Force: 5 to 15 pounds
RPM: 150 to 450
Direction: comp. to contra
Volume of Abrasive: 0.33 to 1.83 mL/min
Surface Selection: Hard woven cloth to rigid
grinding disk
Results of changes shown on next slide

Grinding / Polishing

Increasing the Removal Rate

Increase in Removal Rate (%)

400

300

200

100

0
Force

RPM

Direction

Volume of
Abrasive

Surface
Selection

Baseline procedure: Al specimens, 9m diamond, 150 RPM, 5 lbs/specimen, comp, UltraPol

Grinding / Polishing

Time
Each step must remove the deformation
from the previous step
Increase time; increase material removal
Smaller jumps in abrasive size, shorter
times required
Increases in specimen surface area may
require longer times

Grinding / Polishing

Traditional Method
Surface

Abrasive/Size

Load Lb. (N)/

Specimen

Base Speed
(rpm)/Direction

Time
(min:sec)

CarbiMet

120 (P120) SiC*

6 (27)

240 300/Comp.

Until plane

CarbiMet

240 (P280) SiC*

6 (27)

240 300/Comp.

1:00

CarbiMet

320 (P400) SiC*

6 (27)

240 300/Comp.

1:00

CarbiMet

400 (P600) SiC*

6 (27)

240 300/Comp.

1:00

CarbiMet

600 (P1200) SiC*

6 (27)

240 300/Comp.

1:00

Canvas

6-m diamond paste

6 (27)

120 - 150/Comp.

2:00

Billiard

1-m diamond paste

6 (27)

120 - 150/Comp.

2:00

MicroCloth

0.05-m alumina
slurry

6 (27)

120 - 150/Comp.

2:00

Based on 1 mount size *Water cooled

Grinding / Polishing

Contemporary Method
Surface

Abrasive/Size

Load Lb. (N)/

Specimen

Base Speed
(rpm)/Direction

Time
(min:sec)

CarbiMet
paper

180, 240 or 320

(P180, P240, or P400)
SiC, water cooled

6 (27)

240 300
Comp.

Until plane

UltraPol

9-m MetaDi
Supreme diamond
suspension

6 (27)

120 150
Comp.

5:00

TriDent

3-m MetaDi Supreme

diamond suspension

6 (27)

120 150
Comp.

4:00

MicroCloth

0.05-m MasterPrep
alumina suspension

6 (27)

120 150
Contra*

2:00

Based on 1 mount size

*Use contra only with low-speed heads (<100 rpm)

Preparation Procedures

For Preparation, Metals Are Grouped

According to Like Characteristics

Preparation Procedures

Procedure Development
Materials are grouped by common
characteristics; periodic table used as a guide
Primary equipment used for development
8 (200 mm) platen
six 1.25 (30 mm) diameter specimens
central force holder

Light Metals

Aluminum Procedure
Surface

CarbiMet paper
UltraPol cloth
TriDent cloth
TriDent cloth
MicroCloth pad

Abrasive/Size

240- (P280) grit SiC

Water cooled
9-m MetaDi Supreme
diamond suspension
3-m MetaDi Supreme
diamond suspension
1-m MetaDi Supreme
diamond paste
0.05-m MasterMet
Colloidal silica

Load Lb.
(N)/
Specimen
5 (22)
5 (22)
5 (22)
5 (22)
5 (22)

Base Speed
Time
(rpm)/Direction (min:sec)
240
Comp.
150
Comp.
150
Comp.
120
Comp.
120
Contra

Until
plane
5:00
4:00
2:00
1:30

Light Metals

Material

206
Al-4.4Cu-0.3Mg0.3Mn

Etchant

Tint etched with

Wecks reagent

Description

As-cast Al etched to
reveal a dendritic
structure. Viewed
with crossed
polarized light and
sensitive tint.

Light Metals

Material

AA 5754-F Strip
Al-3.2Mg-0.4Mn+Cr

Etchant

Electrolytically
etched with Barkers
reagent
(30 V dc, 2 min.)

Description

Wrought Al strip
annealed at 343 C-2h
viewed with crossed
polarized light and
sensitive tint.

