Microstructural Characterization Using EBSD

Electron Backscatter Diffraction

Sometimes referred to as Backscattered Kikuchi Diffraction (BKD) A diffraction technique for obtaining microtextural information from small areas of bulk samples in the scanning electron microscope (SEM)

Steven R. Claves

Advantages

Disadvantages

Imaging & Crystallography Crystalline samples Orientation of individual grains Free of excessive plastic strain Simple sample preparation

Components of an EBSD system

SEM source
High current High brightness

Components of an EBSD system

Phosphor Screen
Size Position
# poles Detail

Sample
~70 tilt BSE yield
Forward scattered Detector position

Camera
TV rate (speed/cost) CCD (quality)

OIM*
Computer scan control Data analysis
OXFORD
*Sometimes referred to as ACOM (automated crystallographic orientation measurement)

resolution
OXFORD

Tilt correction Dynamic focus

OIM* - (orientation imaging microscopy)

How the Pattern is Formed

EBSP - Electron Backscatter Diffraction Patterns

Map of the angular relationships between the atomic planes Orientation determined by indexing the EBSPs

OXFORD

high energy electrons are elastically scattered by atomic planes in a crystallographic sample

Si single crystal Three Euler Angles

EBSP - Electron Backscatter Diffraction Patterns

As the sample is rotated, the pattern changes to reflect the new orientaion

EBSD Samples
BSE yield depends upon elements
Lateral resolution & depth as well

Si single crystal

EBSD is a surface sensitive technique

0 5

Flat surface (irregularities ok for non-mapping applications) High dislocation densities mar pattern quality

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15

20

25

30

Mechanical polishing, 0.05 m colloidal silica Light etch to remove surface deformation Alternative final steps
Lapping Electropolish / electroetch (non-anodizing) Chemical polish

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Step 1: Loading the Sample

Orientation data (i.e. angles) with respect to what? Sample must be aligned properly in microscope
detector

Step 2: Acquire a Background

Use fast scan at low mag. to acquire an average pattern from many differently oriented grains Flat, even intensity

TSL
Crystallographic orientation related to sample orientation

TSL
System geometry

Step 3: Single Grain EBSP

Fix beam position (spot mode) within a grain Raw pattern will have weak contrast

Step 4: Subtract Background

Remove constant bkg to increase contrast (bkgs may also be divided or other manipulations)

History
EBSP first observed in 1954 (Alam et.al.) Venables & Harland 1973 SEM with video rate camera Background correction / flat fielding Eventually high gain CCD cameras Burns algorithm for edge detection (Wrights,Adams92) Hough Transform (Krieger Lassen, Jensen 92)
Orientation Imaging: The Emergence of a New Microscopy
B.L. Adams, S.I. Wright, K. Kunze Met Trans 24A 1993

Hough Transform
Sum up pixel intensities along line Move the position and angle of the line Convert Kikuchi bands (2D) to a point (1D)

Hough Transform

Step 5: Load Phase Information

Phase page from TSL software

distance

angle

Calculated position of poles from: Point group lattice parameters Calibration

start with vertical line move counterclockwise

EBSPs
Poles are identified by their inter-relationships
based upon known interplanar angles

Interplanar Angles
Lattice parameter and space group will determine the interplanar angles (measured by distance on the pattern)
FCC - Aluminum

Can identify poles by eye using crystal symmetry

Fm3m a = 4
<100> 4/m

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<110>

<110> 2/m

3D cube showing the symmetry of the m(-3)m space group.

<100>

Step 6: Calibration & Indexing

Distances between poles are fixed for system setup
Calibration based upon screen position & WD

EBSD Mapping
e- beam rasters across sample generating EBSPs Computer instantaneously indexes each point Records orientation data for each beam position
Incident e- beam phosphor screen Fiber-optic cable to video camera

Location of the poles on the pattern determines the orientation

crystalline sample

diffracted electrons

Diffracted patterns appear on screen

Microtexture
A population of orientations measured on a grain-by-grain basis

Grain Mapping
Computer determines point-to-point misorientations When angle exceeds a certain threshold a new grain is declared

6xxx Al Alloy

x,y 1, , 2 CI IQ phase

Large Areas
Capability to perform large area scans as well
Stage scan Stage/beam scan combo.

