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The Business of Science

Oxford Instruments
Recent Developments in EBSD
Jenny Goulden

Oxford Instruments 2015

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Agenda

Product Updates:
10:15-10:45 EBSD developments :
Hardware, basic Aztec, ease of use, indexing, mapping,
Synergy
10:50-11.30 Advanced functions:
Large area mapping, refined accuracy, updates to
post processing

More application specific talks later

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Introduction
Developments driven by market / application requirements
What are the challenges
Which solutions work / dont work
How can we help?
Market requirements
Improved spatial resolution EBSD (lower kV & beam current)
Faster data acquisition (reduce SEM time, more data, better
statistics)
Improvements to data acquisition
Improvements to EDS integration
Easier to acquire better quality data

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Introduction
Result number of development
Detector developments
Improve sensitivity
Improve speed
AZtec platform launched 2011
Updates about every 6 months
Brief overview of product
Key features and functions

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EBSD Hardware Developments


NordlysNano
Better sensitivity
Improved spatial resolution
NordlysMax2
Faster acquisition speed
Retain sensitivity
Forescattered Detectors
Better orientation imaging
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Detector Developments - NordlysNano


EBSD detector with HIGHER sensitivity
Designed to for the requirements of nano scale
applications
Developed in direct response to customer requests
To work at low kV
To work at low beam current
Best spatial resolution
Highest quality patterns (high pixel count)

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Higher Spatial Resolution

20kV Iron Pyrite

5kV Iron Pyrite

The challenge for improving spatial resolution is operation at


low kV
Low signal
Weaker patterns especially at edges
Broader Bands
Requires optimisation the signal to the sensor
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NorldysNano
Delivers the best possible sensitivity while accurately imaging
the EBSP
60% more sensitive than older EBSD detectors

Sensitivity is directly related to quantum efficiency of the CCD


coupled with the detector optics
NordlysNano has 70% Quantum efficiency
Coupled with bespoke optics specifically optimised to
work with our CCD
Eliminates distortion from the pattern (zero barrel distortion)
Barrel distortion present in all optics
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Barrel Distortion Removal:


Old lens ~2% distortion

New lens <0.5% distortion

Best pattern quality: important in applications looking at pattern


detail or subtle differences in EBSPs
For example cross correlation techniques
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NordlysNano
Capability to work at lower beam energies, important for:
Nano materials where low kV offers better spatial
resolution
Beam sensitive samples, where higher beam energies
damage the samples
Insulators, where lower kV can remove the need to coat
the sample
Excellent for TKD

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NordlysNano
5kV Ni 0.5um grain size 100Hz

Aluminia Insulator

10kV

Alumina NO coating
Hit Rate 85% (porous sample) at
90Hz
5kV
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NordlysNano
Transmission Kikuchi Diffraction
Cu15B-strained-4nm-IPF-Z
This is a strained nanocrystalline copper
IPF-Z direction, high angle boundaries in black and CSL
boundaries in colour.
Step size 4nm.

Acknowledgement: Saritha
Samudrala (University of Sydney)
and Kevin Hemker (Johns Hopkins
University)
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Sensitivity vs High Resolution


Target to deliver both high sensitivity and high resolution
NordlysNano matches customised optics and CCD
Without this optical design full resolution of megapixel CCDs
cannot be achieved
High resolution images not simply a matter of more
pixels in the pattern
Important in applications looking at pattern detail or subtle
differences in EBSPs
e.g Cross correlation techniques
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Faster Data Acquisition


SEM time becoming more valuable / expensive
Challenged with more efficient use of SEM time
Collect more data / better statistics
Traditionally with EBSD faster data collection has required higher
beam current up to maximum speed
Challenge was to develop hardware which could operate:
Faster maximum speed
Fast acquisition at lower beam energy
Operate at lower kV and beam current

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Nordlys Max2 Detector


30% faster, with better sensitivity
Fastest speed 870Hz (or patterns per second)
870Hz at 5nA - acquire and solve in real time
870Hz with simultaneous EDS data - acquire and solve
Operation at 5kV
Operation at lower beam current (100pA)
Achieved by improving CCD

