Sampling, Preparation and Area Selection

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SAMPLING, PREPARATION AND AREA SELECTION
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DOI: 10.13140/RG.2.2.26813.97767
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28.05.2018
SAMPLING, PREPARATION AND AREA

SELECTION
Gert Nolze, BAM Berlin

Outline
1. Sampling
2. Area selection
3. Sample preparation
The basic problem for a metallographer preparing a specimen is that the

preparation process itself modifies the specimen surface and, theoretically,
a “true structure” completely without artifacts can never be obtained.
Geels, K.; Fowler, D. B.; Kopp, W.-U. & Rückert, M.
Metallographic and Materialographic Specimen Preparation,
Light Microscopy, Image Analysis and Hardness Testing.
ASTM International, 2007
28.05.2018 Sampling, preparation & area selectione 2

Sampling
You will get what you collect!

 Complex components versus simplified specimen geometry
(it is not the analyst’s fault when a specimen is not well selected or
improperly manufactured; cf. sample and microstructure symmetry)
 If you are part of a service unit, you are not responsible for the
collection / selection of the investigated sample.
 Nevertheless, try to get as many information as possible about

the specimen and the investigation issue before you start any
sample sectioning or preparation.
 Ask for the amount of specimen to be compared since this

decides whether you can use manual or you have to use
automated preparation procedures.

Sampling
 Sampling describes the extraction

of a subset in mass, volume, or
amount of specimens using defined
guidelines.
 For water, soil, air, blood and

many other materials very accurate
guidelines for sampling are
formulated in order to keep results
comparable and reproducible.
 In contrast to e.g. XRD, for EBSD a

standard procedure (DIN or ISO) for
sampling does not (yet) exist, i.e.
everybody uses his own procedure.
Therefore, sampling, sample prep
and area selection need to be
described as accurate as possible.

What is the purpose of a sample?
 A sample is selected to enable reliable findings and conclusions in

a representative way about quality, condition, composition etc.
 The aim of a sample but also of a scanned area by EBSD is a

statistically verified description of a specific material condition
(phase distribution, orientation, misorientation etc.) under ideal
imaging conditions (drift, distortions).
 Any possible variation/change/modification of the sample

properties during sampling or caused by a subsequent treatment
like preparation or selected investigation conditions diminishes the
key role of a sample and has to be prevented.
 Possible interferences have to be discussed critically, e.g. any

potential change during sample preparation (sampling, cutting,
embedding, grinding, polishing, coating), or reduced phase stability
in SEM due to electron or ion interaction (surface cleaning),
vacuum etc.
Area selection
The selected map is used to represent the entire material.

Therefore, make sure:
 The required area might not be identical with the location on
the sample where the best hit rates can be reached.
There might be a serious reason, why a mapping is possible or
not!
 Define position and size of the orientation map with respect

to the aim of the investigation (statistical relevance, reliability,
high confidence).
 If the area of interest is contaminated (e.g. by dust) or shows

damage remove the sample and clean or reprepare the
sample again, and do not move to a less relevant place.
 For publication or representation do not use the nicest but

the most informative orientation map.

Area selection
You will get what you select!

 For area selection this is the ordinary truth in particular for EBSD
because of the
‒ very short information depth ( sample preparation),
‒ often low statistical relevance ( multiple areas)
‒ (common) focusing on maximum hit rate in order to
get stunning orientation maps ( select areas you need)
‒ possibly existing microstructure gradients
‒ …
 We might not be responsible for a suitable sample selection, but
for area selection, preparation and measuring performance
we are!
 Please note: Data acquisition at high tilt angles can be tricky!
Area selection
Imaging and mapping at high tilt
 Tilt correction appears to be simple but practically it is extremely

challenging because of possible misinterpretations.
 Slight topography will be exaggerated artificially.
non-tilted 70° tilted tilt corrected
 Small (unknown) deviations from ideally flat surfaces distort the

corrected image in an unpredictable way.
 In case of topography high tilt prevents the scanning of hidden
surface areas.
Sample preparation

