EBSDPrep

Mechanical Specimen
Preparation for EBSD
G. F. Vander Voort, Buehler Ltd

and
E. P. Vander Voort, Polzunov Institute
Rules for Pain-Free Preparation!
• >90% of all problems start in sectioning

• Sectioning is a very violent process
• Minimize sectioning damage and your life
is much easier!!
Most problems come from excessive damage

created during sectioning, therefore -
Cut specimens with an abrasive blade

designed for metallography using
adequate coolant and avoiding excessive
pressure to minimize damage!
If the specimens are not too big, <1-inch

(25-mm) in diameter, use a low-speed
saw or a precision saw with the
appropriate blade. These blades are very
thin and the damage introduced in
sectioning is very low while the surface
finish is excellent.
Shearing Damage
Damage
This piece of cartridge brass, Cu –

30% Zn, was sheared.
Band Saw Cutting Damage
Cartridge brass, Cu – 30% Zn, cut with a band saw:

LOM image (left) and EBSD IQ+GO maps (right).
Abrasive Saw Cutting Damage
1000x
Cartridge brass, Cu – 30% Zn, cut with an abrasive

saw: LOM image (left) and EBSD IQ+GO map (right).
Sectioning Damage
Sectioning damage on Al – 0.5% Cu (left)

and Al – 2% Cu (right).
Sectioning Damage in CP Ti (hcp)
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).
Damage from Lack of Coolant
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 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

Abrasive Wheel Selection
• SiC wheel - nonferrous materials
• Al2O3 wheel- ferrous materials
• “Hard” bond wheel - cut soft material
• “Soft” bond wheel - cut hard material

“Hard” and “soft” are poor terms, what we are trying to say is a blade
with strongly bonded abrasives versus one with weakly bonded abrasives
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

Rubber Al2O3
HRB
Medium Hard Nonferrous Materials:
Uranium, Titanium, Zirconium (Refractory Rubber SiC
Metals)
Soft Nonferrous Materials: Aluminum, Brass,
Rubber SiC
etc.
Very Hard, Brittle Fracture Materials:

Metal Diamond
Carbides, Ceramics, Minerals
Precision Saws
• Precision positioning
• Small kerf loss
• Diamond blades, thin abrasive
wheels
• Applications
– Delicate components
– Ceramics, Carbides, Nitrides
– Biomaterials
Wafering Blade Selection
Application Blade
Plastics, polymer, rubber 30 HC diamond
Aggressive sectioning: ferrous and nonferrous materials 20 HC diamond

including titanium alloys
General use: ferrous and nonferrous alloys, copper, aluminum, 15 HC diamond
composites, thermal spray coatings, pc boards
Hard/tough materials: Boron nitride, Silicon nitride 20 LC diamond
Hard/brittle materials: structural ceramics, glass, electronic 15 LC diamond

substrates, alumina, zirconia, concrete
Lower hardness/low density ceramics, electronic packages, 10 LC diamond
packaged integrated circuits, GaAs, AlN
Soft, friable ceramics, electronic packages, un-mounted silicon 5 LC diamond
chips, carbon composites, CaF2, MgF2
Carbon steels, high alloy steels, cobalt alloys, nickel-based Cubic boron nitride
superalloys, and lead alloys
• If edge retention is required, mount your

specimens using a compound that avoids
shrinkage gaps, such as EpoMet resin.
• For conductivity, use ProbeMet – which
also gives excellent edge retention
• To get the best flatness, use central force
loading rather than individual force
loading
Un-mounted Specimens Yield Poor
Edge Retention!
The decarburized surface of this heat treated specimen of 440A stainless steel
cannot be measured accurately due to rounding; the specimen was not mounted
(Fry’s Reagent).
Edge Retention
PhenoCure™ mounting compound EpoMet® mounting compound

Improperly carburized 8620 alloy borided 42CrMo4 alloy steel
(arrow points to gap) 500 X 1000 X
Edge Retention
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.
Edge Retention
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.
Use an automated grinder/polisher for

best results and reproducibility. Execute
each step using the correct
load/specimen, time, rpm of the platen
and holder, and the relative platen and
holder directions.
Automation Benefits
• Increase daily output