Copper, Nickel and Cobalt

Copper Procedure
Surface

CarbiMet
UltraPol
TexMet 1500
TriDent
MicroCloth

Abrasive/Size

320- (P400) grit SiC

Water cooled
6-m MetaDi Supreme
diamond suspension
3-m MetaDi Supreme
diamond suspension
1-m MetaDi Supreme
diamond suspension
0.05-m MasterMet
Colloidal silica

Load Lb.
(N)/
Specimen
6 (27)
6 (27)
6 (27)
6 (27)
5 (22)

Base Speed
Time
(rpm)/Direction (min:sec)
240
Comp.
150
Comp.
150
Comp.
120
Comp.
120
Contra

Until
plane
5:00
3:00
2:00
2:00

Copper, Nickel and Cobalt

Material

Cartridge brass
Cu - 30Zn

Etchant

Klemms III

Description

Wrought cartridge
brass, cold reduced
50% and annealed at
704 C producing
equiaxed alpha grains
containing annealing
twins. Viewed with
cross polarized light
and sensitive tint. 50X.

Copper, Nickel and Cobalt

Material

Eutectoid aluminum
bronze
Cu - 11.8Al

Description

Wrought, eutectoid
aluminum bronze, heat
treated to form
martensite (900 C-1h,
WQ). Viewed with
cross polarized light.

Ferrous Metals

Steel Procedure
Surface

CarbiMet paper
ApexHercules H
rigid grinding disk
TriDent cloth
MicroCloth pad

Abrasive/Size

240- (P280) grit SiC

Water cooled
9-m MetaDi Supreme
diamond suspension
3-m MetaDi Supreme
diamond suspension
0.05-m MasterPrep
alumina suspension

Load Lb.
(N)/
Specimen
6 (27)
6 (27)
6 (27)
6 (27)

Base Speed
Time
(rpm)/Direction (min:sec)
240
Comp.
150
Comp.
150
Comp.
120
Contra

Until
plane
5:00
3:00
1:30

Ferrous Metals

Material

UNS K11430
ASTM A588
C 0.15 Cr 0.52 Cu
0.32 Mn 1.05 Si 0.22
V 0.6 balance Fe

Etchant

4% picral followed by
2% nital

Description

Hot-rolled plate steel

etched to reveal a
moderately banded
structure of ferrite and
pearlite.

Ferrous Metals

Material

UNS J04001
AMS 1040
C 0.4 Mn 0.85
Si 0.6 balance Fe

Etchant

2% nital

Description

Microstructure of
annealed carbon
steel revealing
ferrite and
pearlite.

Ferrous Metals

Material

UNS G40270
SAE 4027
C 0.27 Mn 0.80 Mo
0.25 Si 0.25 balance Fe

Etchant

2% nital

Description

Microstructure of hotrolled alloy steel

revealing a bainitic
structure with a few
patches of pearlite,
acicular ferrite and
some patches of
proeutectoid ferrite.

Ferrous Metals

Material

W1 (1.05% C) tool steel

Etchant

Berahas tint etch: 100 mL

water, 10 g Na2S2O3, 3 g
K2S2O5

Description

Microstructure of overaustenitized W1 (927 C

1 h, BQ, 149 C 2 h)
where all of the Fe3C has
been put into solution
causing retention of
considerable austenite in
the martensitic matrix,
1000x.

Ferrous Metals

Material

P/M T15 High Speed

Steel

Etchant

Berahas Sulfamic Acid

Reagent

Description

Microstructure of
spheroidize annealed
P/M T15 high speed
steel showing the ferrite
matrix colored and the
carbides unaffected,
1000x

Ferrous Metals

Stainless Steel Procedure

Surface

CarbiMet paper
UltraPol cloth
TriDent cloth
MicroCloth pad

Abrasive/Size

240- (P280) grit SiC

Water cooled
9-m MetaDi Supreme
diamond suspension
3-m MetaDi Supreme
diamond suspension
0.05-m MasterPrep
alumina suspension

Load Lb. (N)/

Base Speed
Time
Specimen
(rpm)/Direction (min:sec)

6 (27)
6 (27)
6 (27)
6 (27)

240
Comp.
150
Contra
150
Contra
120
Contra

Until
plane
5:00
5:00
2:00

Ferrous Metals

Material

UNS S41600
AISI 416 (CTC P70)
C 0.10 Cr 13.0 S >0.15
balance Fe

Etchant

Berahas CdS reagent

Description

Microstructure of freemachining martensitic

stainless steel in the
quenched and tempered
condition. Note: gray
elongated sulfide
inclusions, white delta
ferrite and martensitic
matrix.