Significance of sample preparation
 Practically, sample preparation is the most essential factor for a

meaningful microstructure description…not only for EBSD.
During preparation a sample surface can be disastrously modified.
 Please note: You can have the best equipment and operators. If
your sample is improperly prepared, any measurement is
meaningless and conclusions are highly questionable.
 You can measure very accurate and precise, e.g. with EBSD, but if
the prepared sample surface does not reflect the characteristic
microstructure anymore, any experiment is insignificant.
 The opposite, an imperfect SEM, however, can be compensated

until a certain degree. You possibly need to measure with a lower
resolution, but still the object you really want analyse.
 The key question is:
How is it possible to recognize the true microstructure?
True microstructure
1. No additionally implemented deformation

Plastically deformed layer caused by preparation should be removed.
2. No scratches
Scratches normally indicate a surface that is not yet sufficiently
prepared.
3. No pull-outs
Especially in brittle materials.
4. No introduction of foreign elements

Abrasive grains can be embedded in the surface.
5. No smearing
The matrix or one of the phases might smear (flow).
6. No relief or rounding of edges

Relief can develop between different constituents of the surface,
caused by different hardness or other condition.

True microstructure
Requirements for reliable EBSD results
 The small information depth of EBSD (a few 10nm only) requires an

exceptional quality of surface preparation. (10nm are maximal 30 unit cells)
 Nobody knows, which preparation technique is suitable to deliver a defect-

poor surface! All mechanically prepared surfaces will have defects!
 Earlier used statements like: “If Kikuchi patterns are visible”

…or…”When we reach a high hit rate”…are definitely misleading!
 “Fortunately”: Remaining preparation artefact are hidden by the limited

accuracy and precision of the indexing procedures used in EBSD software.
 This means: The better the orientation precision, the higher the
requests on the surface preparation.
 For an orientation approximation, e.g. a texture interpretation, this error

is typically irrelevant.
 In contrast, for interpretation of misorientations it is essential to be sure

that the derived small misorientation is not the result of sample preparation.

Surface preparation for EBSD
Standard Typical workflow for the

materialographic Sampling Ni plating surface preparation
required for EBSD.
Sectioning
In simple terms:
hot Mounting cold A common standard
materialographic surface
Parallel preparation is followed
grinding by an EBSD specific
surface finishing in order
Grinding to remove all remaining
damages from former
Polishing steps.
Ion (Vibration) Electrolytic

polishing polishing polishing
(Coating)
EBSD specific
Some general preparation rules
1) Cutting: Use the gentlest possible cutting technique (cooling!).

Sectioning is a violent process and it can introduce massive damage if done
improperly.
2) Grinding:
a) First, make all of the specimens in the holder co-planar.
b) Gently remove the damages caused during sectioning.
c) Grind with fresh abrasive paper changing grit and direction.
3) Polishing:
a) Utilize flat, low-resilience woven cloths or pads that minimize relief
problems.
b) Keep the polishing surface uniformly coated with abrasive and
lubricant during polishing.
4) Cleaning: Clean and dry carefully without touching the surface.
With a bit experience you will see:

There is absolutely no mystery!

Machining and cutting
Transverse taper section of a surface of annealed 30% Zn brass

orthogonally machined by a planning tool with a -35° rake angle, the
depth of cut being 25µm.
SBL: shear-band layer, DL: deformed layer
 Typically samples are machined or cut

from some materials using destructive
techniques like sawing or cutting.
 Alternative techniques like spark
erosion or ion etching (FIB) change the
material at the surface by carburization
(surface roughness!) or ion
implementation (ion channeling!).
 Non-destructive techniques like wire
etching or water jet cutting are best
suited since they are assumed to
Samuels, L. E. damage the surface only marginally.
Metallographic Polishing by Mechanical
Methods. ASM International, 2003

Cutting
Some general rules
• Preparation faults introduced during sectioning a sample are

very difficult to remove.
• A gentle cutting lasts longer, does not modify the microstructure
and finally saves time during subsequent polishing.
• Common tools are precision saw (very thin blade), or wire saw
(takes longer time).
• In all cases ensure adequate cooling!
• Please note: The damage depth also depends on the material,
i.e. depends on chemical composition and crystal structure.
Depth of damage after band-saw cutting

of fcc, hcp and bcc materials.
P.T. Pinard et al. Microsc. Microanal. 15 (2009)
fcc (Cu) hcp (Ti) bcc (Fe) Suppl 2, 778-779

Cutting
Laboratory abrasive saw
• For abrasive cutting the damaged zone is clearly thinner.