• Improve consistency
• Improve edge
retention, relief
control and overall
flatness
When you have obtained a low-damage

surface and a decent surface finish,
begin grinding with the finest possible
particle size abrasive, either as SiC or
Al2O3 papers or fixed diamond (DGD)
or diamond added to a RGD
Damage from 60-Grit SiC Grinding
1000x
Damage from grinding cartridge brass with 60-grit SiC:

LOM image (left) EBSD IQ+GO map (right)
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
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
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
Use flat, woven “hard” cloths,

chemotextiles or synthetics for the
diamond polishing stages with an adequate
amount of lubricant.
Keep the polishing surface uniformly

covered with abrasive and lubricant
throughout the polishing cycle. Don’t let
the surface get dry as this will lead to
smear, distortion and pull-out. The
lubricant must exhibit lubricity.
Sufficient abrasive must be added to
achieve a good cutting rate.
Depending upon the metal/alloy being

prepared, it may be necessary to use an
attack-polishing agent in the final step, or
follow preparation with a brief chemical
polish or with a vibratory polish (20-30
minutes is usually adequate).
But, these processes, e.g., electrolytic, ion-
beam or chemical polishing, must not
reduce surface flatness
Nano-indentation Test Results on Cartridge
Brass as a Function of Test Load
All
Hit 1 um Diamond Hit 3 um Diamond Hit 0.05 um Master Prep Alumina Hit 0.05 um MM colloidal Si Vibra
3000
2800
2600
2400
Hardness
2200
2000
1800
1600
1400
1200
1000
0.1 0.3 0.5 0.7 1 1.2 1.5 2 3 4 5 6 7 8 10 12.5 15 20 40 60 80 100
Load
As surface damage is removed, the same true hardness is

achieved at lower and lower test loads.
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.
Embedded Abrasive
10 µm
Examples of embedded abrasives: Left, SiC from grinding

embedded in a weld in 6061-T6 aluminum (0.5% HF etch);
Right, 3-µm diamond embedded in a steel specimen (unetched).
SiC
Embedded
in Lead – 100 µm
and its
After 0.05-µm Al2O3 – 5 min
After 1-µm Diamond Polish removal
100 µm
After Colloidal Silica, Vibratory Polish,
After 0.05-µm Al2O3 – 3 min Pollack’s Reagent
Water Stains – Poor Drying
Example of a poorly dried steel specimen (Nomarski DIC).

Vibratory Polishing
• Remove fine scratches

• Useful for materials
prone to smearing
• Great for difficult to
prepare materials
• Removes remnant
preparation damage
• Great for EBSD work!
Table 4: Band Contrast Improvement Due to Vibratory Polishing (20 min.*)
* A 60 minute vibratory polish was used for the lead specimen.
Improvement in Band Contrast Due to

Vibratory Polishing
High-Purity Element Mean Band Contrast (0 to 255)
Standard Method Standard + Vibratory

Polish
Mg 161.2 175.25 (+8.7%)
Si (single crystal) 205.75 233 (+13.2%)
Ti 134.0 146.2 (+9.1%)
Ni 85.0 102.8 (+20.9%)
Nb 145.6 151.2 (+3.8%)
Pb No pattern 108.0
20 minutes was used for all except 60 minutes for the lead
Influence of the Preparation Method on EBSD Measurements
Material: Invar T (Fe-36Ni) Preparation: mechanical only
Inverse Pole Figure Image Quality Kernel Average Misorientation
Green areas = areas

with higher deformation
Scan2
Material: Invar T (Fe-36Ni) Preparation: mechanical + electro-polish (A3, 29V, room temp., 25 s)
IQ gets worse because electro- Less deformation within

polishing caused rough surfaces most grains
Scan6
Material: Invar T (Fe-36Ni) Preparation: mechanical + electro-polishing (A3, 29V, room temp., 50 sec.)
IQ gets better again Less deformation within

most grains
Scan4
Material: Invar T (Fe-36Ni) Preparation: mechanical + electro-polishing (A3, 29V, room temp., 70 sec.,
Very bad due to

overpolishing
Scan5 Was lernt uns das? More is not always better …
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
Consult our SumMet Guide book,

