Austin Shearin pg.

1
MAT 760 Homework 4 Topas and EDX measurements
Using the EDX measurements from the SEM, we can see a list of the possible elements in the
sample we have. The data from the EDX is as follows:
EDX Results
Pre-annealed sample
Copper substrate
Element
Atomic
%
C
5.21
O
66.95
Na
0.31
Mg
0.43
Al
6.81
Si
17.45
S
0.17
K
0.78
Ca
0.14
Ti
0.10
Fe
1.19
Cu
0.46

Silicon substrate
Element
Atomic
%
C
1.22
O
70.68
Na
0.32
Mg
0.44
Al
7.02
Si
17.90
S
0.15
K
0.79
Ca
0.14
Ti
0.10
Fe
1.23

Post-annealed sample
Copper substrate
Element
Atomic
%
C
3.13
O
68.65
Na
0.34
Mg
0.43
Al
7.09
Si
17.80
K
0.77
Ca
0.13
Ti
0.09
Fe
1.25
Cu
0.30

Silicon substrate
Element
Atomic
%
C
1.28
O
67.00
Na
0.32
Mg
0.44
Al
7.74
Si
20.34
K
0.98
Ca
0.18
Ti
0.13
Fe
1.59

Looking at the results, with the very minute percentages of certain elements, I regarded them as
mostly noise. Carbon is hard to justify being in the samples as there is a carbon buildup from
exposure to the SEM. Copper can be eliminated as its only present on the copper substreate. The
largest percentages of elements that I believed were not noise were silicon, oxygen, aluminum,
and iron. Its also safe to assume that with the large amount of oxygen, and since these were
found in nature, that these elements are in the form of oxides. I looked for the (.cif) files for the
molecules of Fe2O3, Al2O3, and SiO2 on the international crystallography database. From the
multiple space groups of each of the molecules, I first looked up which appeared most commonly
in nature and used Mercury software to identify the most intense peaks that corresponded with
the XRD data we have. I used (.cif) files for these space groups of molecules:
Molecule
SiO2
Al2O3
Fe2O3

Space group
P 32 2 1
R -3c
R -3c

Finally, I fitted the XRD data in the Topas Software with the results as follows:
The pre-annealed sample had much more amorphous structure in it so I had to use a much high
order background to get a decent fit. I also excluded the regions before 15 as it was an
amorphous peak and wasnt good for the fitting results. My goodness of fit was 1.43.

Austin Shearin pg. 2

Austin Shearin pg. 3

The annealed sample had much less background and had sharper peaks. I was able to get a much
better fit. My goodness of fit got down to 1.16.

Austin Shearin pg. 4

My phase percentages from the Topas fitting is as follows:
Topas Phase Percentages
Pre-annealed
Molecule
Phase Percentage (%)
SiO2
58.973
Al2O3
39.687
Fe2O3
1.339

Post-annealed
Molecule
SiO2
Al2O3
Fe2O3

Phase Percentage (%)

50.209
36.631
13.160

It can be seen that the EDX atomic percentages correlate to the Topas phase percentages. The
pre-annealed sample had a weaker fit, but the Topas phase percentage for iron oxide matches up
better with the EDX atomic percentage results.
Ive attempted to insert the files I have into my paper below:
unknown
annealed.pro

unknown
pre-annealed.pro

topas output
annealed.txt

topas output
pre-annealed.txt

Topas Results.opj