The displayed profiles simply use the band contrast measured along the
cross section of cut surfaces.
abrasive saw
band-saw
P.T. Pinard et al. Microsc. Microanal. 15 (2009)

fcc (Cu) hcp (Ti) bcc (Fe) Suppl 2, 778-779

Embedding
Electrically conductive resin (hot mounting)
Advantages
 fast (for a single mount)
 reduces charging
 higher abrasion resistance
(reduces rounding effects along
the interface)
Struers
 reduced fissure formation
 Hot mounting provides parallel top
and bottom surfaces
(no out-of-plane distortions).
 Most hot mounting materials are
stable in vacuum.
 No out-gassing or vapor which
may cause contaminations.

Embedding
Electrically conductive resin (hot mounting)
Disadvantages
 Not transparent!
 Only limited specimen size.
 Possible contamination from
the filler.
 Fragile and brittle materials
Struers
cannot be hot mounted.
 For soft materials the abrasion
rate is possibly higher so that the
sample will not polished properly.
 In case of high temperature
embedding 180°C are required
(cold embedding: during polymerization
shortly 110°C are reached)

Grinding
• Grinding particles are at least 100-times bigger than the

information depth of EBSD. How big is the deformation zone?
• Band contrast analysis demonstrates: The damage depth is
approximately one tenth of the particle size.
Depth of damage
after grinding of Cu.
P.T. Pinard et al. Microsc.
Microanal. 15 (2009)
P80 ≈200µm P220 ≈70µm P1000≈18µm Suppl 2, 778-779
P80 ≈200µm
• In contrast, respective FIB images
suggest a misleading smaller depth, i.e.,
instead of 15…20µm only ≈5µm.
5µm
P.T. Pinard et al. Microsc. Microanal.
16 (2010) Suppl 2, 700-701

Mechanical polishing

Deformation during preparation
 The depth of a deformation zone

of a material is in general unknown!
Only a cleaved surface is perfect!
 Each preparation step removes
material but also implements new
surface damages.
 For standard metallography this is
often not essential because of a
Sketch of an ideal preparation procedure
subsequent etching which removes
removing step by step the (unknown) this layer, or because of the lower
inherent deformation, but mainly the newly
implemented damaging during polishing.
image resolution used in light
microscopy.
Piotrowski, T. & Accinno, D. J.
Metallography of the precious metals.
Metallography 10 (1977), 243-289  For EBSD any unrepresentative
damaging is significant, anyway if
still remaining or just implemented.

Polishing
Induced deformations Samuels, L. E.
Metallographic Polishing by Mechanical Methods
ASM International, 2003
During preparation different surface damaging can happen:

A. a loose, tumbling particle,
B. a fixed particle plowing a groove,
C. a fixed particle cutting a chip
All of them generate deformations around and below them which
are usually invisible in the surface image since smeared up by
removed material.
 After standard polishing always deformations exist.
Silica polishing
 As surface finishing a polishing with colloidal silica is preferred.

 Colloidal silica is a chemo-mechanical polish which combines
mechanical and chemical attacking. (topography!)
 Typical abrasive size is 0.05 micron.
 Please note: Not all silica is the same!
Different pH-levels and lubricants cause various etching behavior.
Warning:
 Colloidal silica crystallizes readily and will ruin polishing
cloths if left to dry. Clean them carefully!
 More problematic, a film can be formed on the polished surface.
 To prevent this, flush the polishing cloth with (hot) water during
the last few seconds of polishing.
 Remove and dry the sample using a solvent with low water
content. Alcohol is ideal. Do not use acetone!

Vibration polishing
 Designed to prepare high quality surfaces on a

wide variety of materials by an automated polishing
with colloidal silica.
 As pressure the own sample mass or small
additional weights are used.
 A horizontal vibratory motion of typically 7200
cycles per minute produces a very effective polishing
action.
 Often long-time polishing (several hours) is
reported.
 The vibratory action generates less deformation,
flatter surfaces and lower edge rounding.
 It also yields a stress-”free” surface without the
use of dangerous electrolytes associated with electro-
polishing.

