Buehler’s

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

Preparation Requirements: To
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

Designating Sampling Planes

1. Transverse section
2. Longitudinal “planar” section parallel to the
rolled surface
3. Longitudinal section perpendicular to the rolled
surface
n
io
ct
ri e
d
g
llin
Ro

1 2 3
 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 µm

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

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

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

“Hot” Mounting Presses


Selecting a “Hot” Mounting Compound
Phenolic (PhenoCure™)
• 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
Mounting of Specimens
Acrylics (TransOptic™)
• Transparent
• Long Curing Cycle
• High Shrinkage
• Defect Prone
• Low Chemical Resistance
• Poor Heat Resistance
 Edge Retention

Salt-bath nitrided 1215 carbon steel

mounted in a) Epomet resin, b) phenolic
resin; and c) methyl methacrylate resin and
all prepared in the same holder revealing
variations in edge retention (nital etch). The
arrows point to the iron nitride surface layer.
The needle-like particles are nitrides.
 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
• Low Cost • 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

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
 Introduction

Grinding / Polishing
 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 and flatness
• Yield the true structure with sharpness and good
contrast
 Polishing Problems

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 Problems

Embedding of
SiC abrasive is
a common
problem with
SiC embedded in Pb (after 1-µm diam)
low-melting
metals.
Polishing with 5 min polish with 0.05-µm Al2O3
diamond
abrasive does
not remove the
embedded
particles, but
alumina does.

After 3 min. polish with 0.05-µm Al2O3

Vibratory polish, SiO2, Pollack’s etch
 Polishing Problems

This shrinkage gap caused bleed out of water after drying which
obscures detail and creates confusion.
 Polishing Problems

Improper drying has left spots of water on the surface. DIC

 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

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

Wheel and Head: Direction

• Contra is slightly more aggressive
• Complementary tends to throw abrasive off the wheel
• Most methods use a combination of directions

Contra Comp
 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

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
Load Lb. (N)/ Base Speed Time
Surface Abrasive/Size
Specimen (rpm)/Direction (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-µm diamond paste 6 (27) 120 - 150/Comp. 2:00

Billiard 1-µm diamond paste 6 (27) 120 - 150/Comp. 2:00

0.05-µm alumina
MicroCloth® 6 (27) 120 - 150/Comp. 2:00
slurry
Based on 1 ¼ mount size *Water cooled
 Grinding / Polishing

Contemporary Method
Load Lb. (N)/ Base Speed Time
Surface Abrasive/Size
Specimen (rpm)/Direction (min:sec)
180, 240 or 320
CarbiMet 240 – 300
(P180, P240, or P400) 6 (27) Until plane
paper Comp.
SiC, water cooled
9-µm MetaDi® 120 – 150
UltraPol™ Supreme diamond 6 (27) 5:00
suspension Comp.

3-µm MetaDi Supreme 120 – 150

TriDent™ 6 (27) 4:00
diamond suspension Comp.
0.05-µm MasterPrep™ 120 – 150
ChemoMet® 6 (27) 2:00
alumina suspension Contra*

Based on 1 ¼ 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
 Copper, Nickel and Cobalt

Copper Procedure
Load Lb.
Base Speed Time
Surface Abrasive/Size (N)/
(rpm)/Direction (min:sec)
Specimen

320- (P400) grit SiC 240 Until

CarbiMet 6 (27)
Water cooled Comp. plane

6-µm MetaDi Supreme 150

UltraPol 6 (27) 5:00
diamond suspension Comp.
3-µm MetaDi Supreme 150
TexMet® 1000 6 (27) 3:00
diamond suspension Comp.
1-µm MetaDi Supreme 120
TriDent 6 (27) 2:00
diamond suspension Comp.
0.05-µm MasterMet 120
MicroCloth 5 (22) 2:00
Colloidal silica Contra
Copper, Nickel and Cobalt

Material
• UNS C52400
• ASTM B103
• SAE J461
• Cu – 0.16 P - 10 Sn
• Phosphor Bronze

Etchant
• Klemm’s III reagent

Description
• Dendritic structure of
chill-cast phosphor
bronze
Copper, Nickel and Cobalt

Material
• Cartridge brass
• Cu - 30Zn

Etchant
• Klemm’s III

Description
• Wrought cartridge
brass, cold reduced
50% and annealed at
704 ºC 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
Load Lb.
Base Speed Time
Surface Abrasive/Size (N)/
(rpm)/Direction (min:sec)
Specimen