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NordlysMax2
Phase Map

870Hz
99% indexed
12nA

Ni sample

Ni X-ray Map

100um

W X-ray Map

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Simultaneous EBSD &


EDS
Tungsten heavy alloy
870pps
Real time sample
characterisation
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NordlysMax2 Low kV EBSD Patterns


20kV

Patterns from tungsten


20kV
5kV
But still able to solve
5kV
5kV

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EBSD Dynamic Studies


In-situ experiments are performed in the SEM chamber
Monitor change while experimenting on the sample
Typically heating and/or tensile testing
Specialised stages are used in conjunction with EBSD
Increasingly used to study and understand solid state events:
Microstructure development
Recrystallisation and recovery
Failure analysis
Phase transformations and phase relationships
(Keith will talk about this later)
Detector hardware is also important
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NordlysMax2 Dynamic Studies

NordlysMax2 has an integrated a IR filter


High sensitivity compared to conventional high temperature
phosphor screens

EBSP from Ti
Transformation at 882C
from alpha to beta phase
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In Situ Heating Example: Low C steel


945oC

895oC 0 mins

austenite

895oC 6 mins

880oC

ferrite

GATAN Heating stage


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Forescatter Detector Imaging


Nordlys EBSD detectors can have up to 6 diodes

positioned around the phosphor


Top atomic number(Z) contrast images
Lower - orientation contrast
Side mixed images
FSD images useful for imaging a
well prepared tilted sample (as in EBSD)

These diodes are controlled independently within the Aztec


platform

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Forescatter Detector Control


Up to 6 individual images can be acquired
Settings are controlled within the AZtec interface both
manual and auto settings are available
Automatic optimisation means easy to collect excellent images
Default Z contrast or Orientation contrast settings
Or customise settings
Up to 6 individual images can be
mixed

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Automatic Image Optimisation


This automatic beam optimisation is capable of collecting images
under a full range of beam current and kV.

20kV 10nA

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20kV 5nA

20kV 0.5nA

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AZtec Platform Developments

How Aztec helps in getting better data with ease


Improved Indexing
Distinguishing similar crystal structures
High Angular Accuracy
EDS Integration
Analysis Tools

Point & Linescan


Line Large Area Mapping

TKD
Post Processing
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Collecting Good EBSD Data.....

Takes time and expertise: several variables will impact the result:
Pattern quality: Background, exposure time, SEM conditions
System Calibration: Detector position, working distance
Band detection & Indexing: Manual band selection, choice of

bands and reflectors


The impact if wrong
Lower hit rate, poor phase discrimination, etc...

So there are number of improvements to EBSD acquisition with


AZtec

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Pattern Quality Background Correction


Signal across raw EBSD pattern is steep
Typically static background collection required

Scan speed, grain size, kV,


phase (different Z), and magnification
Potential negative impact on indexing success
New dynamic background correction
implemented in AZtec
Compensates as conditions change
Pattern by pattern contrast optimisation
Works where static background was
inadequate

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Raw EBSP

Background corrected

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AutoExposure
Optimises signal strength to avoid under or over exposure of

the camera
Optimum exposure time calculated for given binning and gain
Uses Signal Strength to optimise the pattern signal : noise

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System Calibration
Accurate indexing requires an accurate calibration of the pattern
centre
Dependant on the geometry of acquisition (i.e. WD & DD)
Refinement is required when conditions/ sample change
Historically extracted from a single pattern
Using AZtec system is always calibrated
Collect data at a full range of WD & DD without refinement
10mm wd

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15mm wd

20mm wd

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Weighted band (Hough peak) selection

Bands chosen preferentially by length as well as intensity


Generally improves fit between detected & actual bands
Allows greater numbers of bands detected in routine use
Improved performance for low density materials demanding a
higher numbers of detected bands (e.g. low symmetry phases)

Plagioclase,
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Typical mapping quality pattern

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Band selection comparison


Example pattern: Low-density silicate mineral at typical mapping speed
Non-weighted band detection