Vibration polishing
An improvement of the band contrast of only ≈10…20% after 20

min vibration polishing may not look that much.
However, it tells us that the applied standard polishing was
definitely imperfect, and the EBSD maps suboptimal.

Some references
Standard metallographic preparation
Bauer, O. & Deiß, E.: Probenahme und Analyse von Eisen und Stahl, Verlag Julius
Springer, 1922
Berglund, T. & Meyer, A.: Handbuch der metallographischen Schleif-, Polier und
Ätzverfahren, Verlag Julius Springer, 1940
Miley, D. V.; Calabra, A. E.; McCall, J. L. & Mueller, W. M. (Eds.): Metallographic
Specimen Preparation: Optical and Electron Microscopy. Springer US, 1974
Elssner, G.; Hoven, H.; Kiessler, G. & Wellner, P.: Ceramics and Ceramic Composites:
Materialographic Preparation, Elsevier Science, 1999
Chinn, R. E.: Ceramography: Preparation and Analysis of Ceramic Microstructures, ASM
International, 2002, 35-44
Samuels, L. E.: Metallographic Polishing by Mechanical Methods
ASM International, 2003
Vander Voort, G. F. (Ed.): Metallography and Microstructures, ASM International, 2004,
volume 9
Geels, K.; Fowler, D. B.; Kopp, W.-U. & Rückert, M.: Metallographic and
Materialographic Specimen Preparation, Light Microscopy, Image Analysis and
Hardness Testing, ASTM International, 2007
Echlin, P.: Handbook of Sample Preparation for Scanning Electron Microscopy and X-
Ray Microanalysis. Springer Science+Business Media, 2009

Cleaning of samples
• Any contamination during or after sample preparation disturbs.

• Frequently, ultrasound baths are used in order to remove or
reduce dust particles or lose dirt on sample surfaces.
They are also used by some people after each preparation step
in order to prevent any contamination for the following step.
• If strong contaminations appear during imaging in SEM try distilled
or de-ionized water.
It is said that the latter prevents carbon contamination during
scanning in SEM.
• In case of cracks, holes, pores etc. use a heating stage at
moderate temperatures to remove hidden water.
Otherwise, in SEM from each cavity the remaining water flows out
and contaminates the surface again.

Cleaning of samples
• Sometimes, a sample surface is contaminated by dirt which is not

removable by a gentle air flow or ultrasound bath, e.g. crystallized
silica.
• A possible solution can be acetate tape (Formvar) which is
commonly used for replica in TEM.
• Cover your sample surface with acetone, put a thicker
acetate foil on the wet surface and wait until it is dry (this lasts
a few minutes only).
• Strip the tape carefully.
• All loose dust and many silica particles are now fixed in the
tape, and the surface can be investigated without repolishing the
sample.

Omnipresent charging
A few tricks
 Minimize surface topography!

 Coat with gold before the final polishing step.
This fills the cracks and voids with a conducting network.
 Prepare a conductive tract from the sample to the stub/holder –
using some silver paint or metallic tape.
 Scan the surface for 30min or longer at low magnification.
 If possible, leave the sample over night in the SEM.
 Work in variable pressure / low vacuum mode (if you have).
Often a chamber pressure of 5-20 Pa is sufficient.
A higher pressure decreases resolution as well as the pattern quality.
 More efficient: Gas injection systems.
They blow gas molecules directly in the electron beam.
 Use higher acquisition speed (needs fast & sensitive detectors).
The beam has a minimal dwell time.
 Work at lower probe current and/or vary the accelerating
voltages.
Sample transport
• Best procedure is to go after sample preparation directly into the

SEM.
• If this is impossible, use Joseph paper (thin, soft and lint-free
tissue paper) to protect the surface.
It also helps against accidental touches.
• Before mounting in the SEM, always clean the surface by a gentle
air flow.
• Do not use any air brushes since the used
air often contains oil which contaminates
your sample surface ever more!

