Preparation for Electron
Backscatter Diffraction with LaboPol-4 /
LaboForce-1
Danka Katrakova1, Morten J.
Damgaard2 and Frank Mücklich3
1
Continental AG, Hannover,
Germany; previously at 3;
katrakova@hotmail.com
2
Struers A/S, Kopenhagen,
Denmark
3
Saarland University, Functional
Materials, Saarbrücken,
Germany
Abstract
The LaboPol-4/LaboForce-1
combination that allows low load
and low rotation speed was used
to prepare a large variety of sam-
ples for Electron Backscatter Dif-
fraction (EBSD).
As the signal comes from inter-
action in a very thin surface layer,
this method requires a very gen-
tle preparation without any re-
sidual distortion on the specimen
surface.
In this paper a preparation strat-
egy for EBSD is discussed and
successful preparation proce-
dures for 16 different materials
(metals, intermetallics and ce-
ramics) are given. The results are
compared with alternative prepa-
ration routes like modified stand-
ard polishing and vibratory pol-
ishing.
Introduction
Electron Backscatter Diffraction
(EBSD) has become very popular
among materials and earth sci-
entists since the first commercial
automatic systems were avail-
able in 1994. The main advan-
tage of this method is the possi-
bility to link morphology (grain
size and shape) with
crystallographic features (phase,
orientation, disorientation) on the
microscopic scale but still in a
representative specimen area
[92Ran], [93Schw], [93Wri],
[98Kat]. The preparation is far
simpler than that of thin foils for
TEM, but it is also much more
demanding than that for normal
imaging in the SEM. This is
mainly due to the very low infor-
mation depth of the EBSD signal
based on channelling effects.
After standard preparation proce-
dure - mechanical grinding and
polishing - a thin residual surface
distortion layer is left [82Sam],
[99Pet], [99Van]. This layer is not
really disturbing when light or
scanning electron microscopy is
used, especially if it is removed
by etching. In the case of EBSD
though this is often not sufficient
for a good pattern quality. Some
additional effort may be neces-
sary. In general, classical etching
is not needed for EBSD because
the contrast is defined through
the orientation differences. It is
even avoided as the induced sur-
face roughening is disturbing due
to the high specimen tilt (70°).
Preparation Strategy
for EBSD
In order to obtain a flat Mechanical grinding and polishing
and even distortion free
specimen surface the
standard grinding and Mechanical
polishing procedures treatment
have to be adjusted.
These modifications
mainly concern the final
preparation stage.
polishing
vibratory
As a general guideline
reduced loads and ro-
tation speed should be
used for mechanical
grinding and polishing.
The final step can be Fig.1: Preparation strategies
performed in different for EBSD
ways that would depend on the
type of material as summarised
in Fig. 1. Very often vibratory pol-
ishing with colloidal silica is the
best solution. The polishing time
can be of about some hours.
Therefore polishing cloths should
be chosen very carefully in order
to avoid relief on the specimen
surface. If such equipment is not
available normal rotation polish-
ing with silica could also provide
acceptable results. Some
etchant may be used for speed.
Chemical polishing and slight
etching are very fast and they
surely remove any residual distor-
tion. But care should be taken to
avoid surface layers as well as
pitting and/or severe roughening.
Another very recommended
method is electropolishing.
Again, no surface layer should be
left. Unfortunately electro-
polishing is restricted to electri-
cally conductive materials.
Some physical methods are very
useful for 'difficult' materials like
ceramics, minerals or metals with
high oxygen affinity. Especially
oxidation layers should be
final step
Chemical Physical
treatment treatment
electropolishing
colloidal silica
etch-polishing
annealing
ion beam
polishing
polishing
chemical
cleaning
etching
plasma
slight
19
avoided - therefore annealing of
metals for example should take
place in inert gas atmosphere or
in vacuum. Beam energies if us-
ing ion beam or reactive plasma
should be rather low to avoid ad-
ditional damage.
Experimental
Equipment
Conventional mechanical rota-
tional grinding and polishing al-
low 5 N force and 150 rpm rota-
tion speed as a minimum. This
equates to a relative velocity of
approximately 1 m/s in a 250
mm system. With the LaboForce-1
the load can be varied between 0
and 20 N in 2,5 N steps. The
LaboPol-4 allows gradual change
of the rotation speed between 0