Ferrous Metals

Material

420 Stainless steel

Etchant
Vilellas Reagent
Description

Microstructure of
quenched and
tempered 420
martensitic stainless
steel, 1000x

Ferrous Metals

Material

Custom Flo 302 HQ

Fe-<0.08C-18Cr-9Ni3.5Cu

Etchant

Tint etched with

Berahas BI reagent

Description

Microstructure of hotrolled and solution

annealed and aged
precipitation hardened
stainless steel
revealing a fully
austenitic matrix. (bar
is 100 m long).

Ferrous Metals

Material

7 Mo PLUS Duplex
Stainless Steel

Etchant

85 mL H2O 15 mL
HCl 1 g K2S2O5

Description

Microstructure of & Mo
PLUS duplex stainless
steel in the hot rolled
and annealed condition
(ferrite colored, 200x).

Ferrous Metals

Cast Iron Procedure

Surface

CarbiMet paper
UltraPol cloth
TexMet 1500 pad
TriDent cloth
MicroCloth pad

Abrasive/Size
240- (P280) grit SiC
Water cooled
9-m MetaDi Supreme
diamond suspension
3-m MetaDi Supreme
diamond suspension
1-m MetaDi Supreme
diamond suspension
0.05-m MasterPrep
alumina suspension

Load Lb. (N)/

Base Speed
Time
Specimen
(rpm)/Direction (min:sec)
6 (27)
6 (27)
6 (27)
6 (27)
6 (27)

240
Comp.
150
Comp.
150
Comp.
120
Comp.
120
Contra

Until
plane
5:00
4:00
3:00
2:00

Ferrous Metals

Material

Pearlitic Ductile Iron

Etchant

Berahas CdS
reagent

Description

Microstructure of
pearlitic ductile iron
containing graphite
nodules surrounded
by ferrite. Viewed
with polarized light
plus sensitive tint.

Ferrous Metals

Material

Pearlitic Gray Iron

Etchant

Berahas CdS
reagent

Description

Microstructure of
pearlitic gray cast
iron containing
ferrite near the
flakes.

Ferrous Metals

Material

Ductile Iron

Etchant

Berahas CdS Tint Etch

Description

Microstructure of heat
treated ductile cast iron
revealing an elongated
agglomerate of several
graphite nodules,
tempered martensite,
carbide and retained
austenite, 1000x

Titanium

Titanium Procedure
Surface

Abrasive Size

Load Lb.
(N)/Specimen

Base Speed
(rpm)/Direction

Time
(min:sec)

CarbiMet
paper

320-grit (P400) SiC

water cooled

6(27)

240
Comp. or Contra

Until Plane

UltraPol (psa)
cloth

9-m MetaDi
Supreme diamond
suspension

6(27)

150
Contra

10:00

MicroCloth
pad

MasterMet Colloidal
Silica (1 part H2O2,
30% conc., to 5 parts
colloidal silica)

6(27)

150
Contra
(head <100 rpm)

10:00

Titanium

Material

CP Ti
ASTM F67 Grade 2

Etchant

Modified Wecks

Description

Wrought as-rolled CP
Ti with banded grains
revealed with
polarized light plus
sensitive tint. Note
mechanical twins.
Magnification bar is
100 m long.

Titanium

Material

Ti-8Al-1Mo-1V

Etchant

Krolls

Description

Transverse plane, wrought

Ti811 heat treated (1010
C-1 h, AC, 593 C-8h,
AC) below the beta transus
( 1040 C) revealing
equiaxed alpha and beta
transformed to lamellar
alpha and beta (bar is 10
m long)

Etching

Etching
Techniques
Swab
Immersion
Electrolytic

To Reveal

Grain boundaries
Constituents
Banding, segregation
Deformation

100 m

Etching

Etching Reveals

Grain boundaries
Phases
Constituents
Homogeneity
Coatings and Platings
Interfaces
Heat affected zones
Reaction zones