Demagnetisation
• EBSD measurements are based on the interaction of electrons with

a sample.
• The electron beam in SEMs is controlled by electric or magnetic
fields.
• This means: If the sample or the detector charges, the electron
beam path is influenced by the respective fields. Quartz pattern
• Sometimes, however, samples or only single phases
can be magnetic as well.
• Magnetism disturbs if patterns are impossible to index
since their bands are no more straight.
• Therefore, before investigating it is recommend to
demagnetize the sample.
• For really strong magnets this option does not exist.

How to prepare unknown samples for
EBSD?
Grinding and polishing vary for different
materials, production and loading conditions…

Struers: standard preparation
The Metalogram displays materials according to specific

physical properties: hardness and ductility.
Hardness (Vickers):
The easiest attribute to measure but is not
sufficient information about a material to find
the correct preparation method.
Ductility:
The ability of a material to deform plastically
is important for grinding and polishing.
This property expresses how the material
responds to mechanical abrasion.
A MgAl-alloy, cast Procedure:

B Cu (pure)
C CuZn alloy, cast
1. Find the hardness on the X-axis.
D Grey cast iron fast procedures 2. Estimate ductility according to any
E Ball/Bearing steel 100 Cr6 X AlSi alloy previous experience.
F WC/Co sintered carbide Y Tool steel
Ductility is no precise number!
G Ceramic Si3N4 Z Carbides in
metallic matrix The condition is to have an idea of how a
https://e-shop.struers.com/BG/EN/methods/ ductile or brittle material will perform.

Struers: standard recipes
https://www.struers.com/en/Knowledge/Grinding-and-polishing#grinding-polishing-how-to
A: MgAl alloy B: Cu C: medium C-steel D: low C-steel
E: white cast Fe F: WC/Co sintered G: ZrO2
X: AlSi alloy Y: tool steel Z: carbides in metal

Struers: Special EBSD preparation
For EBSD, however, additional

preparation step(s) are required
which remove the remaining or
during the last polishing step
introduced deformation layer.
For ferrous materials a special
application note is available:
https://www.struers.com/-/media/Library/
Brochures/English/Application-Note-EBSD.pdf

Buehler: standard preparation
 About 150 pages of fundamentals

and recipes (free available)
 for EBSD only some basics (p.
23-25) referring to vibration and
electrolytic polishing.

George Vander Voort
Rules for Pain-Free Preparation!
http://www.georgevandervoort.com/metallography/general/ebsd/
20001256-mechanical-specimen-preparation-for-ebsd-struers.html
Automated polishing
Vander Voort, G. F. Metallographic specimen preparation for Electron Backscattered Diffraction: Part I
Prakt. Metallogr., 2011, 48, 454-473
This generic mechanical preparation process is suitable for many

metals and alloys.
For tough materials like Ti the 3µm diamond polishing should be
omitted.
41
Manual preparation
In BAM we always start with a 4-step manual preparation.

It practically works for ca. 90% of all materials (metals, minerals,
ceramics…).
The rotation speed during grinding and polishing is constant.

The applied force is a matter of feeling (personal experience).

42
Special recipes
For pure Zr:
25€ /l 28€ /l

Alternatives
Electrolytic polishing

 Widely used technique because of

excellent results
 contact-free preparation
 Works for non-planar surfaces
 Factors controlling etching /
polishing behavior are:
‒ Electrolyte composition
‒ Electrolyte temperature
‒ Electrolyte stirring
‒ Area to be polished/etched
Oxford Instr.
(current density)
‒ Voltage

Oxford Instr.

Advantages: Disadvantages:
 Polishing & etching are  Conductive specimens only
possible
 Not all alloys can be polished
 Fast preparation process,
 Preferential attack or pitting
i.e. easily repeatable if
can occur (no flat surface)
required
 No edge retention
 Reproducible when the
process is automated  Limited polishing area
 No mechanical deformation  Limited scratch/material
removal
 Can produce excellent
surfaces for EBSD  Hazardous electrolytes
 Temperature control

Chemical etching
 Commonly easy to handle and fast.