and 150 rpm; the specimen
holder rotates at 8 rpm, that al-
lows relative velocities between 0
and 0.88 m/s. Obviously by us-
ing this equipment a very gentle
preparation is possible. But of
course preparation time signifi-
cantly increases.
20
This is a disadvantage when
compared to standard mechani-
cal polishing. Another drawback
is the relatively poor polishing dy-
namics obtained when using pol-
ishing speeds above 10 rpm.
Due to the large difference be-
tween sample mover and disc
rotation speed the sample is
preferential polished in one direc-
tion. When using soft polishing
cloths this will lead to polishing
artefacts like comet tails [00Gee]
It can be also quite inconvenient
if really a long time is needed for
silica polishing, as it is not eco-
nomical regarding abrasive sus-
pension and manpower. Com-
pared to vibratory polishing this
is a disadvantage. But regarding
time this gentle rotational polish-
ing is still much faster than the
vibratory method so that the
whole preparation and not only
the final step can be completed
in reasonable time. Also wavi-
ness, that is typical when vibra-
tory ground, is almost not ob-
served.
Materials
Different materials were prepared
so that EBSP's of good quality
were obtained. The test materials
differ in hardness (which strongly
influences the preparation behav-
iour) and also in their EBSD infor-
mation depth.
The escape depth of the back-
scattered electrons depends on
the atomic number and weight
as well as on the density of the
material and on the energy of the
electrons [93Joy]. Only little is
known about the exact informa-
tion depth of EBSD. Since only
backscattered electrons with low
energy loss contribute to the pat-
tern formation (whereas the other
build the diffuse pattern back-
ground) it is much lower. It de-
pends on the atomic number and
weight, the density, also on the
acceleration voltage in the SEM.
Some attempts have been made
to calculate the spatial resolution
(including depth) for some mate-
rials via Monte Carlo simulation
[98Ren]. Considering those re-
sults the information depth for
Fig. 2:
Test materials
differing in hardness
and EBSD
information depth;
R(BS) corresponds
to the escape depth
of the backscattered
electrons at 20 kV;
R(EBSD) is about
25 % of R(BS).
EBSP of some
materials are
included with their
PQI
 Sample
1 standard
2 standard
3 standard
4 new
the EBSD signal is ap-
proximately a fourth of 5 vibratory
the escape depth of the
backscattered elec-
trons in general for a cut-off en-
ergy of 90 % that of the primary
electrons.
For mechanical preparation and
the residual strain induced into
the materials surface it is impor-
tant to consider the hardness of
the material. Main parameters for
hardness are the chemical com-
position and processing history.
The investigated materials cover
the range from 5.5 to 1756 HV,
the roughly estimated EBSD in-
formation depth is between 20
and 370 nm (Fig. 2) [00Kat].
All materials were chosen to be
coarse grained and relaxed to
ensure that any pattern distortion
comes from the preparation.
Procedure
From each material five samples
were taken. Three of them were
ground and polished on a stand-
ard rotational polishing machine
(RotoPol-22 / RotoForce-4). The
final step was done once on the
same machine, once on the new
one (LaboPol-4 / LaboForce-1)
and on the vibratory polisher re-
spectively. The fourth sample
was prepared entirely on the new
machine and the last was vibra-
tory ground and polished (Fig. 3).
Preparation was stopped when
an optically (light microscopy)
good specimen surface was
achieved. EBSP quality was
checked. If needed the final step
was repeated, modified or con-
sidered inappropriate and conse-
quently another approach was
chosen.
Grinding Final
polishing polishing
standard
new
vibratory
new
vibratory
Results and Discussion
The quality of the preparation
was judged by using the EBSP
quality (pattern quality index) as a
measure [00Kat].
A reliable automatic EBSD scan
is only possible if the EBSP's are
of good quality (contrast) so that
they can be recognized by the
computer. The average height of
the detected peaks in the Hough
transformation that is used for
pattern recognition [92Kri] can be
used as a quality parameter
[94War], [98TSL]. It should be
noticed that the so defined pat-
tern quality index (PQI) is also
dependent on other factors like
crystal system, orientation, etc.
Nevertheless it is a very good
measure, even not absolute, for
the strain in the diffraction vol-
ume of material. For automatic
scans a PQI above 80 is desir-
able. But depending on the crys-
