SAND2014-0145C

Introduction to EBSD and Crystallography

Joe Michael
Sandia National Laboratories
Albuquerque, NM USA

Sandia is a multiprogram laboratory operated by Sandia Corporation, a Lockheed Martin Company,

for the United States Department of Energy under contract DE-AC04-94AL85000.
 Characterization in the SEM

A cornerstone in the study of both natural and technological materials is

characterisation of microstructure. In the widest sense this topic encompasses, for all
phases present:

Morphology, including size and shape distributions

Chemical composition, phase identification

Crystallographic parameters, including orientation and orientation

relationships

Before development of EBSD – each aspect was measured separately using different
techniques and tools

Now, with EBSD, the SEM is a legitimate tool for the measurement and understanding
of the sample crystallography (texture, phase identification).
Number of EBSD Journal Citations over past 23 years

1000

Number of publications
800

600

400

200

0
1990 1995 2000 2005 2010
Year
From Index Search - using EBSD, EBSP, BEKP, t-EBSD and TKD for
search criteria
Applications of BEKP to Materials

Two Areas of application for BEKP:

Orientation Analysis
crystallographic orientation of small areas
use patterns to calculate the relationship between the crystallographic
axes some external reference frame ( i.e. rolling direction)
use patterns to determine the crystallographic relationship between two
adjacent areas of the sample (i.e. grain boundary misorientation,
precipitate/matrix orientation)
Micro-texture imaging of polycrystalline samples with automated pattern
indexing

Phase Identification
Identify unknown phases from their crystallography
Bulk samples (metallographically polished surfaces)
Particulate on substrate (no preparation needed)
Fracture surfaces (identify phases directly on fracture surfaces)
EBSD provides structural information about
phases present in crystalline materials, namely
the crystallographic orientation at precise
locations. The combination of good spatial
resolution, large area coverage, relative ease of
use, and supplementation with other SEM tools
has promoted EBSD to one of the premier
techniques for microstructural analyses.

EBSD Capabilities include:

• Orientation mapping
• Grain size and grain boundary analysis
• Texture measurements
• Phase identification
• Strain analysis
 Microtexture

A definition of microtexture is:

‘A population of crystallographic orientations whose individual components

are linked to their location within the microstructure.’

Example: W wire drawn

to 11 m diameter.
Typical fiber texture
developed.
Phase Identification

Particle mounted on polished carbon

substrate
Identified as Plattnerite (PbO2) tetragonal
Alternative Techniques

Alternatives to SEM
Transmission electron microscopy – sample prep, small areas
X-ray diffraction – large areas, no imaging

SEM-based alternatives to EBSD

Selected area channeling patterns – normal incidence, low resolution,

more difficult to set up

Kossel diffraction – low spatial resolution, high accuracy, not applicable

to all samples
 History of EBSD

Backscattered Electron Kikuchi Patterns

BEKP
Electron Backscatter Diffraction (Patterns)
EBSD or EBSP
Backscattered Kikuchi Diffraction
BKD
Wide Angle Kikuchi Patterns
WAKP
First observed in 1954 - before SEM invented
1970’s Venables et al. were first to observe EBSP in SEM
1980’s D. Dingley et al., N. H. Schmidt R. Schwarzer began using these
patterns for orientation studies
1990’s Wright and Adams developed automatic system for texture
Michael et al. develop technique for phase identification
 Early Work on EBSD (before the first SEM was invented)

M. N Alam, M. Blackman, D. W.
Pashley, “High Angle Kikuchi
Patterns”, Proc. Royal Society of
London, A221, 1954, p. 224
 Early Work on EBSD (First SEM application)

Harland, Akhter and Venables,”Accurate microcrystallography at high spatial resolution using

electron back-scattering patterns in a field emission gun scanning electron microscope”, Journal
of Physics E, vol 14, 1981, p. 175.
Interesting References from the 1980’s

D. J. Dingley, A comparison of diffraction techniques in the SEM, SEM-1981, p273

Good early review of EBSD, SACP and Kossel

D. J. Dingley, Diffraction from sub-micron areas using EBSD in an SEM, SEM-1984, p.

569.

