M ICROSTRUCTURAL DESIGN AND CHARACTERIZATION OF INORGANIC

MATERIALS

CHIM-H-412

Electron diffraction and microscopies

Students:
Teachers:
D E P ELSMAEKER Casper
L EFEVER Gerlinde
M ANGIALETTO Jessica
S HARMA Ravi

D ELPLANCKE Marie-Paule
G ODET Stphane

November 8, 2016

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Introduction

The objective of this experiment is to get familiar with the use of electron diffraction patterns
for the structural characterization of materials by using transmission electron microscopy, in
which exists a correlation between the image and the electron diffraction patterns.

2
2.1

Experimental
Analysis in situ, with TEM Philips CM20, of the electron diffraction pattern
of a nanometric crystalline powder in order to identify it. Relate in details the
different steps of your analysis.

A TEM microscope can be used to analyze a sample in 2 significant ways. Firstly the microstructure of the sample can be determined by first letting the electron beam pass through
the sample and afterwards through an aperture. When this is done the particles in the sample
will scatter the incident electron beams making the beam no longer coherent. Because of this
the aperture will eliminate these incoherent scattered beams. This will cause a dark spot of low
intensity on the otherwise bright background. At the end, an image will be obtained showing
all particles as dark spots and hereby giving an idea of the microstructure.
To accompany this analysis of the microstucture an EDX can be build in the microscope to analyse the chemical composition of the observed image. This is done by detecting the X-rays emitted by the excited atoms of the sample. Each element will emit X-rays with a certain amount
of characteristics energy levels. Because of this the different peaks on the EDX spectrum can
be assigned to different elements which make up the composition of your sample. However,
the EDX will not give any idea about the relative amount of these elements. Using this method
on the nanometric crystalline powder that was given, an EDX spectrum was obtained. The
spectrum obtained in figure 1 shows that Th and Cl were the major elements identified in the
sample.
A second way to analyze a sample with a TEM is by obtaining its diffraction pattern. This can
be obtained by putting the aperture in the back focal plane of the objective lens. In this plane
the diffracted beams will produce bright spots while the background will be black because the
unscattered beam is eliminated. Because the beams that are diffracted have to fulfill Briggs
law, these spots will be at discrete locations which are linked to specific Miller planes. These
locations will either be rings or spots depending on whether a polycristal or monocristal respectively is analyzed.
The diffraction pattern obtained through this method can be analyzed either by hand or with
the software built in the TEM. The distance on this pattern can be directly related by both methods to the interplanar distance d. The method for measuring the interplanar distance by hand
is further explained in the second part. For the analysis with the TEM a built-in measuring
equipment can be used, as shown in figure 2. After analyzing this pattern for the nanometric crystal powder sample several interplanar distances were obtained. For the four analyzed
rings the interplanar distances d were, from the center outwards:
d1 = 404pm
d2 = 283pm
d3 = 199pm
d4 = 161pm

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Using these distances and with the knowledge that our sample was composed of Th and Cl, the
complete identification of the sample could be done. For this the obtained data was compared
to the reference material. The first book contained tables of compounds with their most prominent interplanar distances while the second book contained more detailed information listing
all of the interplanar distances. After finding a possible compound in the first book by looking
at the elements found by EDX, a reference for this compound for the second book is given.
There, the measured interplanar distances d can be compared to the distances mentioned by
the reference.
After comparison with the reference, the nanometric powder sample was identified to be ThCl.

2.2

Analysis of electron diffraction patterns of crystal A obtained on a thin aluminum foil.

To analyze the electron diffraction patterns of crystal A, as shown in the figure 3, the distance
between the spots has been measured, by choosing one spot as (0,0,0). The values of the R and
the angle phi is shown in figures 7 and 8. And with same diffraction constant, the proportion
between the distances R1, R2 and R3, which will be same as the proportion between the interplanar distance d1, d2 and d3 as shown by the formula in figure 4. And with the angles
between each vector measured, the family of plane was derived, with the help of tables provided during the laboratory session.
For the crystal A, the family of planes (h,l,k) calculated was found to be: (1,1,-1); (1,1,1); (2,2,0).
To validate that the planes found were correct, coherent indexation was applied by calculating
the angles in between the planes and validating with the values of angles found in figure 3.
The formula for the coherent indexation is shown in figure 5.
The zone axis was calculated by the cross product of two planes, i.e., (1,1,-1) x (1,1,1) = (2,2,0). And to calculate the diffraction constant , knowing that aAl = 0.404nm, with the formula
presented in figure 6, the interplanar distances d are calculated.
d1 = 0.233nm
d2 = 0.233nm
d3 = 0.143nm
And by the formula shown in figure 4 the diffraction constant will be R*d = 0.396 cm*nm.

2.3

Does the electron diffraction pattern C correspond to a ferritic steel or to an

austenitic steel? Justify your answer, using the crystallographic software CARINE
and perform a complete indexation of the pattern.

To start, the R and values of crystal C are measured. The obtained values can be found in
table 9 and will be used in the crystallographic software.
In order to find the crystal structure corresponding to crystal C, both the FCC and BCC structure are matched with the values found for R and . It was seen that for an FCC structure, the
error on the -value was about 20o , which indicates the wrong choice of crystal structure. A
match between measured crystal parameters and a BCC structure was found. The sample is
thus a ferrite steel.
Afterwards, the (h,k,l) planes were found, being: (1,1,0);(1,1,0);(2,1,1). The zone axis is then
calculated and found to be (1,-1,-1).

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2.4

Measure the relative disorientation between the image and the electron diffraction pattern with the method proposed by Alderson and Hillary, using a MoO3
particle.

In order to measure the relative disorientation between the image and the electron diffraction
pattern, the ratios of the interplanar distance (d) of the electron diffraction pattern and the ratios
of the different R on the image were compared. It is known that if the ratio of the interplanar
distances and the ratio of the R are the same, they correspond to the same couple of planes.
IN this way it can be determine to which plane corresponds each direction of the diffraction
pattern.
By considering the direction of the plane (0,0,1) of the crystal and the direction (0,0,1) in the
diffraction pattern, shown in figure 10, the rotation angle is of 22 degrees.

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Figure 1: EDX spectrum of the nanometric crystal powder.

Figure 2: Diffraction pattern of nanometric crystal powder. An arrow is used to estimate the
interplanar distances.

Figure 3: Image Crystal A.

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Figure 4: Relation between R and d .

Figure 5: Coherent indexation.

Figure 6: Formula for calculating interplanar distance.

Figure 7: Values of R calculated through the image provided during the lab session.

Figure 8: Values of phi calculated through the image provided during the lab session.

Figure 9: Measured values of R and for crystal C.

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Figure 10: Relative disorientation calculated by Alderson and Hillary method for a MoO3 particle.