Buehler’s Guide to Materials
Preparation, and read our extensive
paper, Mechanical Specimen
Preparation for EBSD, for methods
and ideas.
Generic Preparation Practice
Surface Grit/Abrasive Rpm Head/ Time
Load Base (min)
CarbiMet 120-320 grit 240-300 Contra U.P.
SiC/Water 5-6 Lb
UltraPol 9-µm Diamond/ 120-150 Contra 5
Cloth MetaDi Fluid 5-6 Lb
TriDent 3-µm Diamond/ 120-150 Contra 4
TriDent 1-µm Diamond/ 120-150 Contra 3
MicroCloth MasterPrep or 100-150 Contra 3
Pad MasterMet 5-6 Lb
1-µm step is optional; use with most difficult specimens
Charging a Cloth With Diamond
•Apply a liberal amount of paste over the cloth
surface
• Press the paste into the cloth with finger tip
• Add MetaDi Fluid and start cycle
• In contra*, squirt on a small amount of MetaDi
Diamond suspension every 30 s (more often in comp.)
• Keep cloth covered with abrasive and lubricant
* Contra is best with head speeds <100 rpm
Preparation of Aluminum
Surface Abrasive Load Platen Time
Size Lb (N) Speed/Direction (min.)
CarbiMet 240-grit SiC* 5 (22) 240 rpm 1 per
Contra sheet
UltraPol 9-m Diamond** 5 (22) 150 rpm 5
silk Contra
TriDent 3-m Diamond** 5 (22) 150 rpm 5
Polyester Contra
TriDent 1-m 5 (22) 150 rpm 3
Polyester Diamond** Contra
MicroCloth 0.05-m MasterMet 5 (22) 150 rpm 3
MicroCloth 0.05-m MasterMet - VibroMet2 60
* Water cooled; ** Add MetaDi Fluid lubricant

99.999% Al (fcc)
Standard Preparation: BC 151.1

Microstructure of Pure Al (99.999%)
Keller’s Reagent, 100x, DIC Barker’s Reagent, 50x, XP+ST

Preparation of Aluminum Alloys
Size Lb (N) Speed/Direction (min)
CarbiMet 220-320-grit SiC 5 (22) 200-240 rpm 1 each
water cooled Contra
UltraPol silk 9-m Diamond 6 (27) 150 rpm Contra 5-10
with MetaDi
Fluid
TriDent 3-m Diamond 6 (27) 150 rpm Contra 5-7
polyester with MetaDi
Fluid
MicroCloth MasterMet 6 (27) 100-150 rpm Comp. 3
Colloidal Silica
MicroCloth MasterMet - VibraMet 2  30
-Al dendrites in As-Cast Al – 7.12% Si
PQI = 87 ± 4.2
Microstructure of As-Cast Al – 7.12% Si
Bright Field Nomarski DIC
-Al dendrites and -Al/Si eutectic revealed by

etching with 0.5% HF, 200x
Preparation of Antimony
CarbiMet 320-grit SiC* 3 (13) 200 rpm 1 per
(waxed) Contra sheet
TexMet 9-m Diamond** 3 (13) 150 rpm 7
1500 Contra
TexMet 3-m Diamond** 3 (13) 150 rpm 6
1500 Contra
TriDent 1-m Diamond** 3 (13) 150 rpm 4
Polyester Contra
MicroCloth 0.05-m MasterMet 3 (13) 150 rpm 3

Antimony (rhombohedral)
Standard Preparation BC 180.2 Standard + Vibratory BC 184.8