D. J. Dingley, et al, Online Analysis of EBSD Patterns, SEM-1987, p. 457.

Demonstrated on-line indexing of patterns for texture measurement

D. J. Dingley and Baba-Kishi, Use of EBSD patterns for determination of crystal

symmetry elements”SEM-1986, p. 383.
Nice demonstration of crystal structure inference from symmetry

D. J. Dingley et al., Application of backscatter Kikuchi diffraction for phase

identification and crystal orientation measurement, Microbeam Analysis, 1989, p. 435
On-line indexing of patterns
Wright and Adams Contributions

Wright and Adams, Automatic analysis of electron backscattered diffraction

patterns, Metallurgical Trans. A., vol 23A, 1992, p. 759.
Excellent discussion of automated line finding algorithms (Hough,
Burns)

Adams, Wright and Kunze, “Orientation Imaging: The Emergence of a New

Microscopy, Metallurgical Trans. A., vol 24A, 1993, p. 819.
coins term “Orientation Imaging” demonstrates automated mapping
Automated indexing requires 2 seconds per pattern!!!
 Phase Identification

Baba-Kishi and Dingley, Backscatter Kikuchi diffraction in the SEM for

identification of crystallographic point groups, Scanning, vol.11, 1989, p. 305
Excellent demonstration of using EBSD patterns and symmetry
elements to determine point group of an unknown.

Michael and Goehner, Crystallographic phase identification in the scanning

electron microscope: Backscattered electron Kikuchi patterns imaged wth a
CCD-based detector, MSA Bulletin, vol 23, 1993, p. 168
First images recorded using CCD camera

Goehner and Michael, Phase identification in a scanning electron microscope

using backscattered electron Kikuchi patterns, J. of Research of the National
Institute of Standards and Technology, vol 101, 1996, p. 301.

Demonstration of phase identification using CCD camera and PDF

crystallographic database.
 Channeling Patterns and Contrast - Theory

Backscattering probability related to how close the electrons approach the

nucleus of an atom

For crystalline materials, some

orientations will result in the electrons
moving parallel to planes of atoms

This results in a modulation of the

backscatter yield that is related to the
orientation of the crystal lattice
 Effect of Crystallography on BS Yield

Si Lattice
diamond cubic

(110)
(3 1 6)

Many open channels in this orientation Few open channels in this orientation
 Channeling Contrast - Examples

Tantalum tensile sample Weld in stainless steel

Channeling Patterns - Theory

During the scan the

incidence angle of the beam
with the specimen is
continually changing.
At some beam positions
Bragg’s Law is satisfied
resulting in a change in the
backscatter yield.
Electron Channeling Pattern (ECP) of Mo at 20 kV
Fine Structure in Diamond ECP

25 kV

Fine structure in ECP is very

sensitive to variations in:
operating voltage
30 kV crystallographic plane spacings
Kossel Patterns - Theory

X-rays generated by the electron

beam are diffracted on exit from
the specimen surface.
These diffracted characteristic
x-rays form cones on intensity.

Specimen must efficiently

diffract its own characteristic x-
rays. If not a technique called
pseudo-Kossel may be used.
 Kossel Pattern of Ni

Kossel X-ray Diffraction in the

SEM provides:

•Accurate lattice spacing

measurement to 5 parts in 104
•Spatial resolution of 10-100 µm
•Depth resolution of 1-2 µm
•Accurate lattice spacing
measurement will permit the
determination of strain tensor
on a µm length scale
•Possibility of strain mapping
Pattern recorded at 20 kV and 20 nA. of microstructure
EBSD Pattern of PbMoO4 (Wulfenite)

Pattern Features:
Parallel lines are Kikuchi line
pairs
Spacing between pairs is twice
the Bragg angle and inversely
related to the d-spacing
Places where lines intersect
called zone axis
Angles between zone axes are
indicative of crystal structure
Origin of EBSP ( Backscattered electron distributions)

Amorphous Sample Crystalline Sample

Tilted Crystalline Sample

Backscattered Electron Angular Distribution

Note the low

contrast of the
EBSD signal
 Origin of Kikuchi Lines (Diffraction or Channeling?)

Electrons are initially scattered inelastically

(small energy loss) followed by elastic
scattering from atomic planes in the Plane trace
sample. The angular separation between
Kikuchi lines is twice the Bragg angle





Source of electrons

Diffracting planes
Sample surface

Alternatively: Electrons are channeled out of the sample, thus

EBSD patterns are reciprocity related to selected area
channeling patterns.
Effect of Beam Voltage on EBSD

5 kV 10 kV 20 kV

30 kV 40 kV
 Why do we need to tilt the sample?