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Weighted band detection

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Aztec Class indexing

Allows effective use of larger numbers of detected bands


Fewer non-solutions and indexing mistakes
Robust indexing on challenging phases
Improves ease of use (# bands no longer critical setting)
Better accommodates overlapping patterns, e.g. at grain
boundaries
Solution from dominant group of bands (from one side)
generally supersedes any mistaken four-band
combinations which include representatives from either
side
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AZtecClass indexing
Improved indexing for overlapping patterns
All-band indexing

Class indexing

Steel

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AztecClass indexing
Improved indexing for phase discrimination
Traditional indexing method

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Class indexing method

Gabbro

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AZtecClass indexing
Improved indexing % for challenging phases
Traditional indexing method

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Class indexing method

Gabbro

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Traditional Indexing Challenges No of bands


Duplex steel sample: four phases; Iron FCC, Iron BCC, Sigma & Chi

12 bands

Too many bands selected


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8 bands

Too few bands selected


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New AZtec Indexing


12 bands

No misindexing
No patches with no solution
Grain boundary minimised

8 bands

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Higher accurate hit rates


Indexing is less sensitive
to user defined settings
Same result 8 or 12
bands
Analysis more robust

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Discrimination of Similar Crystal Structures


Differentiation of two phases with closely related structures and
slightly different unit cell sizes
Pt & Ni weld from the central electrode tip of a spark plug
Pt and Ni same crystal structure
Pt
Ni
9-10% difference in lattice parameter
cubic
cubic
Pt

Ni

fcc

fcc

3.924

3.52-3.57

space
group=225

space group
=225

Conventional indexing cannot


distinguish between the two
phases
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Accurate Phase Discrimination


Sorting solutions based on differences in band width to see detail
of the two separate phases and the mixed region in the weld
Ni Map

Pt Map

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Discrimination of Similar Crystal Structures - TruPhase


This function is applicable on integrated EBSD/ EDS systems
Applies the EDS signal collected in Real Time, simultaneously
with EBSD to assist in distinguishing phases with similar crystal
structure but different chemistry
Then re ranks EBSD solutions, but does not overrule the EBSD
Where there is more than one viable phase identified
through indexing alone the EDS is used to weight the results

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Discrimination of Similar Crystal Structures - TruPhase


TruPhase applies the full X-ray spectrum profile not specific
windows integrals
Therefore it is robust to issues such as changes in background
intensity, peak overlaps and peak pile up
By applying the spectrum profile it does not rely on automatic
peak identification
Reliable operation during Fast Mapping when the X-ray
spectra is likely to contain less statistics
Can be applied in real time as data acquired or within re analysis

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Application Example - Differentiating Cu & Ni:


Phase map

FSD mixed image


Ni

Phase map

Hough based
indexing

TruPhase

Cu

Ni K1

Cu K1
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Cu

Ni

Cubic high

Cubic high

a=3.61

a=3.57

b=3.61

b=3.57

c=3.61

c=3.57
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TruPhase Example Biotite and Muscovite

Fe map

Na map
Al map

Biotite distribution
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Muscovite distribution

Albite distribution
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TruPhase Example Biotite and Muscovite

Normal EBSD map


Similarity between muscovite and biotite
makes it difficult to differentiate the two
phases resulting in the speckly solving in the
muscovite phase

Reanalaysed using TruPhase


Better differentiation of the two phases,
which corresponds to the element
distribution seen in the X-ray maps
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More Advanced Functions


High Orientation Accuracy
Refined Accuracy
EDS Integration
Point & Linescan
Large Area Mapping
TKD

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High Orientation Accuracy Mode


Many factors influence EBSD accuracy (including pattern
resolution, CCD pixels, acquisition conditions, Hough resolution
and band detection)
Aztec Refined Accuracy improves the accuracy of band detection
Delivering more
Traditional Hough based band
accurate
Example shows Ni EBSP
detection
orientation
Refined Accuracy Mode
measurement

Traditional band detection is good


Refined accuracy is better
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Refined Accuracy
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Primary band detection


Apply fast, low resolution Hough to detect a set of 2D bands. High
Hough resolution is used to increase angular resolution. Through PC
and DD convert these to 3D plane normal vectors.