 Additionally, etching delineates the grain structure but may
attack grain boundaries excessively.
 Etching may attack different phases preferentially.
 Materials that are difficult to polish may benefit from repeated
etching and re-polishing.
 Using special acid or alkali resistant cloths, it is also possible to
dilute etchants to the polishing cloth during polishing. (effective
but difficult to control)
 Any etchant used has to dissolve the specimen surface in an even
manner without formation of any oxide or reaction product
layers.

Alternatives
Ion polishing

Broad Ion Beam (BIB) polishing (milling)
Principle
HITACHI
 Non-focused ions are used to bombard and erode the surface.

 Sample rotation required to generate flat surfaces.
 It can also cause damages by ion implantation which can lead to
an amorphous layer or phase transformation.
 Reactive gases (in vacuum) increases the milling rate.
 A specimen mask enables cross sections (curtaining!)
Ion implementation
BIB polishing (Ar) at Si
Electron beam voltage for EBSD

5 kV 10 kV 15 kV 20 kV
Final ion polish voltage
5 kV
3 kV
2 kV
courtesy of Dr. Joe Michael at Sandia National Lab, Albuquerque, USA

BIB polishing (10kV, Ar) at Cu
Also here for each material parameters have to be optimized.

 For copper 10 min polishing of 10kV Ar under an angle of 8° (or 82°
compared to EBSD) would give best results.
 However, lower kV will likely result in higher image qualities (IQ).
Dankházi, Z.; Kalácska, S.; Baris, A.; Varga, G.; Radi, Z. & Havancsák, K.
EBSD Sample Preparation: High Energy Ar Ion Milling
Materials Science Forum, 2015, 812, 309-314

BIB polishing (milling)
 Also ion beam milling is no solution for

everything!
 Very useful for all materials where any
mechanical handling generates artefacts.
 Target preparation using specimen mask.
 The optimization of parameters
is time-consuming.
Possible drawbacks:
‒ anisotropy of milling (topography)
‒ curtaining, if sample cannot be
rotated
‒ possible phase transformation
‒ point defects (ion implantation)
‒ comparatively slow
BIB polishing
Sample cooling
Hitachi
During interaction with ions the sample heats up and the
microstructure may change considerably:
phase transformation, evaporation or sublimation.
In order to prevent this, samples need to be cooled.
Focused ion beam (FIB) preparation
Phase transformation
A special thermo-mechanical treatment produces

causes a transformation from bcc to fcc. The
lathes are nicely visible already in the SE image
of the FIB cut.
The EBSD scan shows nicely as well the phase
boundaries and the orientation differences.
Surprisingly the software identify all fcc-grain
close to the surface as bcc phase!
EBSD related preparation literature
Katrakova, D. & Mücklich, F.: Specimen Preparation for EBSD - Part I: Metals.
Prakt. Metallogr., 2001, 38, 547-562
Katrakova, D. & Mücklich, F.: Specimen Preparation for EBSD - Part II: Ceramics. Prakt. Metallogr.,
2002, 39, 644-662
Wynick, G. & Boehlert, C.: Use of electropolishing for enhanced metallic specimen preparation for
electron backscatter diffraction analysis. Mater.Charact., 2005, 55, 190-202
Vander Voort, G.; van Geertruyden, W.; Dillon, S. & Manilova, E.: Specimen Preparation for Electron
Backscattered Diffraction. Microsc. Microanal., 2006, 12p, 1610
Schwarzer, R.: The preparation of Mg, Cd and Zn samples for crystal orientation mapping with BKD in
an SEM. Microscopy Today, 2007, 15, 40-42
Vander Voort, G. F.: Metallographic specimen preparation for Electron Backscattered Diffraction. La
Metall. Ital., 2009, 11-12, 71-79
Vander Voort, G. F.: Metallographic specimen preparation for Electron Backscattered Diffraction: Part I.
Prakt. Metallogr., 2011, 48, 454-473
Vander Voort, G. F.: Metallographic specimen preparation for Electron Backscattered Diffraction: Part II.
Prakt. Metallogr., 2011, 48, 527-543
Koll, L.; Tsipouridis, P. & Werner, E. A.: Preparation of metallic samples for electron backscatter
diffraction and its influence on measured misorientation. J. Microsc., 2011, 243, 206-219
Halfpenny, A.; Hough, R. M. & Verrall, M.: Preparation of Samples with Both Hard and Soft Phases for
Electron Backscatter Diffraction: Examples from Gold Mineralization. Microsc. Microanal., 2013, 19,
1007-1018
Brodusch, N.; Demers, H. & Gauvin, R.: Field Emission Scanning Electron Microscopy: New Perspectives
for Materials Characterization, Chapter 10, Springer Singapore, 2018