# Backscattered electrons

0 10 20 30
Energy (kV)
Tilted sample has higher BS electron yield
Sample tilt results in sharp peak in BS electron energy distribution. Better defined
energy of BS electrons results in sharper Kikuchi lines.
 Spatial Resolution of EBSD

Incident
beam

Incident
beam

Absolute radii for 0.5 keV loss

are 40, 15 and 10 nm for Al, Cu
and Au.
Resolution of EBSD in Aluminum

Resolution depends on direction Smaller probe sizes (lower current)

due to sample tilt. improves resolution.

2.5 1.40
perpendicular
parallel parallel
perpendicular
1.20
2
Resolution (m)

Resolution (m)
1.00
1.5

0.80

1
0.60

0.5
0.40

0 0.20
15 20 25 30 35 40 45 0.1 1 10 100

Accelerating voltage (kV) Probe Current (nA)

(Standard conditions are: 20 kV, 5 nA, 15mm, 70°)

Data from: V. Randle, Microtexture Determination and its Application, The Institute of
Metals, 1992.
 Measured Spatial Resolution ( FEGSEM)

Longitudinal Resolution Lateral Resolution

2000 350

300

1500
Spatial Resolution (nm)

250
Al
200
1000

150

100
500 Cu
50

0 0
5 10 15 20 25 30 35 5 10 15 20 25 30 35

Beam Voltage (kV)

From:S. X. Ren et al. , Microscopy and Microanalysis, 4, 15-22, 1998

 EBSD of Au Islands on Si

Single crystal patterns have been obtained from 0.1 m Au islands.

Alumina (Al2O3) On Thin Substrate
 Depth Resolution of EBSD (calculated)
250
From Monte Carlo
electron trajectory
200
simulation assuming a
maximum energy loss of
10%.
Depth Resolution (nm)

150

100

50

0
10 15 20 25 30

Beam Voltage (kV)

From:S. X. Ren et al. , Microscopy and Microanalysis, 4, 15-22, 1998

 Depth Resolution of EBSD (thin Al sample)

Sample thickness:
CBED - 240. nm
EELS - 190 nm
Direct measurement - 220 nm

Monte Carlo
Backscatter yields
20 kV 40 kV
Bulk 0.5 0.5
Thin 0.3 0.14
Remainder of
electrons in thin
sample are
20kV 40kV transmitted.
Transmission Kikuchi Diffraction of FIB prepared thin samples in the SEM

TEM FIB prepared sample imaged at 30 kV

Experimental set up in FIB

Au with 2 vol % ZnO –Transmission Kikuchi Diffraction Resolution

FIB prepared plan-view sample. Mapping was performed with

a 4 nm step size. (minor processing applied)
3D EBSD now fully automated with dual platform FIB

Electroplated Sn with whisker

 Summary

EBSD has been around a long time – has become a more common tool
Early EBSD work was in 1954!
EBSD patterns result from either diffraction or channeling of the electrons
Lack of an exact understanding of the pattern formation does not
stop us from using them
EBSD has two main uses:
Orientation and phase identification
There are alternatives to EBSD
All suffer severe disadvantages when compared to EBSD
Spatial resolution of EBSD in the SEM is very good
Less than 100 nm is routinely attainable in back reflection mode
and 2-10 nm in transmission mode
 Useful Reference Books

Crystallography:
C. Hammond, “The Basics of Crystallography and Diffraction”,Oxford University Press, 1997.

SEM:
J. I. Goldstein et al.,”Scanning Electron Microscopy and X-ray Microanalysis”,Kluwer
Academic/Plenum Press, 2003.

EBSD:
V. Randle, “Microtexture Determination and its Applications”, The Institute of Materials, 1992.

A. J. Schwartz, et al., “Electron Backscatter Diffraction in MaterialsScience”,Kluwer

Academic/Plenum Press, 2001.
V. Randle and O. Engler, “Texture Analysis”, Gordon and Breach Science Publishers, 2000.

Hough Transforms:
V. F. Leavers,”Shape Detection in Computer Vision Using the Hough Transform”, Springer-Verlag,
1992.