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Homework 3

Nikhil Dube

1) a.

4 22 4 40
4 40

4 04
2 20

242
4 04 2 24
2 02 0
2 2 0
4 4
242

440
022 000
2
2 4

2
0 2
220

4
0 4
242

The separation between two Kikuchi lines is equal to the separation between the (hkl) the
(000) diffraction spot. The direction of diffraction spots is normal to the diffracting
planes, so the angles between Kikuchi line pairs is equal to the angles between their
corresponding diffraction spots.
b.

Ewald sphere construction of the given pattern is sketched below for silicon [ DB Williams,
CB Carter, Transmission Electron Microscopy, Diffraction II, Springer, NY (1996)]

The figure below shows Ewald sphere construction that illustrates the diffraction
condition, with sg > 0 for -404 reflection.
c.

g2 x
Deviation parameter s is given as s = , where x is the distance between the
k r
diffraction spot and its corresponding bright Kikuchi line and r is the distance between
the Kikuchi lines of order g.
The measurements taken for diffraction spot -24-2 have values x = 1 cm, r = 3.5

g2 x g2
s= = .286 = 1.794 g 2 λ
k r k

For g =2

s = 7.177 λ

Where λ is the wavelength of X ray radiation.

2)
WinWulf © 2007, JCrystalSoft is used to solve the present problem.
a.
[011] Stereographic Projection

(111) twinning plane


The positions of the poles after twinning are found by reflecting them across the great
circle of the (111) twinning plane. The diffraction pattern from the twin is found by
taking the poles of the original crystal, reflecting them through the twinning plane, and
seeing which poles then lie on the circumference of the stereographic projection. The
poles on the circumference provide the diffraction pattern.

(111) twinning plane


b.

The diffraction pattern is generated from WinWulf software by rotating stereographic


projection so that Line A coincides with the circumference of great circle.

Diffraction Pattern of twinned FCC cystal

3)
The indices in white correspond to the Al matrix, whereas the indices in blue correspond
to the θ’ precipitate. θ’ has a tetragonal crystal structure and Aluminium is FCC.

The figures are taken from B. Fultz and J.M Howe Transmission Electron Microscopy
and Diffractometry of Materials, 2nd Ed., Springer, NY, (2002).

2 20
020
1 30 130 220

2 20 020
1 10 220
110

2 00
000
200
1 10
110

2 20
220

1 30
130
2 20
020
220

The θ’ phase forms as thin plates on all three {001} Al matrix planes. When a thin foil is
viewed along a <001>Al orientation, one variant of θ’ is face on, while the other two
variants are edge-on and perpendicular to each other. The Al matrix and each variant of
θ’ phase each produce a different diffraction pattern. When all three variants are present
within the selected area aperture, all of these diffraction patterns are superimposed.
The diffraction patterns for the Al matrix in a <001> orientation, and two variants of the
θ’ phase, one face-on along [001] and the other edge-on along [100] are shown below.
The diffraction pattern for the third variant can be obtained by rotating the [100] θ’
pattern by 90 degrees. The superposition of the three variants and the Al matrix yield the
diffraction pattern shown above.
Comparing the superimposed diffraction pattern with all three variants to the one given in
the problem, the given diffraction pattern is an [001] Al matrix with [001] θ’ precipitate
phase.

4)
a

The intensity oscillations originate from dynamical diffraction conditions under strong
scattering. Energy is transferred between the forward scattered beam and the Bragg beam.
The following are the assumptions for this method to be valid.
• The foil should not be tilted too far from its position normal to the beam.
• Low order reflections should be avoided to minimize the effects of multiple
scattering from the systematic reflections.
• The reflections with very small d values (< 0.5 Ǻ) are not reliable because of their
low overall intensity and long exposure times.
• The choice of the reflection should be exact Bragg position in an orientation where
the region around both the diffracted spot and the center spot is free of Kikuchi lines.
In this way, the pattern is closest to true two-beam and multiple scattering form stray
reflections are reduced.
b

The values of si are determined by measuring the distance Δθi from the center of the
diffracted beam to each successive minimum, and the distance 2θd between the center
spot and the diffracted spot
λ  ∆θ 
si = 2  i 
d  2θ d 
where λ is the wavelength and d is the spacing of the operating reflection.

2 2
s  1  1  1
Foil thickness is calculated using the relation  i  +    =
 ξ 2  t2
 ni   ni   g

The plot (si/ni)2 versus (1/ni2) gives the foil thickness as the y-intercept. Since n is an
integer, the other n are successive integers. The choice of the correct value for ni should
be obtained from a trial plot of (si/ni)2 versus (1/ni2).

The greatest sources of error would arise from the measurements of Δθi and 2θd .

5)

The reflections which are forbidden in kinematical diffraction can occur in CBED
patterns by double diffraction with the addition of symmetry elements due to its
dynamical nature. When two or more equivalent double diffraction paths exist in a given
orientation, the kinematically forbidden reflection that occurs will have a central line of
zero intensity passing through the disk which is Gjonnes-Moodie line.

The screw axis must be perpendicular to the direction of electron beam to allow for the
destructive interference along the central line of the disk to which the beams are
perpendicular. Only in this case would a kinematically forbidden reflection be absent.

Gjonnes-Moodie lines are shown in figure below which are characterized by lines of
dynamic absence due to cancellation of diffraction vectors with equal, but opposite
amplitudes
DB Williams, CB Carter. Transmission Electron Microscopy, Diffraction II, Springer, NY (1996)

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