Indexing
From the 3D inter-planar angles, identify all or a subset of the
detected bands as crystallographic lattice planes.

Secondary band detection (only in AZtec Refined Accuracy)


Indexing determines the Bragg angle and thereby the band width.
With this information, refine the band positions in the EBSP, and
utilize the curvature of the Kikuchi bands.

Form the crystal orientation


Calculate the crystal orientation relative to the EBSD detector.
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Refined Accuracy

Refined Accuracy provides :


Higher angular accuracy of orientation measurement
Smaller spread of data, better standard deviation
Better fit pattern & solution

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Integration of EDS & EBSD


Collect and view all data

simultaneously
Apply full data cube to further
interrogate the sample
Phase ID
Identify additional /
unexpected phases
Re-analyse if required

How accurate is EDS


data at high tilt?
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Accurate Integration of EDS & EBSD


Variation in the specimen/ beam interaction causes changes in
Spectra from XPE16 alloy
spectrum background
& peak shape compared to flat samples
collected at 0 (solid) and 70 tilt
(red line ).

AZtec X-ray mapping uses a FLS filtering used for background removal
This is tolerant to changes in background shape
So we can collect accurate X-ray and EBSD maps at tilt
Processed
using
AZtec:
standardless, unnormalised quant routines
But what
about
quant?
with XPP matrix correction (Pouchou et al.)
Comparable result at high tilt & on flat samples:
Wt %
XPE16 - Flat
XPE16 - Tilted 70 deg
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Al
1.23
1.16

Si
0.18
0.19

Ti
1.36
1.16

Cr
17.55
17.78

Fe
33.51
34.01

Ni
42.40
42.94

Mo
3.58
3.53

Total
99.80
Pt100.79
Map
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Phase Identification

Collect spectrum & pattern simultaneously


Multiple EBSP & spectra can be collected
Metal valve used in power engines

matrix is steel, multiple secondary phase


AutoID & quantify spectrum (or select
elements manually).
Based on composition the selected data
bases are searched.
Possible candidate phases listed.
EBSP is searched against the candidate
phases
View pattern with solution overlay to see fit
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Phase Identification EDS & EBSD


Gneiss sample
Phases visible
on BSE image
Collect spectra
from 3 phases:
quartz,
plagioclase &
orthoclase
Select from Am.
Min database
Collect patterns
Collect phase
map
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Phase ID & Re-Analysis


High temperature steel sample mapped
Secondary phase not expected
Therefore no solution
Investigate the map data extract

pattern & spectrum


Identify phases using Phase ID tool
Two additional phases identified
Additional phases added to phase list
Data reanalysed offline to complete
map

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Point Analysis
EBSD Point Analysis
Collect EBSPs and measure the orientation at a series of
points
Tabulate misorientaion between the each point and a
reference
Example
shows a
nanowire

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Linescan
EBSD (& EDS) Linescan
Define a line in either x or y direction, collect EBSPs at
defined step size or based on number of points
Plot misorientation
profile through the
line
Review phase, MAD
etc over the line
Select point on
profile and highlight
in table
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AZtec Large Area Mapping


Unattended collection of high resolution electron images, EBSD and
EDS maps from large specimen areas:
Micro- and Nano- scale from a single data set
Analysis coarse grained material
Statistically valid analysis

2 cm
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How it Works
Collect and montage (EBSD & EDS) data at high resolution and
analyse the montaged image as a single data set
Collect >1500 fields
Automatic field alignment during acquisition using image
correlation
Keeps the sample in focus over the complete sample area,
even when the sample Is not flat

Best illustrated with some examples


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Data Acquisition

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Coarse Grained Mantle Xenolith


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Montaged data set can be interrogated as a single site of interest

1cm

Forsterite
IPF
Cr Map

1cm
1cm
Acknowledge University of Otago
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Folded Rolled Nickel Sheet


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Gas pipeline material, examine texture changes through fold


