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Ebsd Oim

This document provides an overview of electron backscatter diffraction (EBSD) techniques. EBSD can determine the orientation of crystalline materials by indexing electron backscatter patterns. It allows identifying phases, measuring grain size and textures. EBSD is well-suited for nanomaterials and requires little sample preparation. Examples shown include using EBSD to characterize deformation in rocks, measure grain size in cemented carbides, and determine the 3D grain structure in gold wire.

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thuron
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185 views54 pages

Ebsd Oim

This document provides an overview of electron backscatter diffraction (EBSD) techniques. EBSD can determine the orientation of crystalline materials by indexing electron backscatter patterns. It allows identifying phases, measuring grain size and textures. EBSD is well-suited for nanomaterials and requires little sample preparation. Examples shown include using EBSD to characterize deformation in rocks, measure grain size in cemented carbides, and determine the 3D grain structure in gold wire.

Uploaded by

thuron
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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Imaging and Analysis

Techniques in Materials
Science II
Pat Trimby
LINK Nordiska

Talk 2 Outline
EBSD Overview
What is EBSD?
EBSD Phase ID
What EBSD tells us
EBSD Performance
Sample Preparation

3 EBSD Application Examples

What is EBSD?
EBSD Electron Backscatter Diffraction
Other names:

EBSP Electron Backscatter (Diffraction) Pattern


BKD Backscatter Kikuchi Diffraction
OIM - Orientation Imaging Microscopy
OM Orientation Mapping
COM Crystal Orientation Mapping

EBSD is:
a Scanning Electron Microscope (SEM)
based technique
a surface analysis technique
a technique that can be used to analyse
any crystalline material (e.g. metals, rocks,
ceramics...)

EBSD Set-up

Diffraction Pattern Generation

Electrons are inelastically scattered in all directions from a source point


close to the sample surface (top 20nm)
Electrons that satisfy the Bragg diffraction condition (n=2dsin) for a
particular lattice plane are channelled differently to the other electrons - thus
producing a change in intensity
For each crystallographic plane, these electrons form two cones (with large
semi-apical angles of [90- Bragg angle], i.e. almost flat discs)

Real EBSP (Fe-BCC)

Software derives the


orientation of the
crystal lattice

The EBSD Cycle

Automated EBSD

EBSD analysis on a grid of points, from


which the complete microstructure can
be reconstructed.

A typical "orientation map" from an automated


EBSD analysis (150,000 measurements) of a
steel sample

EBSD Phase Identification


A relatively recent approach combining EDS and
EBSD
Used for identifying unknown phases in a
sample (note that this is not "phase
discrimination" distinguishing between several
known phases in a sample such as ferrite and
austenite in duplex steel)
Phase ID involves a modified EBSD Cycle

The Phase ID Cycle


Mo + C

1. Position Beam
2b. Collect EDS Spectrum +
identify peaks

3b. Search database(s) for


matching phases
Mo2C - Space Group 60, orthorhombic
Mo2C - Space Group 194, hexagonal
Mo2C - Space Group 187, hexagonal
Mo2C - Space Group 162, trigonal
Mo2C - Space Group 29, orthorhombic

2a. Snap EBSP

4. Index EBSP
3a. Detect Bands

Mo2C Hexagonal
(SG 194)
5. Save result

What can EBSD tell us?


EBSD provides 3 main types of information:
The absolute 3D orientation of the crystal lattice
Discrimination between phases based on their
crystallographic differences (e.g. austenite (FCC)
and ferrite (BCC) in steel; (HCP) and (BCC)
Titanium)
Identification of unknown phases (Phase ID) when
used in conjunction with EDS

EBSD cannot:
analyse non-crystalline (amorphous) materials,
such as glass, plastics, wood etc.
provide information about the crystal orientations
within the volume of a sample it is purely a
surface technique
analyse samples with poor surface preparation
or thick coats (e.g >10nm thick)
Discriminate between phases with similar
crystallography without EDS info (e.g. Fe-FCC
and Al)