Preparation of Bismuth
Size Lb (N) Speed/Direction
CarbiMet 240-grit SiC 4 (18) 240/contra 1 min
each
MicroCloth 5-m Al2O3 4 (18) 150/contra 5 min
MicroCloth 0.3-m Al2O3 4 (18) 150/contra 4 min
MicroCloth 0.05-m MasterPrep 4 (18) 150/contra 3 min
MicroCloth 0.05-m MasterMet - VibroMet 2 60
Pure Bismuth (rhomb./trigonal)
Standard Preparation, BC 255 Standard + Vibratory, BC 255

Microstructure of pure bismuth, as-polished.
Pure Bismuth
As-polished, Polarized Light

Preparation of Chromium
CarbiMet 240-grit SiC* 6 (27) 240-300 rpm 1 per
Contra sheet
CarbiMet 320-grit SiC* 6 (27) 240-300 rpm 1
Contra
UltraPol 9-m Diamond** 6 (27) 150-200 rpm 10
silk Contra
TriDent 3-m Diamond** 6 (27) 150-200 rpm 8
Polyester Contra
MicroCloth 0.05-m MasterMet 6 (27) 120-150 rpm 5
plus attack polish

Pure Chromium (Wrought)
EBSD patterns before (left) and after (right) indexing the body-centered cubic
crystal structure; pattern quality index = 260 ± 13.1
Wrought Pure Chromium
BF, Glyceregia Etch Nomarski DIC, Glyceregia Etch
Microstructure of the wrought pure chromium

Preparation of Copper

CarbiMet 240-grit SiC* 6 (27) 240 rpm/contra 1 each
CarbiMet 320-grit SiC* 6 (27) 240 rpm/contra 1
UltraPol 9-m Diamond** 6 (27) 150 rpm/contra 5
TriDent 3-m Diamond** 6 (27) 150 rpm/contra 5
TriDent 1-m Diamond** 6 (27) 150 rpm/contra 4
MicroCloth 0.05-m MasterMet 6 (27) 150 rpm/contra 3
MicroCloth 0.05-m MasterMet - VibroMet 2  60

99.98% Cu (fcc)
Standard Preparation BC 122.6

Microstructure of 99.98% Cu
Beraha’s PbS Tint Etch, XP + ST

Tough Pitch Copper - Wrought
With Twins After Twin Removal

1:1 NH4OH-H2O2 (3%) Beraha’s PbS Tint Etch

-Cu in Wrought Cu – 30% Zn (fcc)
PQI = 221 ± 8.6

Microstructure of Cartridge Brass

-Cu grain structure and annealing twins revealed using equal
parts of ammonium hydroxide and hydrogen peroxide (3%
concentration), 100x
Cu – 40% Zinc, Alpha-Beta Brass
SEM Image Index of Quality Map

Grain Orientation Map Inverse Pole Figure Map

Grain Orientation + IQ Map Inverse Pole Figure + IQ Map

Preparation of Cobalt and Alloys
CarbiMet 220-320 grit SiC – 6 (27) 200-250 rpm 1 each
water cooled Contra
UltraPol silk 9-m Diamond with 6 (27) 120-150 rpm Contra 10
MetaDi Fluid
TriDent 3-m Diamond with 6 (27) 120-150 rpm Contra 7
polyester MetaDi Fluid
TriDent 1-m Diamond with 6 (27) 100-150 rpm Contra 5
polyester MetaDi Fluid
MicroCloth 0.05-m MasterMet 6 (27) 100-150 rpm Contra 3
or MasterPrep
MicroCloth 0.05-m MasterMet - VibraMet 2  60
FCC Matrix in Elgiloy
PQI = 221.4 ± 7.4

Co – 20% Cr – 15% Ni – 15% Fe – 7% Mo – 2% Mn – 0.15%C
Microstructure of Elgiloy
Grain structure and annealing twins revealed by etching with

15 mL HCl – 10 mL acetic acid – 10 mL HNO3, 100x
Preparation of Pure Iron
Size Lb (N) Speed/Direction (min.
)
CarbiMet 240-grit SiC* 6 (27) 240 rpm/Contra 1 per
sheet
UltraPol 9-m Diamond** 6 (27) 150 rpm/Contra 5
silk cloth
TriDent 3-m Diamond** 6 (27) 150 rpm/Contra 5
polyester
TriDent 1-m Diamond** 6 (27) 150 rpm/Contra 3
MicroCloth 0.05-m MasterMet 6 (27) 150 rpm/Comp. 3