Dendritic patterns
Segregation
Deformation

Etching

Techniques
Swab
Immersion
Electrolytic

Attack rate controlled

by chemical selection,
temperature, time,
current, voltage

Etching

Guidelines

High magnification evaluation; shallow etch

Low magnification evaluation; deeper etch
Time is less reliable than appearance
Best results occur when etching right after
polishing, time can create a passive surface
If you are not satisfied, an etch-repolish-etch
sequence may improve the results

Etching

Etchant Selection Example

Low-Carbon Sheet Steel

2% Nital

4% Picral

Berahas reagent

Reveals ferrite grain

boundaries and cementite

Reveals cementite

Colored grains based on

crystallographic orientation

Etching

Etchant Selection Example

Carbon Steel Weld

Weld

Heat-Affected Zone

Base

This carbon steel weld was

etched with 2% nital (top),
but it revealed the grain
structure poorly compared to
Klemms I (bottom). Note
the very strong delineation of
the interface between the
base metal and the heataffected zone (Ac1
temperature).

Etching

Etchant Selection Example

High-Carbon Steel

2% Nital

Alkaline Sodium Picrate

90 C, 60 s

4% Picral

Intergranular and intragranular cementite is revealed best by selective etching

with alkaline sodium picrate in this as-rolled 1.31% carbon tool steel.

Etching

Etchant Selection Example

Ferrite, Pearlite and Martensite in 8620 Alloy Steel

2% Nital

4% Picral

Klemms I

8620 alloy steel isothermally heat treated to form a proeutectoid ferrite (927 C (1700 F) 30
min, 677 C (1250 F) for 60 s water quenched), the remaining austenite formed as-quenced
martensite. Nital revealed the ferrite (f) and as-quenched martensite (m), but picral does not
reveal either phase. Tint etched with Klemms I reagent which colored the as-quenched
martensite dark blue (non-uniform coloring) and colored ferrite white, light yellow, dark
yellow/brown and several light shades of blue.

Etching

Etchant Selection Example

Upper Bainite and Martensite in 5160 Alloy Steel

2% Nital

4% Picral

10% Na2S2O5

5160 alloy steel isothermally heat treated to form a small amount of upper bainite (830 C
(1525 F) 30 min, 538 C (1000 F) for 60 s water quenched), the remaining nontransformed austenite formed martensite. Nital revealed both constituents. Picral reveals only
the cementite in the upper bainite. Aqueous 10% sodium metabisulfite colored the as-quenched
martensite brown while the bainite was blue and white.

Etching

Etchant Selection Example

Lower Bainite and Martensite in 5160 Alloy Steel

2% Nital

4% Picral

10% Na2S2O5

5160 alloy steel isothermally heat treated to form a small amount of lower bainite
(830 C (1525 F) 30 min, 343 C (650 F) for 5 min. water quenched), the
remaining austenite formed martensite. All three etchants reveal the lower bainite,
although picral mainly shows the cementite within the bainite. Sodium metabisulfite
colors the martensite brown and the bainite blue.

Etching

Etchant Selection Example

Spheroidize Annealed W1 Tool Steel

4% Picral

Alkaline Sodium Picrate

90 C, 60 s

Klemms I

Three ways to reveal cementite in W1 carbon tool steel.

Etching

Etchant Selection Example

Spheroidize Annealed M4 High Steel Steel

Alkaline Sodium Picrate

90 C, 60 s M6C colored,
MC unaffected

1% CrO3 3V dc, 10 s
Murakamis, 20 C, 20 s
MC attacked, M6C
M6C Attacked, MC
unaffected
unaffected
Selective etching of carbides in M4 high-speed tool steel.

Etching

Etchant Selection Example

D3 Cold Work Die Steel (1950 F, OQ)

Vilellas Reagent

100 mL H2O, 0.6 mL HCl,

1 g K2S2O5

Murakamis Reagent,
20 C, 6 s

Microstructure of over-austenitized D3 tool steel.

Etching

Etchant Selection Example

17-4 PH Martensitic Stainless Steel

20 m

Mod. Frys Reagent

20% NaOH, 20 V dc, 20 s

Super-Picral

Martensite and delta ferrite stringers in wrought, solution annealed and aged 17-4
PH stainless steel.