240- (P280) grit SiC 240 Until

CarbiMet paper 6 (27)
Water cooled Comp. plane
ApexHercules™ H 9-µm MetaDi Supreme 150
6 (27) 5:00
rigid grinding disk diamond suspension Comp.
3-µm MetaDi Supreme 150
TriDent cloth 6 (27) 3:00
diamond suspension Comp.
0.05-µm MasterPrep 120
MicroCloth pad 6 (27) 1:30
alumina suspension Contra
 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 hot-
rolled alloy steel
revealing a bainitic
structure with a few
patches of pearlite,
acicular ferrite and
some patches of
proeutectoid ferrite.
 Ferrous Metals

Stainless Steel Procedure

Load Lb. (N)/ Base Speed Time
Surface Abrasive/Size
Specimen (rpm)/Direction (min:sec)

240- (P280) grit SiC 240 Until

CarbiMet paper 6 (27)
Water cooled Comp. plane

9-µm MetaDi Supreme 150

UltraPol cloth 6 (27) 5:00
diamond suspension Contra
3-µm MetaDi Supreme 150
TriDent cloth 6 (27) 5:00
diamond suspension Contra
0.05-µm MasterPrep 120
ChemoMet pad 6 (27) 2:00
alumina suspension Contra
 Ferrous Metals

Material
• UNS S41600
• AISI 416 (CTC P70)
• C 0.10 Cr 13.0 S >0.15
balance Fe
Etchant
• Beraha’s CdS reagent
Description
• Microstructure of “free-
machining” martensitic
stainless steel in the
quenched and tempered
condition. Note: gray
elongated sulfide
inclusions, white delta
ferrite and martensitic
matrix. 500X.
 Ferrous Metals

Material
• Custom Flo 302 HQ
• Fe-<0.08C-18Cr-9Ni-
3.5Cu
Etchant
• Tint etched with
Beraha’s BI reagent
Description
• Microstructure of hot-
rolled and solution
annealed and aged
precipitation hardened
stainless steel
revealing a fully
austenitic matrix.
Magnification bar is
100 µm long.
 Ferrous Metals

Cast Iron Procedure

Load Lb. (N)/ Base Speed Time
Surface Abrasive/Size
Specimen (rpm)/Direction (min:sec)

240- (P280) grit SiC 240 Until

CarbiMet paper 6 (27)
Water cooled Comp. plane

9-µm MetaDi Supreme 150

UltraPol cloth 6 (27) 5:00
diamond suspension Comp.
3-µm MetaDi Supreme 150
TexMet 1000 pad 6 (27) 4:00
diamond suspension Comp.
1-µm MetaDi Supreme 120
TriDent cloth 6 (27) 3:00
diamond suspension Comp.
0.05-µm MasterPrep 120
ChemoMet pad 6 (27) 2:00
alumina suspension Contra
 Ferrous Metals

Material
• Pearlitic Ductile Iron

Etchant
• Beraha’s CdS
reagent

Description
• Microstructure of
pearlitic ductile iron
containing graphite
nodules surrounded
by ferrite. Viewed
with polarized light
plus sensitive tint.
500X.
 Ferrous Metals

Material
• Pearlitic Gray Iron

Etchant
• Beraha’s CdS
reagent

Description
• Microstructure of
pearlitic gray cast
iron containing
ferrite near the
flakes.
 Precious Metals

Precious Metals Procedure

Load Lb.
Base Speed Time
Surface Abrasive/Size (N)/
(rpm)/Direction (min:sec)
Specimen

220- to 320- (P240 to P400) 150-240 Until

CarbiMet 3 (13)
grit SiC, water cooled Comp. plane

9-µm MetaDi II diamond 150-240

TexMet ® 1500 3 (13) 5:00
paste* Comp.
3-µm MetaDi II 150-240
TexMet 1500 3 (13) 3:00
diamond paste* Comp.
1-µm MetaDi II 150-240
TexMet 1500 3 (13) 2:00
diamond paste* Comp.
0.05-µm MasterPrep 100-150
MicroCloth 2 (9) 2:00
Alumina Comp.
* Use water as the lubricant, but keep the pad relatively dry.
 Precious Metals

Material
• Fine Silver,~100% Ag

Etchant
• Equal parts of 10%
NaCN and 10%
ammonium persulfate

Description
• Equiaxed FCC grain
structure with
annealing twins
 Precious Metals

Material
• 18-k Gold, 75 Au –
22 Ag – 3 Ni

Etchant
• Equal parts of 10%
NaCN and H2O2
(30% conc.).