99.98% Fe (bcc)
Specimen not fully recrystallized

99.98% Fe (bcc)
Standard + Vibratory BC 111

Pure Iron (99.98%)
Grain Orientation Map Index of Quality Map

Pure Iron (99.98%)
IQ + Grain Orientation Map Klemm’s I, XP + ST 50X

Ferrite in Wrought Pure Iron
PQI = 249.6 ± 5.5

Microstructure of Pure Fe
Ferrite grain structure revealed by etching with 2% nital, 100x

Motor Lamination Steel, As-Received
Motor Lamination Steel
Klemm’s I, XP+ST 200x IQ + GO Map

Ferrite in Silicon Core Iron (bcc)
PQI = 199.9 ± 7.4
Fe – 0.03% C – 2.5% Si; Wet H2 Annealed

Microstructure of Silicon Core Iron
Ferrite grain structure revealed using 2% nital, 100x

10B21 Carbon
Steel
LOM Marshall’s/Nital
Grain Orientation Map
Index of Quality Map

2205 Duplex Stainless Steel
Grain Orientation Map

Inverse Pole Figure Map

Grain Orientation + IQ Map

Inverse Pole Figure + IQ Map

Preparation of Lead
CarbiMet 240-grit SiC* 4 (18) 240/contra 1 min
each
* Coat the SiC with paraffin wax

Relatively Pure Wrought Lead
EBSD patterns before (left) and after (right) indexing the face-centered cubic
crystal structure; pattern quality index = 49.3 ± 3.0
First attempt with Pb – 40 minutes Vibratory Polishing after standard prep.
Wrought Pure Lead – 1st Attempt
BF, Pollack’s Reagent DIC, Pollack’s Reagent
Microstructure of relatively pure wrought lead

Standard preparation plus 40 minutes Vibratory Polishing
Pure As-Cast Lead (fcc) – 2nd Trial
Standard + 60 minutes Vibratory Polish BC 108

(no EBSD pattern with standard preparation alone)
As-Cast Pure Lead – 2nd Trial
Pollack’s reagent, BF (left), DIC (right), 100x

Standard preparation plus 60 minutes Vibratory polish
Preparation of Magnesium
CarbiMet 240-grit SiC* 3 (13) 200 rpm/comp. 1/sheet
CarbiMet 320-grit SiC* 3 (13) 200 rpm/comp. 1
TexMet 1500 9-m Diamond** 5 (22) 150 rpm/comp. 8
TexMet 1500 3-m Diamond** 5 (22) 150 rpm/comp. 5
TriDent 1-m Diamond** 5 (22) 150 rpm/comp. 5
ChemoMet 0.05-m 3 (13) 120 rpm/contra 3
MasterPolish
MicroCloth MasterPolish - VibraMet 2  60
* Water as lubricant; ** Oil-based MetaDi Diamond Suspensions

Pure Magnesium (hcp)

Preparation of Pure Nickel
UltraPol 9-m Diamond** 6 (27) 150 rpm/comp. 8
MicroCloth 0.05-m 6 (27) 150 rpm/contra 3
MasterPrep
* Water as lubricant; ** Add MetaDi Fluid as lubricant

High-Purity Ni (fcc)
Standard Preparation BC 85 Standard + Vibratory BC 102.8

Wrought Ni 200, Relatively Pure Ni
EBSD patterns before (left) and after (right) indexing the face-centered
cubic crystal structure; pattern quality index = 176.3 ± 17.6
Wrought Cold Worked Ni 200
BF, 15 HCl – 10 Acetic – 10 HNO3 DIC, 15 HCl – 10 Acetic – 10 HNO3
Microstructure of wrought cold worked Ni 200