Typical Measurements with EBSD

Phase distribution
Phase identification
Texture strength ("Texture" = degree and nature of
alignment of the crystal lattices in a sample,
sometimes called LPO or CPO in geology)
Grain size
Boundary properties (e.g. twin boundary frequency)
Misorientation data (difference in orientation between
different points in the sample)
Recrystallised / deformed fraction (proportion of the
sample that has been recrystallised and deformed)
Intra-granular deformation
Plus much, much more

EBSD Performance
Critical Parameters:
Spatial resolution - <20nm (in a FEG SEM)
Angular resolution - <0.5
Indexing speed - >50 pts/sec

These make EBSD an ideal technique for


analysing thin films, nanomaterials and ultra-fine
grained metals and alloys linking texture, grain
size and boundary properties with good statistics

Sample preparation for EBSD


Very important, as diffraction pattern signal originates
in top 5-20nm
Needs damage-free crystal lattice
Mechanical polish alone is insufficient needs a final
stage to remove the mechanically damaged layer
High tilt angle necessitates very flat surface (otherwise
shadowing...)
Standard carbon coating is too thick for EBSD
BUT some samples need no preparation (e.g. thin
films)

EBSD Application Fields


In general there are 3 main application areas:
3. Materials sciences
4. Microelectronics
5. Earth and planetary sciences

Application Examples
1. Deformation styles in a polyphase rock
sample
2. Grain size analyses in cemented Tungsten
Carbide (WC) tools
3. 3D grain analyses in Au wire

Deformation styles in a deformed


rock sample
Key Question: Can we determine the down-temperature
deformation styles using EBSD?
"Gabbros" from the mid ocean ridge in the Indian Ocean
show many complex deformation zones
Different deformation zones contain different phases,
and show contrasting styles of deformation
Evidence exists for deformation from very high
temperatures (>900 C) to low temperatures (<300 C)
EBSD is the ideal technique to look at the development
of lattice preferred orientations (LPOs - texture) in a wide
range of minerals

Step 1 identifying unknown phases

Phase ID
using
EDS-EBSD

Step 2a EDS Mapping

Fe counts

Step 2b EBSD Mapping and Phase Discrimination


Chalcopyrite

Augite

CuFeS2

(Ca(Mg,Fe)Si2O6

Ilmenite

Enstatite
(Mg,Fe)SiO3

Hornblende

FeTiO3

Plagioclase

Step 4 Orientation analysis

Note plagioclase
twinning

Large scale transect across different deformation zones

Transect width 6.6mm


Very coarse grained, magmatic
plagioclase weak deformation
twinning

XPL
Photomicrograph
of plagioclase
zone note
annealed
microstructure

Development of very strong alignment of


plagioclase <100> axes with the shear
direction possibly due to the High T slip
system (001)[100]

Central, mylonitic shear zone

Enstatite
Weak or non-existent LPO in
mylonite zone

Plagioclase
Weaker alignment of plagioclase
<100> axes than in plag zones
outside mylonite

Hornblende
Strong alignment of hornblende
(100) planes with the shear plane

Chemical variations
Fe counts

Ca counts

Simultaneous EDS analyses show how the


central shear zone has a high
concentration in some elements (e.g. Fe)
but low concentration in others (e.g. Ca)

Gabbro Preferred Orientations Conclusions


EBSD and EDS have been used to characterise the
phases, chemistry and lattice preferred orientation in a
polyphase gabbro shear zone
The plagioclase zones have developed a strong <100>
LPO, indicative of high T deformation (>800 degrees C)
in dislocation creep field
The finer grained mylonite zone has a weaker
plagioclase LPO, no enstatite LPO but a strong
hornblende LPO; this indicates continued deformation by
dilocation creep localised on the hornblende phase down
to lower T "amphibolite facies" conditions (<600 deg C)
Simultaneous chemical mapping by EDS highlights the
chemical variations associated with the deformation
zones

Microstructure enhancement in
cemented carbides ("hardmetals")
Facts and Figures, 2004

38,000 tons of hardmetal were


produced world-wide
~ 15,000 of that had sub-micron
grainsize (~40% of total)
~ 2,000 tons for PCB tools <=>
>500,000,000 tools
70 m diameter carbide microdrill
Acknowledgement: Data and images courtesy of Mattias
Elfwing, Sandvik Tooling