Description
• Equiaxed FCC grains
with annealing twins.
Specimen was attack
polished.
 Precious Metals

Material
• Paliney 7 (35% Pd –
30% Ag – 14% Cu –
10% Pt – 10% Au –
1% Zn)

Etchant
• Aqua regia

Description
• As-cast dendritic
structure.
 Precious Metals

Material
• As-cast ruthenium

Etchant
• None, polarized light

Description
• As-cast grain
structure of high-
purity ruthenium.

200 µm
 Low-Melting Point Metals

Low-Melting Point Metals Procedure

Load Lb.
Base Speed Time
Surface Abrasive/Size (N)/
(rpm)/Direction (min:sec)
Specimen

400- (P600) grit SiC, water 150-250 Until

CarbiMet 4 (18)
cooled, wax coated Comp. plane

600- (P1200) grit SiC, water 150-250

CarbiMet 4 (18) 5:00
cooled, wax coated Comp.
800- (P1500) grit SiC, water 150-250
CarbiMet 4 (18) 3:00
cooled, wax coated Comp.
1-µm Micropolish II 120-150 4:00 –
MicroCloth 5 (22)
alumina suspension Comp. 5:00
0.05-µm MasterPrep 80-150
MicroCloth 4 (18) 4:00
Alumina Contra
Use candle wax to coat the SiC paper
 Precious Metals

Material
• Cd – 20Bi

Etchant
• None, polarized light

Description
• As-cast dendritic
structure – primary
Cd dendrites and a
Cd-Bi eutectic

200 µm
 Precious Metals

Material
• Zn – 0.1Cu – 0.1 Ti

Etchant
• None, polarized light

Description
• As-cast cellular
structure of alpha-
Zinc and a ternary
eutectic. Note the
large mechanical
twins from
deformation.

50 µm
 Precious Metals

Material
• Bi – 40 Sn

Etchant
• FeCl3 – HCl - Ethanol

Description
• As-cast eutectic of
nearly pure Bi and Sn

20 µm
 Precious Metals

Material
• Bi – 55% Pb

Etchant
• Pollack’s reagent

Description
• As-cast. Primary β,
BiPb3, and then a
eutectic of β and Bi
formed.

50 µm
 Introduction

Etching
Techniques
– Swab
– Immersion
– Electrolytic

• Black & White

• Color 100 µm
 Etching

Etching Reveals
• Grain boundaries • Dendritic patterns
• Phases • Segregation
• Constituents • Deformation
• Homogeneity
• Coatings and Platings
• Interfaces
• Heat affected zones
• Reaction zones
 Etching

Techniques
• Swab
Attack controlled by
• Immersion chemical selection,
time, current, voltage
• Electrolytic
 Etching

Etchant Selection
Low-carbon sheet steel

2% Nital 4% Picral Beraha’s reagent

Reveals ferrite grain Reveals cementite Colored grains based on
boundaries and cementite crystallographic orientation
 Etching

4% Picral 2% Nital

Microstructure of as-rolled Fe – 1.31% C – 0.35% Mn – 0.25% Si high-carbon water

hardenable tool steel. Note the Widmanstätten intragranular cementite that precipitated as pro-
eutectoid cementite before the eutectoid reaction. Originals at 1000X.
 Etching

Microstructure of the as-rolled Fe – 1.31% C – 0.35% Mn – 0.25% Si specimen with the

intergranular carbide network clearly visible after etching with alkaline sodium picrate, 90 °C –
60 s. Original at 500X magnification. Note also some intragranular Widmanstätten cementite.
 Etching

Cartridge Brass, 50% CR,

200 µm Fully Annealed
NH4OH-H2O2 (3% Conc.)

Klemm’s I Klemm’s II
Polarized Light + Sensitive Tint
Cartridge Brass, 50% Etching
CR, Fully Annealed

Klemm’s III Beraha’s PbS

Polarized Light + Sensitive Tint

 Carbon Steel Weld HAZ Etching

2% Nital

Base
Weld Metal

Klemm’s I
 Technical Help

Information Availability
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– Buehler Book
– Tech Notes
• Email
– Techsupport.com, ask a specific question directly to
Buehler’s lab
– Join Buehler’s E-club
• Technical updates
• New product information
Etching
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