FCC Matrix of Wrought Hy Mu 80
PQI = 196.7 ± 7.2
Ni – 14.6% Fe – 4.3% Mo
Microstructure of Hy Mu 80
Grain and twin structure revealed by etching with 15 mL HCl

– 10 mL acetic acid – 10 mL HNO3, 100x
Alloy 625,
SA at 1100 °C
Grain Orientation Map Twins Removed
LOM 15 HCl-10Acetic-
10 HNO3
Index of Quality Map IQ + GO Map

FCC Matrix of Wrought Custom Age 625 PLUS
PQI = 200.5 ± 6.5

Microstructure of Custom Age 625 Plus
Austenitic grain structure and twins revealed by etching with

15 mL HCl – 10 mL acetic Acid – 10 mL HNO3, 200x
Preparation of Pure Niobium
Surface Abrasive Size Load Platen Time
Lb (N) Speed/Direction (min)
CarbiMet 240-grit SiC* 6 (27) 240/contra 1 each
CarbiMet 320-grit SiC* 6 (27) 240/contra 1
UltraPol 9-m Diamond** 6 (27) 180/contra 20
TriDent 3-m Diamond** 6 (27) 180/contra 16

ChemoMet 0.05-m MasterMet 8 (36) 150/contra 3
99.95% Nb (bcc)

BCC Matrix of Wrought Pure Nb
PQI = 166.2 ± 17.1

Microstructure of Wrought Pure Nb
Grain structure revealed by etching with lactic acid, nitric

acid, hydrofluoric acid (6:3:1), 500x
Preparation of Ruthenium
CarbiMet 120-grit SiC* 6 (27) 240/comp. 1 each
CarbiMet 240-grit SiC* 6 (27) 240/comp. 1.5
MicroCloth 3-m Diamond** 6 (27) 180/contra 8
MicroCloth 1-m Diamond** 6 (27) 180/contra 5
MicroCloth 0.05-m MasterMet 6 (27) 150/contra 3
* Add water as lubricant/coolant

HCP Matrix of Wrought Pure Ru
PQI = 266.2 ± 21.8

Microstructure of Wrought Pure Ru
Polarized Light, 100x Nomarski DIC, 500x
Grain structure of as-polished, wrought pure (99.95%) Ru

Preparation of Pure Silicon
each
Pure Single-Crystal Silicon (Diamond Cubic)
Standard Preparation BC 205.8 Standard + Vibratory BC 233

Polycrystalline Si (99.99999%)
EBSD patterns
from opposite
sides of a twin
boundary
Preparation of Pure Tantalum
CarbiMet 240-grit SiC* 6 (27) 240/contra 1 (2X)

ChemoMet 0.05-m MasterMet*** 8 (36) 150/contra 3
* Add water as coolant/lubricant; ** Add MetaDi Fluid lubricant; ***

1 part H2O2 (30% conc.) to 5 parts MasterMet
High-Purity Tantalum (bcc)

P/M Pure Tantalum
Microstructure of P/M tantalum etched with HCl – HNO3 – HF (equal parts)

Preparation of Pure Titanium
CarbiMet 240-grit SiC* 6 (27) 240/contra 1/sheet
MicroCloth 0.05-m 6 (27) 150/contra 10

MasterMet**
MicroCloth 0.05-m - VibraMet 2  60
MasterMet
* Add water as coolant; 1 part H2O2 (30% conc.) to 5 parts MM

99.999% Titanium
Standard Preparation BC 134 Standard + Vibratory BC 146.2

Three-Step Method for Ti and Alloys
CarbiMet 240-grit SiC with 6 (27) 240-300 rpm 1 each
water coolant Contra
UltraPol silk 9-m Diamond 6 (27) 120-150 rpm 10

with MetaDi Fluid Contra
MicroCloth 5 parts MasterMet 6 (27) 120-150 rpm 10

to 1 part H2O2 Contra
(30% conc)
Can follow with Vibratory polish using colloidal silica to enhance EBSD results
CP Ti – Grain Maps
Band Contrast Euler Coloring Map
Note Mechanical Twins

