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Lecture Electron Microscopy part 4

The document discusses advanced techniques in materials characterization, specifically focusing on electron diffraction. It covers the geometry of electron diffraction, methods for indexing diffraction patterns, and different types of electron diffraction, including selected area electron diffraction and convergent beam electron diffraction. Key concepts such as Bragg's Law, the Ewald sphere, and zone law are also explained in relation to analyzing crystal structures and orientations.

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9 views

Lecture Electron Microscopy part 4

The document discusses advanced techniques in materials characterization, specifically focusing on electron diffraction. It covers the geometry of electron diffraction, methods for indexing diffraction patterns, and different types of electron diffraction, including selected area electron diffraction and convergent beam electron diffraction. Key concepts such as Bragg's Law, the Ewald sphere, and zone law are also explained in relation to analyzing crystal structures and orientations.

Uploaded by

jj6556117
Copyright
© © All Rights Reserved
Available Formats
Download as PDF, TXT or read online on Scribd
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Department of Materials Science and Engineering

Advanced Techniques in
Materials Characterization

By:
M. Sarkari Khorrami
Fall 2016
Electron Diffraction

2
Outline
๏ Introduction

๏ Geometry of Electron Diffraction

✴ Diffraction Spot Patterns

✴ Reciprocal Lattice in Electron Diffraction

๏ How to Index Electron Diffraction Patterns

๏ Other Types of Electron Diffraction

3
Introduction
Electron Diffraction

๏ Elastically scattered electrons passing through a thin specimen

๏ Two types of information:

‣ Angular distribution of scattered electrons:

➡ crystal structure and orientation

‣ Intensity of scattering:

➡ atomic scattering factor / structural factor / interpret TEM image

4
Introduction
Pattern of Various Types of Material

Poly-crystal

W
Single crystal

Amorphous
LaB6

5
Geometry of Electron Diffraction
Bragg’s Law

๏ Locally coherent electron beam:

nλ = 2d.sin θ
๏ Each strongly diffracted beam is
associated with set of crystal planes

๏ Only first order of diffraction

๏ As 𝜆 is extremely small (~0.0037 nm when acc=100 kV) and d~0.4 nm:

sin 𝛉 =0.0046 and 𝛉 =0.26 deg.=0.0046 rad.; so: sin 𝛉 ~ 𝛉

6
Geometry of Electron Diffraction
Diffraction in TEM

๏ Only allowed hkl can diffract (Fhkl)

๏ For small diffraction angle:

g λ
= = 2θ or gd = Lλ
L d

๏ L𝜆: camera constant

๏ g: distance of diffraction spot (∝1/d)

7
Geometry of Electron Diffraction
Selected area electron diffraction
(SAED) pattern

๏ Only planes almost parallel to e-beam can


diffract g

๏ SAED pattern is a scaled section through


the reciprocal lattice normal to the beam.

๏ Scaling factor is L𝜆 (camera constant)

8
Geometry of Electron Diffraction
Selected area electron diffraction (SAED) pattern

9
Geometry of Electron Diffraction
SAED Pattern & Ewald Sphere

๏ SAED patterns contains so many


diffraction spots. Why?

๏ Since wavelength of electron beam


is quite small, radius of Ewald
sphere is large (almost flat)

๏ In XRD, Ewald sphere intersects


the reciprocal lattice at one point.

10
Geometry of Electron Diffraction
ED from Finite Thickness Crystal

๏ Diffraction occurs from planes slightly


deviated from the Bragg angle (s)

๏ Weak diffraction

๏ Thinner crystal => further the crystal


may deviate from Bragg angle and
yet diffract.

๏ How Ewald Sphere can interpret?

11
Geometry of Electron Diffraction
SAED Pattern & Ewald Sphere

12
Geometry of Electron Diffraction
Ewald Sphere for Thin Sample

๏ More probability in intersection of


the reciprocal lattice point and
Ewald sphere

13
Geometry of Electron Diffraction
Zone Law

๏ If the lattice vector [uvw] lies in the plane (hkl):

uh + vk + wl = 0 (zero-order Laue zone)

๏ “Zone axis” in electron diffraction:

Electron beam oriented parallel to a lattice vector

๏ Diffracting planes must be parallel to electron beam. Thus, they obey

the Zone Law.

14
How to Index ED Patterns
Polycrystalline Materials

๏ All possible diffraction similar to powder pattern

๏ Measure radius of each ring

๏ Calculate the ratio R1/R2

๏ Check the ratio for various crystals

๏ R1d1 = R2d2 or R1/R2 = d2/d1

15
How to Index ED Patterns
Single Crystalline Materials

๏ Measure Ri and angles between reflections


๏ Calculate di (=L𝜆/Ri) for i=1,2,3
๏ Compare with theoretical d-values
๏ Compare Ri/Rj with tabulated values for cubic
structure (h2k2l2)

๏ g1,hkl+ g2,hkl=g3,hkl (vector sum must be ok)


๏ Perpendicular vectors: gi ! gj = 0
๏ Zone axis: gi x gj =[HKL]z Orientations of corresponding
planes in the real space
๏ All indexed g must satisfy: g ! [HKL]z=0

16
How to Index ED Patterns
Example:

17
How to Index ED Patterns
Example:

18
How to Index ED Patterns
Example:

19
How to Index ED Patterns
FCC Patterns from Various Zone Axes

20
How to Index ED Patterns
BCC Patterns from Various Zone Axes

21
Other Types of ED
Kikuchi Line Patterns

๏ Inelastic scattering event


scatters electrons in all
directions inside crystal

๏ Some scattered electrons


in correct orientation for
Bragg scattering => cone
of scattering

22
Other Types of ED
Convergent Beam ED Patterns

๏ Instead of parallel illumination


with selected-area aperture,
CBED uses highly converged
illumination to select a much
smaller specimen region.

23
Question
1. Which diffraction pattern can accurately determine the crystal
orientation?

2. What are Kinematical and Dynamical theories of electron


diffraction?

24

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