Background

Most coated carbide drills used today are 10%Co - 0.8 m WC


type
Further grain size decreases would improve the hardness and the
attrition wear resistance
Part of the problem is the densification of the ultra-fine starting
powders without significant grain growth
EBSD combines the statistics, spatial resolution and phase
recognition necessary for accurate quantification of the resultant
hardmetal microstructures
Additional benefits of EBSD are the characterisation of the grain
and twin boundaries and the capability to analyse the surface
coating

Here we look at one dataset to show how


EBSD can accurately measure the key
parameters

EBSP Pattern Quality Map

711 x 589 grid


418,779 pts
Stepsize: 30nm
Note: this is a small
subset of a larger
dataset

Phase Map

WC blue
Co (cubic) red
Co (hex) - yellow

Orientation Map

Note: There is no
strong texture in
the WC in this
sample

Grain size map (WC)

Focusing on abnormally large grains

Sigma 2 boundaries 90 rotation about <10-10>

Sigma 2 Boundary Map

Sigma 2 boundaries in red

Grain size distribution excluding twins

Mean ECD = 0.466 m


N = 1428
Mean ECD = 0.335 m
N = 2663

If twins are
included

PVD coating
The surface coating on
cemented carbides can
also be analysed using
EBSD to determine the
phase distribution,
grain size and texture

WC

TiC /
Ti(C,N)

Al2O3

Cemented Carbide Conclusions


Accurate measurement of grain size and phase
distribution is necessary to assess the physical
properties of ultrafine grained WC hardmetals
The EBSD technique (using a FEG SEM) is ideal for
standard characterisation as it provides, with the
necessary resolution and good statistics:
phase distribution
grain size distribution
grain and twin boundary measurement

EBSD data can be used to push this important


materials technology to the next level: 0.1-0.2 m
grain size

3D Grain Analysis in Au-wire


Understanding the 3D grain and boundary
structures in Au wire is essential for its use in
electronic applications
EBSD in conjunction with a FIB-SEM is used
to measure the 3D grain structure
The combination of automated serial
sectioning in a FIB-SEM with EBSD mapping
is a new development in the last 1-2 years

FIB sectioning Au-wire ideal preparation

ion-channelling
contrast

EBSD analysis of wire section is very


straightforward...
Orientation map
showing the
crystallographic
alignment relative
to the wires axis.
This shows that the
abnormally large
grains have a
<100> fibre texture,
compared with the
standard <111>
fibre texture

Approx 60,000 data points


collected in 30 minutes

Experimental Details
Automated FIB-SEM and EBSD is used here to
analyse 34 slices (spacing 100nm) through part of a
25m Au wire
Each slice is analysed with EBSD, using a grid of
238x232, with a step of 50nm: total data approx.
1.8million analyses
Total volume material analysed: approx 450 m3
Total (unattended) acquisition time 40 hours
Data courtesy of Dr. Ali Gholinia (HKL Technology)
Sample courtesy of Dr. Jan Shischka (FIW Halle)

SE image of the Au wire, prior to analysis

Reconstructed 3D EBSP quality map

Reconstructed 3D orientation map

Reconstructed 3D orientation map axial direction,


showing elongate grain shapes

Reconstructed 3D texture map red grains have


an orientation within 25 of a <111> fibre texture

Movie, showing individual slices (looking down axial direction)

Individual grain highlight, with best-fit ellipse overlay

Individual grain highlight, showing a characteristic


pencil-shaped grain

Conclusions - 3D Analysis of Au wire


Au wire successfully analysed using automated
3D EBSD
2 different grain types round grains and
elongate grains
Elongate grains typically have a strong <111>
fibre texture
A detailed comparison of grain sizes, shapes
and orientations is possible, allowing proper
understanding of the wire's electrical properties
This 3D technique has many potential
applications:
Boundary analyses (e.g. twin boundary plane orientations
in 3D)
Particle shape analyses
Strain around particles
Crack tip morphology in 3D

Overall Conclusions
EBSD is a powerful SEM technique for the
analysis of fine grained, complex
microstructures
EBSD and EDS are commonly integrated to
enable phase identification and simultaneous
crystallographic and chemical mapping
There are many different applications of
EBSD, 3 of which are provided here

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