Etching

Etchant Selection Example

Austenite, Ferrite and Sigma in a Duplex Stainless Steel
7 Mo duplex stainless steel,
annealed and aged at 816 C
for 48 h converting some of
the ferrite (tan) to sigma
(orange) and new austenite
(arrows). Austenite is not
colored. The magnification
bar is 10 m long.

20% NaOH at 3 V dc, 10s

Etching

Etchant Selection Example

Dendritic Structure of Continuously Cast 1100 Al

Barkers Reagent, 30 V dc, 2 min.

Wecks Reagent

Barkers reveals the dendrites but not the coring segregation, as Wecks does.

Etching

Etchant Selection Example

Cartridge Brass
Cu 30% Zn

NH4OH-H2O2 (3%)

Klemms I

Klemms III

Berahas PbS

Cartridge brass, cold rolled to

50% reduction and annealed at
704 C for 30 minutes, was
etched with a standard swab
etch and three color etchants
(these were photographed in
cross-polarized light plus
sensitive tint). The color
etchants reveal the grain
structure very well.

Etching

Etchant Selection Example

Alpha Titanium
Grains in CP Ti

Krolls Reagent

Mod. Wecks Reagent

Polarized Light (not etched)

Heat Tinted on Hot Plate

The alpha grain structure of

CP Ti (different specimens)
was revealed better using
polarized light, color etching
or heat tinting than with
Krolls reagent. The
magnification bars are,
respectively, 50, 100, 100 and
100 m long.

Etching

Chemical Safety
Read MSDS before using
Personal protection
equipment
Safety glasses / goggles
Gloves
Apron

Facility
Hood
Eyewash
Shower

Etching

Chemical Work Area Safety

Label all containers
Clean up any spill, no matter how small
Dispose according to local regulations

Technical Help

Information Availability
Website
Buehler Book
Tech Notes

Email
Techsupport.com, ask a specific question directly to
Buehlers lab
Join Buehlers E-club
Technical updates
New product information

Etching

Etchant Selection Example

Grinding / Polishing

General Procedure Used for Comparing

Material Removal Rates of Aluminum and Steels
Surface

CarbiMet paper
UltraPol cloth
TriDent cloth
ChemoMet pad

Abrasive/Size
240- (P280) grit SiC
Water cooled
9-m MetaDi Supreme
diamond suspension
3-m MetaDi Supreme
diamond suspension
0.05-m MasterPrep
alumina suspension

* Several sheets of SiC paper were used

Load Lb.
(N)/
Specimen
5 (22)
5 (22)
5 (22)
5 (22)

Base Speed
Time
(rpm)/Direction (min:sec)
150
Comp.
150
Comp.
150
Comp.
150
Comp.

6:00*
5:00
3:00
1:30

Grinding / Polishing

Total Depth Removed by Material

with the General Preparation Procedure

Total Removal (mm)

1.2
1
0.8
0.6
0.4
0.2
0
Al (183 HV)

Stainless steel
(168 HV)

Steel (710 HV)

BUEHLER

METHODS Thermal Spray Coating

Thermal Spray Coating electric arc spray NiCrAl
Approximately500X
Prepared on Ecomet
3/Automet 2
Mounted in EpoHeat, 1.25
Surface

Time

Force

RPM Rot.

APEX DGD 60 micron

3:00

5 lbs

300

Contra

APEX DGD 9 micron

3:00

5 lbs

300

Contra

APEX DGD 6 micron

3:00

5 lbs

300

Contra

Texmet 1000 w/3 micron

Metadi Supreme

3:00

6 lbs

120

Comp

Chemomet w/Masterprep

2:00

4 lbs

150

Comp

APEX SYSTEM
BUEHLER CONFIDENTIAL

BUEHLER

METHODS - Ceramic
Dense Ceramic Specimen
Approximately 200X
Prepared on Ecomet
3/Automet 2
Mounted in Phenocure, 1.25

Surface

Time

Force

RPM Rot.

APEX DGD 40 micron

3:00

5 lbs

300

Contra

APEX DGD 9 micron

3:00

5 lbs

300

Contra

APEX DGD 6 micron

3:00

5 lbs

300

Contra

APEX DGD 3 micron

3:00

5 lbs

300

Contra

10 lbs

150

Contra

Texmet 1000 w/Mastermet 4:00

APEX SYSTEM
BUEHLER CONFIDENTIAL