tal symmetry and orientation pat-
tern with much lower PQI can be
indexed correctly as well.
Using standard mechanical
preparation procedure some-
times good results were ob-
tained. This was especially the
case for very hard materials like
ceramics but also for a couple of
metals. It must be mentioned
though that any kind of chemical
or physical support was needed
as well. The most important ad-
vantage remains the short prepa-
ration time. More "difficult" mate-
rials could be managed very of-
ten when transferred for final
38
Preparation for Electron
Backscatter Diffraction
with LaboPol-4 / LaboForce-1
stage to the new machine and
almost always on the vibratory
one.
When the new device was used
for the whole preparation all met-
als could be prepared so that
EBSP of excellent quality were
observed. Often an etchant was
added to increase preparation
speed. Hard materials (HV > 250)
were not easy to prepare espe-
cially without chemical support.
Ceramics could not be prepared
satisfactorily in reasonable time.
Some more trials especially by
varying polishing cloths and
abrasives may lead to another
result.
Vibratory polishing delivers
mostly the best quality EBSP's.
The main drawback is the enor-
mous time expense. But normally
it can be accepted as no addi-
tional abrasive or manpower are
needed. If the entire preparation
(including grinding) is done vibra-
tory a high surface waviness is
observed because the scratch
depth cannot be reduced as effi-
ciently as the deformation depth.
Due to the long polishing time
strong relief may appear, espe-
cially in ceramics. Therefore
cloths must be chosen very care-
fully.
Fig. 4 and Fig. 5 compare the
standard preparation route as
well as vibratory polishing with
mechanical polishing using re-
duced pressure and rotation
speed. In both cases the used
material is Titanium. In compari-
son to the standard preparation
route it can be seen that there is
some deformation left, especially
in the edge region - i.e. deforma-
tion twins. Also the contrast in
the light micrograph as well as in
21
the EBSP is lower that again
confirms surface damage. The
result with this softer rotation
polishing is comparable to that
achieved using vibratory polisher.
But it is much faster. Compared
to a specimen prepared only by
vibratory polishing this machine
has an advantage regarding
evenness and flatness (Fig. 5).
In a laboratory with all these
equipment the preparation strat-
egy for materials harder than 80
HV would be standard mechani-
cal grinding and polishing fol-
lowed by modified final stage on
the polishing device with reduced
pressure and rotation speed abil-
22
ity. Sometimes it may be suffi-
cient to use the standard ma-
chine especially if supported
chemically. But sometimes even
the new machine may have diffi-
culties or imply a very long proc-
ess. In that case the vibratory
polisher would be preferred. Soft
materials (HV below 80) should
be ground and polished on the
new machine and (if needed)
taken to the vibratory polisher for
the final step (Fig. 5). Often etch-
ing between the different polish-
ing steps is very helpful to re-
move the deformation. This also
significantly speeds up the pro-
cedure. If etchant is added on
a)
b)
the final stage it should not be
too much as it is applied just to
speed up the process and solve
the deformed layer, not really to
achieve the etch effect.
Conclusions
LaboPol-4/ LaboForce-1 is a
very useful polishing device for
EBSD specimen preparation. Es-
pecially for soft metals the whole
preparation can be performed
very gently, time efficiently and
with a minimum of surface relief.
It can be also recommended for
the final polishing step when
silica suspension is used. This is
applicable to all materials and
even to ceramics.
This machine might also be use-
ful for the preparation of other
soft materials like polymers or for
other surface sensitive tech-
niques like AFM / STM.
Acknowledgement
The authors would like to thank
all Struers co-workers who sup-
ported them with advice regard-
ing the preparation procedures
for the different materials.
Appendix
Preparation Procedures for the
Investigated Materials
Only preparation procedures
where the LaboPol-4/
LaboForce-1 is involved are in-
cluded. Alternative preparation
Fig. 5:
a) correctly prepared sample with
high PQI (s. Fig. 4a)
- low roughness: 8 nm;
b) whole preparation done by
vibratory polishing - roughness
significantly higher: 229 nm.
Measured area: 1.26 mm x 0.95 mm.
 38
Preparation for Electron
Backscatter Diffraction
with LaboPol-4 / LaboForce-1