Microstructure of CP Ti (Grade 2)
3-Step Method 3-Step Method + Vibratory Polish, 30 min
Polarized Light, 100x

Preparation of Pure Tungsten

ChemoMet 0.05-m MasterMet*** 8 (36) 150/contra 3
* Add water as coolant/lubricant; ** Add MetaDi Fluid lubricant; ***

1 part H2O2 (30% conc.) to 5 parts MasterMet
High-Purity Tungsten (bcc)

BCC W in P/M W – 27% Cu
PQI = 296.9 ± 20.1

W Grains in P/M W – 27% Cu
Grain structure of P/M W-27% Cu, as polished, 500x

Preparation of Pure Vanadium
UltraPol 9-m Diamond** 5 (22) 150 rpm/comp. 10
MicroCloth 0.05-m 5 (22) 150 rpm/3-contra, 6
MasterMet 3-comp.
* Water as lubricant; ** Add MetaDi Fluid as lubricant

High-Purity Vanadium (bcc)

Microstructure of Pure Vanadium
Etched with equal parts glycerol, HNO3 and HF

Early Attempts With Zirconium
Mechanical Polish As Left + Chemical Polish
Pure Zr – neither are indexable.

Specimens Viewed with Polarized Light
High-Purity Zr As-Polished, Polarized Light EB Melted, HE and CD Zr

Preparation of Zirconium and Alloys for EBSD
Surface Abrasive/Size Load Speed Time
lbs. (N) rpm/Direction (min.)
CarbiMet 240 (P280) grit SiC 5 (22) 240 U.P.

water cooled Contra
CarbiMet 320 (P400) grit SiC 5 (22) 240 1

Water cooled Contra
UltraPol cloth 9-µm MetaDi diamond* 6 (27) 200 10

Contra
TriDent cloth 3-µm MetaDi diamond* 6 (27) 200 7

Contra
TriDent cloth 1-µm MetaDi diamond* 6 (27) 200 5

Contra
MicroCloth pad 0.05-µm MasterMet 6 (27) 200 7

Colloidal silica suspension Contra
*Charge with MetaDi Paste, add MetaDi Fluid; add MetaDi Supreme during cycle
**Attack polish with 1 part H2O2 (30%) to 5 parts Colloidal Silica
Results with Improved Method
Pure Zr (99.99%) EB Melted Zr (>99% pure)

Annealed Hot Extruded and Cold Drawn
Excellent Patterns; Indexed with High Confidence

Annealed 99.99% Zr
20 kV, 16.9 mm WD
1000x, 90.46% pixels
BC = 92.34
All Euler Angles + Band Contrast AVG = 22.7 m2

ASTM G = 12.5
Inverse Pole Figure + GBs (completed grains)

EB Melted Pure Zr, HE & CD
20 kV, WD = After grain extrapolation

94.11% pixels, BC = 98.33 Twins detected
<-1-120> blue
Mechanical Preparation Only <-2110> red

Zr – 2.5% Nb, 25% CR
Completed Grains in Random Color

Preparation of Pure Zinc
CarbiMet 240-grit SiC* 4 (18) 240/contra 1 each
MicroCloth 5-m Al2O3 4 (18) 150/contra 8
MicroCloth 1-m Al2O3 4 (18) 150/contra 5
MicroCloth 0.3-m Al2O3 4 (18) 150/contra 4
MicroCloth 0.05-m MasterMet 4 (18) 150/contra 3

Pure Zinc (hcp)

