Evolution of EBSD Patterns

during Sample Preparation

H Jiang and H S Ubhi
Successful EBSD work for characterizing and quantifying microstructures requires good metallographic preparation procedures. This study is an attempt
to illustrate how EBSD patterns evolve through the various metallographic preparation steps using duplex steel and alumina samples as examples.

Methodology
Several specimens about 3 x 4mm were cut from the duplex steel
and alumina sheet samples, and mounted in conductive bakelite. In
order to observe the affects of intrinsic deformation one surface of the
steel sample was shot peened. Samples were prepared using standard
metallographic procedures.
After each stage of grinding or polishing steps given in the Table 1, the
specimens were examined in a FEGSEM and typical images plus EBSD
patterns were recorded. No attempt was made to either optimise any
of the polishing variables like load, rotation, time, or follow any specific
route prescribed by suppliers of metallographic consumables. In the case
of the duplex steel after each mechanical polishing step, the specimens
were further electro-polished. Electro-polishing was carried out using a
mixture of 5% perchloric acid and 95% acetic acid at a voltage of 40V, a
temperature of 5C and about 10s duration in an eletro-lytic cell.

As received
Indexable
EBSPs

Material

Polishing
Surface

Abrasive
Lubricant
Grit size

Rotation
Speed (rpm)

Force
(N)

Time
(min)

Steel

SiC

500

water

300

20

Steel

SiC

800

water

300

20

Steel/Alumina

Grinding disc

Diamond 9m

water

150

20

Steel/Alumina

Satin woven Cloth

Diamond 6m

Alcohol based

150

20

Steel/Alumina

Satin woven Cloth

Diamond 3m

Alcohol based

150

20

Steel/Alumina

Syn. Short Nap cloth

Diamond 1m

Alcohol based

150

15

Steel/Alumina

Porous neoprene cloth

Colloidal Silica

150

15

30

Steel/Alumina

Porous neoprene cloth

Colloidal Silica

Vibratory

Table 1: Details various mechanical polishing steps.

Results and Discussion

Figure 1 shows a series of typical back-scattered , fore-scattered electron
images and EBSD patterns the preparing the alumina sample. An
IPF coloured EBSD map for the final step is also shown. Good quality
patterns are possible from the un-prepared surface, however, for
satisfactory EBSD characterization a flat surface is preferable. Satisfactory
patterns result after final colloidal silica or vibratory polishing steps.
Ceramics being insulators cannot be electro-polished.
Results for the duplex steel for the mechanical and electro-polishing
steps respectively in terms of back scattered electron images, typical
EBSD patterns from the ferritic and austenitic phases and raw phase and
local mis-orientation maps plus a average mis-orientation vs distance
plot in Figure 2. It is clear from these data that weak EBSD patterns are
observed from the ferrite phase after 9m diamond polishing, whereas
austenitic phase starts to produce patterns after the 3m polishing step.
EBSD phase maps from the 3m step clearly show that only the ferrite

9 m diamond
Un-indexable
EBSPs

6 m diamond
Just
indexable
EBSPs

phase is indexedable. After the 3m step both phases can be indexed,

with improved hit rate, although the fraction of the austenite is very low
and the local mis-orientation due to surface deformation are still large.
The best patterns were obtained for both phases after a final colloidal
silica or vibratory polish. EBSD maps from this step give a much truer
picture of the microstructure, due to the removal of surface deformation
which leads to high indexing rates. In addition local mis-orientation is
now observed to be higher in the regions that have been subject to
shot peening Electro-polishing results in excellent quality patterns in
both phases after the final colloidal silica polishing step. No amount of
mechanical or electrolytic polishing can produce sharp patterns from the
intrinsically deformed surface introduced by shot peening, the effects of
which become visible after 3m diamond polishing and persists up to the
electrolytic step. The effect of surface shot peening is clearly shown in
EBSD maps as well as the average mis-orientations versus distance plot.

Electro-polish
ferrite

3 m diamond

austenite

Just
indexable
EBSPs

1 m diamond

ferrite

austenite

ferrite

austenite

Indexable
EBSPs

800 grit SiC

ferrite and austenite

easily indexable

Poor quality
un-indexable patterns

Electro-polish

9 m diamond
Poor quality
un-indexable patterns

ferrite and austenite

easily indexable

6 m diamond

ferrite and austenite

easily indexable

Colloidal Sillica

120

Poor quality
un-indexable patterns

Easily
indexable
EBSPs
Electro-polish
phase map blue=ferrite red= austenite

Vibratory Colloidal Silica

EBSD phase map

3 m diamond

Local misorientation map

bcc just
indexable

ferrite

austenite

ferrite and
austenite just
indexable

ferrite

austenite

ferrite and
austenite easily
indexable

ferrite

austenite

EBSD IPF map

Easily
indexable
EBSPs

20m

BSE image at 0 tilt

1 m diamond

Local misorientation map

FSD images

Typical EBSPs

Figure 1. Series of BEI, FSD and EBSD images at various

steps of polishing for Alumina

Electro-polish

Conclusions
This study clearly shows that evolution of EBSD patterns is dependent
not only on surface polishing but also on the phases and deformation
present in the specimens for visualization of microstructures using
the EBSD technique. Standard metallographic polishing followed by
final colloidal silica polish results in strain free surfaces suitable for
EBSD. Where electro-polishing is possible satisfactory patterns can be
obtained after any stage during mechanical grinding or polishing.

Colloidal Silica

ferrite and austenite

easily indexable
Vibratory
ferrite

austenite
20m

Figure 2. Series of back-scattered images, from the Duplex stainless steel both
mechanically and electro-lytically polished, typical EBSD patterns EBSD phase maps
and local orientation maps and a mis-orientation vs distance plot.

www.oxford-instruments.com
Acknowledgements Dr J R Saithala, Fine Tubes Ltd, Plymouth, UK, for providing the duplex steel sheet, Mr Graham Hammersley, Metal

Improvement Co., Derby, UK for shot peening the duplex steel and Dr P Holdway, QinetiQ plc, Farnborough, UK, for providing the alumina samples.

ferrite and
austenite easily
indexable

ferrite

austenite