Material References

[00Gee] Geels, K.; Gillesberg,

Surface Grit, Lubricant Rotation Force [N] Time B.: Polishing Dynam-
Grain size speed (min) ics, Prakt Metallogr 37
[rpm]
(2000) 150
Sn SiC-paper # 4000 Ethylenglycol 150 5 until plane
MD-Pan 6 µm Blue 150 5 5
Etching: * = 5 g Ammonium Persulfate + 50 ml dist. Water, 10-15 s
[00Kat] Katrakova, D.;
Mücklich, F.;
MD-Mol 3 µm Red 100 5 30
MD-Chem OP-S* Water, Soap 75 2.5 10 Damgaard, M.J.:
Specimen Preparation
Al SiC-paper # 1200 Wax; Water 150 5 until plane
and Electron
MD-Mol 3 µm Green 150 5 15 Backscatter Diffraction,
MD-Dur OP-S Water, Soap 100 5 15 Proc. EuroMet 2000,
MD-Nap OP-S Water, Soap 100 2.5 5 Saarbrücken, Germany
(2000) to appear
Zn SiC-paper # 1200 Ethylenglycol 150 5 until plane
MD-Mol 3 µm DiaPlus 150 5 15
MD-Nap OP-U* Water, Soap 100 5 5
[99Pet] Petzow, G.:
Metallographic Etching,
* = Nital, 3 %
Ohio, ASM International
(1999)
Mg SiC-paper # 2400 Ethylenglycol 150 5 until plane
MD-Mol 3 µm Yellow 150 5 20
[99Van] Vander Voort, G.F.:
Etching: Nital, 3 %( Isoamylalkohol), 10-20 s
Metallography Princi-
MD-Nap 1 µm Yellow 100 2.5 15
MD-Chem OP-S Ethanol (1:1) 75 2.5 15 ples and Practice,
Avoid water contact, Only clean with Ethanol, Use DP-A
Ohio, ASM Interna-
tional, Materials Park
(1999)
Cu SiC-paper # 1200 Water 150 5 until plane
MD-Pan 9 µm DiaPlus 150 5 15
Etching: * = 3.3 g FeCl 3 + 10 ml HCl + 40 ml dist. H 2O, some seconds [98Kat] Katrakova, D.;
MD-Mol 3 µm DiaPlus 150 5 45
Mücklich, F.: Orienta-
MD-Chem OP-S* Water, Soap 100 5 30 tion Imaging
Microscopy - a Power-
Al (Li) SiC-paper # 1200 Water 150 5 until plane ful Tool for Materials
SiC-paper # 4000 Water 150 5 5 Characterization,
MD-Dur OP-S Water, Soap 100 2.5 25 www.uni-sb.de/
MD-Nap OP-S Water, Soap 75 2.5 60
techfak/fb15/fuwe/oim
(1998)
Fe SiC-paper # 800 Water 150 7.5 until plane
MD-Allegro 6 µm Water 150 7.5 10
MD-Dac 3 µm Blue 150 Blue 15 [98Ren] Ren, S.X.; Kenik, E.A.;
MD-Chem OP-S Water, Soap 100 5 10 Alexander, K.B.; Goyal,
A.: Exploring Spatial
Resolution in Electron
routes are given only if they lead LaboForce-1 is not the same as Back-Scattered Diffrac-
to better results by means of the 150 rpm on a standard pol- tion Experiments via
EBSP quality. Generally, Struers ishing machine. This is because Monte Carlo Simula-
tion, Microsc Microanal
consumables were used. Other- the samples rotate at 8 rpm and
4 (1998) 15
wise it is notified. Which are the not as usual at 150 rpm. If an
corresponding products from etchant was added to the silica [98TSL] TSL: OIM Data Collec-
competitors can be found in suspension, this is noted with a tion User Manual,
[99Pet]. Please keep in mind that star (*) and its chemical composi- Drapper, Utah, USA,
150 rpm on the LaboPol-4 / tion is given in the respective TexSEM Laboratories
part of the table. (1998)

23
Material

Surface Grit, Lubricant Rotation Force [N] Time

Grain size speed (min)
[rpm]
Ti SiC-paper # 500 Water 150 10 until plane
SiC-paper # 1200 Water 150 10 20
MD-Chem OP-S Water, Soap 100 7.5 90