EBSD related preparation literature
Please note:
Literature often only describes
how to get Kikuchi patterns, but not,
how to get the patterns you need!

Sample preparation
Final recommendations
 Conventional metallographic preparation is suitable followed by

a polishing with colloidal silica (about 20min).
 Different colloidal silica based polishing agents have different
behaviour. You should test them!
 For conductive materials electro polishing is an excellent option
although for different metals different etchants are required.
Often, for safety reasons, it is no more permitted.
 Spend the time you really need!
For texture investigations the preparation does not have to be
perfect as long as no artefacts will be introduced.
 For misorientation measurements – e.g. GND interpretations –
preparation artefacts have to be minimized!
 The standard orientation determination is not very precise.
On the other hand, the best preparation is for nothing if artefacts
cannot be discriminated by the used orientation determination.
Sample preparation
Final recommendations
 For multiphase materials, sample preparation is always a

compromise since the containing phases react differently.
 At multiphase materials topography can be only rarely prevented.
 For “difficult” multiphase materials ion etching at low energy is
an option since no new scratches will be generated.
However, it also has drawbacks, like increasing topography.
 For composites combining very soft and hard phases, commonly
ion etching under gracing incident is the only option.
Again: Any sample preparation is an intervention with unknown

external interference on the microstructure.
It is not sufficient if Kikuchi patterns can be indexed

with satisfying hit rate !
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SAMPLING, PREPARATION AND AREA SELECTION

Presentation · May 2018

Investigation of hydrogen-induced degradation of austenitic stainless steel View project

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SAMPLING, PREPARATION AND AREA

Gert Nolze, BAM Berlin

The basic problem for a metallographer preparing a specimen is that the

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You will get what you collect!

 Nevertheless, try to get as many information as possible about

 Ask for the amount of specimen to be compared since this

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 Sampling describes the extraction

 For water, soil, air, blood and

 In contrast to e.g. XRD, for EBSD a

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 A sample is selected to enable reliable findings and conclusions in

 The aim of a sample but also of a scanned area by EBSD is a

 Any possible variation/change/modification of the sample

 Possible interferences have to be discussed critically, e.g. any

The selected map is used to represent the entire material.

 Define position and size of the orientation map with respect

 If the area of interest is contaminated (e.g. by dust) or shows

 For publication or representation do not use the nicest but

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You will get what you select!

 Tilt correction appears to be simple but practically it is extremely

 Small (unknown) deviations from ideally flat surfaces distort the

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 Practically, sample preparation is the most essential factor for a

 The opposite, an imperfect SEM, however, can be compensated

1. No additionally implemented deformation

4. No introduction of foreign elements

6. No relief or rounding of edges

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 The small information depth of EBSD (a few 10nm only) requires an

 Nobody knows, which preparation technique is suitable to deliver a defect-

 Earlier used statements like: “If Kikuchi patterns are visible”

 “Fortunately”: Remaining preparation artefact are hidden by the limited

 For an orientation approximation, e.g. a texture interpretation, this error

 In contrast, for interpretation of misorientations it is essential to be sure

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Standard Typical workflow for the

Ion (Vibration) Electrolytic

1) Cutting: Use the gentlest possible cutting technique (cooling!).

With a bit experience you will see:

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Transverse taper section of a surface of annealed 30% Zn brass

 Typically samples are machined or cut

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• Preparation faults introduced during sectioning a sample are

Depth of damage after band-saw cutting

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• For abrasive cutting the damaged zone is clearly thinner.

P.T. Pinard et al. Microsc. Microanal. 15 (2009)

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• Grinding particles are at least 100-times bigger than the

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 The depth of a deformation zone