Documenti di Didattica
Documenti di Professioni
Documenti di Cultura
Oxford Instruments
Recent Developments in EBSD
Jenny Goulden
Page 1
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
Page 2
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
Page 3
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
Page 4
Page 5
Page 6
Page 7
NorldysNano
Delivers the best possible sensitivity while accurately imaging
the EBSP
60% more sensitive than older EBSD detectors
Page 8
Page 9
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
Page 10
NordlysNano
5kV Ni 0.5um grain size 100Hz
Aluminia Insulator
10kV
Alumina NO coating
Hit Rate 85% (porous sample) at
90Hz
5kV
Oxford Instruments 2015
Page 11
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)
Oxford Instruments 2015
Page 12
Page 13
Page 14
Page 15
NordlysMax2
Phase Map
870Hz
99% indexed
12nA
Ni sample
Ni X-ray Map
100um
W X-ray Map
Page 17
Page 18
EBSP from Ti
Transformation at 882C
from alpha to beta phase
Oxford Instruments 2015
Page 19
895oC 0 mins
austenite
895oC 6 mins
880oC
ferrite
Page 20
Page 21
Page 22
20kV 10nA
20kV 5nA
20kV 0.5nA
Page 23
TKD
Post Processing
Oxford Instruments 2015
Page 24
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
Page 25
Raw EBSP
Background corrected
Page 26
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
Page 27
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
15mm wd
20mm wd
Page 28
Plagioclase,
Oxford Instruments 2015
Page 29
Page 30
Page 31
AZtecClass indexing
Improved indexing for overlapping patterns
All-band indexing
Class indexing
Steel
Page 32
AztecClass indexing
Improved indexing for phase discrimination
Traditional indexing method
Gabbro
Page 33
AZtecClass indexing
Improved indexing % for challenging phases
Traditional indexing method
Gabbro
Page 34
12 bands
8 bands
No misindexing
No patches with no solution
Grain boundary minimised
8 bands
Page 36
Ni
fcc
fcc
3.924
3.52-3.57
space
group=225
space group
=225
Page 37
Pt Map
Page 38
Page 39
Page 40
Phase map
Hough based
indexing
TruPhase
Cu
Ni K1
Cu K1
Oxford Instruments 2015
Cu
Ni
Cubic high
Cubic high
a=3.61
a=3.57
b=3.61
b=3.57
c=3.61
c=3.57
Page 41
Fe map
Na map
Al map
Biotite distribution
Oxford Instruments 2015
Muscovite distribution
Albite distribution
Page 42
Page 43
Page 44
Page 45
Refined Accuracy
The Business of Science
Indexing
From the 3D inter-planar angles, identify all or a subset of the
detected bands as crystallographic lattice planes.
Page 46
Refined Accuracy
Page 47
simultaneously
Apply full data cube to further
interrogate the sample
Phase ID
Identify additional /
unexpected phases
Re-analyse if required
Page 48
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
Oxford Instruments 2015
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
Page 49
Phase Identification
Page 50
Page 51
Page 52
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
Page 53
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
Oxford Instruments 2015
Page 54
2 cm
Oxford Instruments 2015
Page 55
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
Page 56
Data Acquisition
Page 57
1cm
Forsterite
IPF
Cr Map
1cm
1cm
Acknowledge University of Otago
Oxford Instruments 2015
Page 58
Page 59
1000um
Oxford Instruments 2015
Page 60
Page 61
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
Page 62
Page 63
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
Oxford Instruments 2015
Page 64
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
Page 65
Page 66
Page 67
Page 68
Page 69
Page 70
Page 71
Page 72
Summary
Page 73