Small Area Maps

Unique Grain Map Each grain given specific color 2.5 m step size EBSD limited by spatial resolution of SEM
! W ~ 0.5 m step size ! Schottky ~ 5 nm

Limited by size of chamber and system geometry Stage / beam scan

Orientation Maps
Inverse pole figure grain map Grains of similar orientations are given like colors Note poor pattern quality at grain boundaries

Applications of EBSD
[Micro]Texture Analysis Misorientation Angles & Special Grain Boundaries Grain Size (Pseudo) Strain Mapping via IQ index Phase Identification
(phase determination)

PF, IPF, & ODF

Discrete Pole Figure

Pole Figures
Display orientations of highest probability

Contour - Inverse Pole Figure

Intensity - Orientation Distribution Function

Inverse Pole Figure Maps

Orientation given with respect to a specific direction
(ND, TD, RD) Extruded Al
-fiber texture along RD

EBSD Comparison

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Individual grains are given unique colors Good Agreement between the simulated grain map and the backscattered electron image

Grain Size Maps

Misorientation Angle

(Can also use linear intercept method)

Special Grain Boundaries

Coincident Site Lattices (CSL) Grain boundary engineered Cu
= 3,9,27

Special Grain Boundaries

Coincident Site Lattices (CSL) Grain boundary engineered Cu
= 3,9,27 65% 3 twins

Strain Measurements
Wilkinson & Dingley (91) Plastic Strain Sharpness of band edges Wilkinson (96/97) Increase distance to camera Small (mrad) shifts in location of zone axes

Phase Identification
Phase determination
Known phases
different crystallographic properties

Phase Identification
Unknown phases In combination with EDS Searchable databases Phase Identification in a Scanning Electron Microscope Using Backscattered Electron Kikuchi Patterns
R.P. Goehner & J.R. Michael J. Res. Natl. Inst. Stand. Technol., 101, 301 (1996)

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-Al8Fe2Si

-Al9Fe2Si2

Varying SEM Conditions

Spot size / beam current, (nm / nA) Accelerating voltage, kV Working Distance, WD (mm) Tilt Angle, degrees ()

Effect of Beam Size

Greater beam sizes = more current
Spot size / C1 current Gun bias

Lower acquisition times Better quality patterns (increased accuracy) Largest possible beam size depends upon
Grain size Desired step size

[ Cast 6xxx Al Sample ]

2x2 binning (650 x 525)

Spot size = 3 (35 nm) Current = ~ 0.1 nA Acquire time = 8s Spot size = 7 (0.58 m) Current = ~ 14 nA Acquire time = 0.2 s

Effect of kV
Changes width of bands Poles stay in same positions

5 kV

15 kV

25 kV

10 kV

20 kV

30 kV

Effect of Working Distance

Moves pattern center (Changes the area of maximum BSE intensity) Calibration is very important
e-

Effect of Tilt Angle

Modifies BSE yield Changes the distance angle conversion Calibration is very important
TSL
e-

x* y*

z*

x* y*

z*

TSL

62 16 mm 20 mm 24 mm 28 mm 58 66

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Microtexture Variation EBSD 2 Metal Forming Examples

surface

Surface

X [100] ND {hkl}

Z [001] RD <uvw>

Pole Figures
Small, Equiaxed
Cube texture {001}<100>

Macro Photographs
I Dead Metal Zone (DMZ) II Shear Intensive Zone (SIZ) III Transition Zone (SIZ 2) IVa Main Deformation Zone (MDZ) IVb - Negative Flow Angle (MDZ 2)
z x
Die face

Large, Elongated
FCC shear texture {111}<110>

IVb

I II IVa III
y
10 mm

Micrographs
Etched in Barkers Reagent
Grain contrast under polarized light Boundaries appear dark
extrusion direction

Micrographs
Record metal flow direction (angle)

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III surface center

Record angle with respect to extrusion direction

centerline

BILLET

surface

Pole Figures

Microstructural Detail
Small step size

<111> <100>