Pure Zinc
100 µm
Palmerton Etch, Polarized Light plus Sensitive Tint

Additional Test Results
Material PQI Material PQI

-Cu in 118.5 ± 8.7 -Cu in 150.4 ± 20.7
CDA 464 CDA 464
316 SS 184.9 ± 8.5 Ni 200 176.3 ± 17.6
Ferrite in 248 ± 15.4 Austenite in 207.9 ± 11
2205 DSS 2205 DSS
FG 718 80.7 ± 4.4 Pure Cr 259.8 ± 13.1
Pure V 125.9 ± 10.3 Pure Ta 169.7 ± 13.0
CP Ti 119.1 ± 4.1 Pure Bi 86.2 ± 1.8
Band Contrast Values using the Oxford Instruments HKL EBSD System
Atomic Number Crystal Structure Band Contrast (0-
High-Purity 255)
Elements
Mg 12 hcp 161.2
Al 13 fcc 151.2
Si 14 diamond cubic 205.8
Ti 22 hcp 134.0
V 23 bcc 102.2
Cr 24 bcc 88.27
Fe 26 bcc 105.4
Ni 28 fcc 85.0
Cu 29 fcc 122.6
Zn 30 hcp 170.8
Zr 40 hcp 77.3
Nb 41 bcc 145.6
Ru 44 hcp 66.0
Sb 51 rhombohedral 180.2
Ta 73 bcc 122.8
W 74 bcc 91.6
Pb 82 fcc 108*
Bi 83 rhomb./trigonal 255
* Results after vibratory polishing, as the band contrast was zero after the standard preparation cycle.
Conclusions
• Mechanical Specimen Preparation is Perfectly
Suitable for EBSD Work When Properly Done
• Do Not Etch Specimens!
• Follow Recommended Methods in the SumMet
Guide and Our EBSD Paper
• Follow Recommended General Rules

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Mechanical Specimen

Preparation for EBSD

G. F. Vander Voort, Buehler Ltd

• >90% of all problems start in sectioning

Most problems come from excessive damage

Cut specimens with an abrasive blade

If the specimens are not too big, <1-inch

This piece of cartridge brass, Cu –

Cartridge brass, Cu – 30% Zn, cut with a band saw:

Cartridge brass, Cu – 30% Zn, cut with an abrasive

Sectioning damage on Al – 0.5% Cu (left)

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

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

• Equipment (abrasive cut-off, precision saw)

Note: Delicate materials may require encapsulation

• SiC wheel - nonferrous materials

• Al2O3 wheel- ferrous materials

• “Hard” bond wheel - cut soft material

• “Soft” bond wheel - cut hard material

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

Very Hard, Brittle Fracture Materials:

Plastics, polymer, rubber 30 HC diamond

Aggressive sectioning: ferrous and nonferrous materials 20 HC diamond

Hard/tough materials: Boron nitride, Silicon nitride 20 LC diamond

Hard/brittle materials: structural ceramics, glass, electronic 15 LC diamond

• If edge retention is required, mount your

PhenoCure™ mounting compound EpoMet® mounting compound

Good edge retention in salt-bath nitrided 1215 carbon steel mounted in a)

Poor edge retention in salt-bath nitrided 1215 carbon steel

Use an automated grinder/polisher for

• Increase daily output

When you have obtained a low-damage

Damage from grinding cartridge brass with 60-grit SiC:

Use flat, woven “hard” cloths,

Keep the polishing surface uniformly

Depending upon the metal/alloy being

As surface damage is removed, the same true hardness is

Examples of embedded abrasives: Left, SiC from grinding

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

• Remove fine scratches

Improvement in Band Contrast Due to

Standard Method Standard + Vibratory

Si (single crystal) 205.75 233 (+13.2%)

Ti 134.0 146.2 (+9.1%)

Ni 85.0 102.8 (+20.9%)

Nb 145.6 151.2 (+3.8%)

Inverse Pole Figure Image Quality Kernel Average Misorientation

Green areas = areas

Inverse Pole Figure Image Quality Kernel Average Misorientation

IQ gets worse because electro- Less deformation within

Inverse Pole Figure Image Quality Kernel Average Misorientation

IQ gets better again Less deformation within

Inverse Pole Figure Image Quality Kernel Average Misorientation

Very bad due to

• Abrasive type, size and amount

Consult our SumMet Guide book,

MicroCloth 0.05-m MasterMet - VibroMet2 60

* Water cooled; ** Add MetaDi Fluid lubricant

Standard Preparation: BC 151.1

Keller’s Reagent, 100x, DIC Barker’s Reagent, 50x, XP+ST

Bright Field Nomarski DIC