Be SiC-paper # 1200 Water 150 10 until plane

MD-Largo 9 µm DiaPlus 150 10 10
MD-Nap 1 µm Red 150 10 15
Slight etching: H 2SO 4, 10 %, some seconds
[94War] Wardle, S.T.; Lin, L.S.;
Cetel, A.; Adams, B.L.:
Ni SiC-paper # 1200 Water 150 15 until plane
Orientation Imaging
MD-Dac 3 µm Green 150 10 20
LeCloth Alumina, 1 µm Water 100 7.5 20 Microscopy: Monitoring
LeCloth Alumina, 0.3 µm Water 100 7.5 25 Residual Stress Profiles
MD-Chem OP-S Water, Soap 100 7.5 15 in Single Crystals Using
an Image Quality Para-
TiAl SiC-paper # 500 Water 150 10 until plane meter, IQ, Proc.
MD-Dur 6 µm Blue+H 2O2,1:1 150 15 35 MSA'94, New Orleans
MD-Dur 3 µm Blue+H 2O2,1:1 150 12.5 15
MD-Chem OP-S* Water, Soap 75 7.5 15 (1994) 680
OPS* = OPS + H2O2 + NH 4OH = 8:1:1
[93Joy] Joy, D.C.: Scanning
Electron Microscopy in
RuAl MD-Pan 15 µm Red 150 15 until plane
MD-Dur 6 µm Blue 150 15 10 Materials Science and
MD-Dur 3 µm Blue 150 15 10 Technology 2A, Cahn,
LeCloth Alumina, 1 µm Water 100 10 20 R. W. ;Haasen, P., VCH
LeCloth Alumina, 0.3 µm Water 100 10 25
MD-Chem OP-S Water, Soap 100 10 15
(1993) 221

[93Schw] Schwarzer, R.A.: The

RhAl SiC-paper # 800 Water 150 15 until plane
MD-Allegro 6 µm Green 150 15 15 Determination of Local
MD-Dac 3 µm Green 150 15 20 Texture by Electron Dif-
MD-Dur 1 µm Green 150 15 30 fraction - A Tutorual
MD-Chem OP-S Water, Soap 100 10 30 Review, Tex Microstr 20
Etching: 10 ml HNO3 + 100 ml HCl + 50 ml H 2O, hot, 1-5 min (1993) 7

[93Wri] Wright, S.I.: A Review

Material of Automated Orienta-
tion Imaging
Microscopy (OIM), J
Surface Grit, Lubricant Rotation Force [N] Time Comp Assisted
Grain size speed (min) Microscopy 5 (1993)
[rpm] 207
BaTiO 3 RotoPol 22 / RotoForce 4
MD-Plan 15 µm Blue 150 25 until plane [92Kri] Krieger Lassen, N.C.;
MD-Allegro 6 µm Blue 150 25 5 Juul Jensen, D.;
MD-Pan 6 µm Blue 150 30 7
MD-Dac 3 µm Blue 150 25 5 Conradsen, K.: Image
LeCloth Alumina, 1 µm Water 150 20 5 Processing Procedures
LeCloth Alumina, 0.3 µm Water 150 20 5 for Analysis of Electron
Etching: 5 ml HCl + 5 ml HNO3 + 1 ml HF + 89 ml H 2O, 5-10 seconds Back Scattering Pat-
terns, Scanning
ZrO2 RotoPol 22 / RotoForce 4 Microscopy 6 (1992)
MD-Plan 15 µm DiaPlus 150 25 until plane 115
MD-Plan 9 µm DiaPlus 150 25 5
MD-Plan 6 µm DiaPlus 150 25 10 [92Ran] Randle, V.: Microtexture
MD-Dur 3 µm DiaPlus 150 25 10
MD-Dur 1 µm DiaPlus 150 25 10 Determination and its
MD-Plus 0.25 µm DiaPlus 150 20 10 Applications, London,
MD-Chem OP-AA Water 150 20 15 The Institute of Materi-
Annealing: 1200 °C, 10 min als (1992)

Al 2O3 RotoPol 22 / RotoForce 4 [82Sam] Samuels, L.E.:

MD-Plan 15 µm DiaPlus 150 30 until plane Metallographic Polish-
MD-Plan 9 µm DiaPlus 150 30 5 ing by Mechanical
MD-Plan 6 µm DiaPlus 150 30 10
Methods, Ohio, ASM
MD-Dur 3 µm DiaPlus 150 30 10
MD-Dur 1 µm DiaPlus 150 25 10 International, Metals
MD-Plus 0.25 µm DiaPlus 150 25 10 Park (1982)
MD-Chem OP-AA Water 150 20 15

24 Annealing: 1200 °C, 15 min