Link texture to corrosion
90 fields collected over Ni sheet
Large area mapping and montaging provides an overview of the
whole sample at a high level of detail:
Grain Boundary map shows:
Black = high angle grain
boundary
Red = twin boundaries
Grey low angle
boundary <2
Indicate regions of
deformation in sheet
1000um
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Folded, Rolled Nickel Sheet


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Rolled Ni sheet, 100 fields


IPF X map, systematic texture variation associated with folding

1000um
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AZtec LAM Image Registration


The montaged image is automatically registered in AZtec and can

be used for relocation and navigation


The montaged image (or other Aztec image) can be imported
into AZtec at a later date, re-registered using fiducial markers and used to relocate to regions of interest on the specimen

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MapQueue
Individual point mapping experiments can
be queued up
Each mapping experiment (EDS or EBSD)
can have different resolutions, dwell times,
solver settings, Phase lists...
Each point acquisition can be EDS, EBSD or
both

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Transmission Kikuchi Diffraction


Powerful variation of EBSD
Lots of interest
Many papers / conference
talks
Applies standard EBSD
system to an electron
transparent sample
Sample close to horizontal
with short working distance
Optimise spatial
resolution
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Challenges with Transmission Kikuchi Diffraction


Typical TKD pattern

Al sample
Pattern distortion resulting from TKD geometry
causes wider bands in the lower pattern
Non symmetric intensity seen in the broad bands
This results in inaccuracy in the band detection

TKD Optimised
Mode
With new band
detection bands are
correctly detected

MAD = 1.1

MAD = 0.13
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TKD Optimised Mode

In this mode a new band detection

routine
is applied which is more accurate
It takes into account the
band position relative to the pattern
centre and detector position
As a result can work with the sample
close to horizontal at short working
distance
Optimising spatial resolution

2um

Strained nanocrystalline copper sample showing IPF-Z


direction, high angle boundaries in black and CSL boundaries in colour. Step size 4nm.
Credit: Saritha Samudrala (University of Sydney) and Kevin Hemker (Johns Hopkins University)
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Data Analysis Improvements


All data can be exported to the post processing packages
64bit so can handle large data sets
Large number of processing and display options
Include clean up functionality
Capability to create subsets
Creation of crystallographic data files

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Data Analysis Improvements


The map data values for grain and grid maps created in Tango

can now be exported as a text file


This means the map calculations can be used as input into
other third party software
The calculated (M)ODF values can also be exported as a text file

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Data Analysis Improvements


New grain sizing filters introduced which follow the ISO
DIS13067
Easier to filter the data so that clusters which are too small to
be considered as a grain can be removed from the grain
statistics.

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Data Analysis Improvements


Export of the Grain ID together with the orientation data added
to the Record Browser
Texture components modified so if multiple components are
used at the same time then the data pixels can only contribute to
one component, easing calculation of area fractions
Axis alignment component to get boundary fraction fulfilling a
given criteria

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Data Analysis Improvements New Maps


GROD Grain Reference Orientation Deviation (GROD) Angle

Visualises substructures in the


sample.
The average orientation is
determined for each grain. The
deviation from this mean
orientation is then plotted for
each pixel within that grain.

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Data Analysis Improvements New Maps


Grain Reference Orientation Deviation (GROD) Axis

The average orientation is


determined per grain.
The axis around which the
orientation is rotated is
calculated and displayed as a
colour
Those grains which are speckled
have an orientation which is
close to the mean

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Data Analysis Improvements New Maps


Grain Reference Orientation Deviation (GROD) Hyper

The GROD Hyper combines both the

axis and angle, relative to the mean


orientation of the grain
This map combines 4 coordinates
(from the axis, x,y & z, and the angle)
in a 3D colour space to display subtle
internal grain structures.
This map is a visual
representation
but is not a
quantification
of the data.
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Summary

Range of applications for EBSD is growing


Increasing requirements to understand how microstructure

influences materials behaviour


Manufacture higher performing materials
Interest in technique is growing
Faster acquisition
Smaller features
Larger Samples
Higher accuracy
More challenging applications
AZtec is solution for all applications

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