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MTRL 451

Progress Report

Author:
Miayan Yeremi

Student #:
18213074

November 2, 2015

The Original Goal

We were given a rock with different minerals materials in it. We were asked to analyze the rock
and determine how many different solid material phases there are in the rock. In addition, we
were required to analyze the different phases on the rock, using optical microscope (OM), scanning
electron microscope, energy dispersive X-ray spectroscopy, and X-ray diffraction. These methods
are being used to determine exactly what these phases are made out of, and if these materials are
valuable.

Background/Experiments and Results

We have taken many steps in the process of answering what the rock we were given is made out of.
To date we have completed four of the five labs needed to completely identify the composition of
the rock. In this section, I will give a background to the techniques we used in these labs and some
of the results we have collected over the 4 labs.

2.1

Sample Preparation Lab

After close observation of our rock we concluded that the rock had three distinct phase. Using visible
light why identified these phase by colours. Our rock has a white grey phase, a gold white phase,
and a dark grey phase. We took a picture with the optical microscope that distinctly highlights
the three phases, see Figure 1. This lab was very important the results of this lab would affect all
the following labs. We were instructed to prepare three different specimens: a powder specimen for
X-ray diffraction lab, a small rock chunk specimen for SEM, and a polished flat carbon medium
embedded specimen for OM and EDS (note, we ensured all three phases were included in all the
specimens). The hardest specimen for preparation was the polished flat specimen. We had to make
sure the sample was as close to flat as possible, because if it was not this would lead to a sample
with varying working distance, which would affect the focus on different regions of the specimen.

2.2

Optical Microscopy Lab

Optical microscope offers a quick and relatively cheap (i.e. when compared to the other techniques
we are using) method of analyzing our sample. It uses visible light to see the sample so the colours
we see using this microscope are the same colours we examine with our eyes. The optical microscope
does not need a vacuum to operate so it is rather versatile in the samples it can except. Its major
disadvantage is low resolution due to visible light diffraction limit. This translates into a maximum
resolution of usually a micron to a few hundred nanometers.
In this lab we mainly explored the affect of changing the numerical aperture (NA) on the
resolution of the optical microscope. The NA of an objective lens is defined as follows,
NA = sin,
where is the lenss refractive index, and is the refractive index of the lens. The resolution of
the OM is affected by the numerical aperture in the following manner,
r=

0.61
,
NA
1

Table 1: OM Objective lenses details


Lens label
1
2
3
4

Lens NA
0.15
0.30
0.45
0.80

Lens Magnefication
5
10
20
50

where r and are the resolution and wavelength of the light, respectively. We used four different
objective lenses that had a built in NA and magnefication. Table 1 shows the NA and magnification
for each lens.
I digitally zoomed all four of lenses pictures to a similar magnification to illustrate the difference
in resolution, see Figure 2. Theoretically speaking the resolution should sequentially increase from
lens 1 to 4 because the NA is increasing. This trend is seen from the Figures 2a-2c. Figure 2d has
less pixelation than the rest of the figures, but the features in the image are not as sharp as some
of the other images. This leads me to believe we did not focus lens 4 sufficiently before taking the
image.

2.3

Scanning electron Microscopy Lab

In this lab we used two of SEMs major signals, the secondary electron (SE), and the backscattered
electron (BSE). Each one of these signals provides different information about the sample. Each of
the signals resolution is influenced by the same factors such as, interaction volume, Atomic number
and density of the specimen, beam size and energy, working distance, etc. BSE has a higher energy
in comparison to SE, which means it explored more of the interaction volume. This reduces the
resolution of BSE when compared to SE. BSE is more sensitive to the density of the specimen so
it give information about the density composition of the sample. SE has a high resolution of up
to a nanometer so it offers information about morphology, and topography of the specimen. BSEs
resolution is on the order of micrometers. Figure 3 shows BSE image of the same region as in Figure
1. Figure 3 gives a qualitative difference in density of the three phases. Figures 4a and 4b, show
the same region with all resolution factors set equal, except for Figure 4a is a SE image, and Figure
4b is a BSE image.
In this lab we experimented with the different parameters that influence the resolution of the
SEM such as working distance, and beam energy. We also experimented with different magnifications. Lastly, SEM offered many advantages when compared to OM in terms of more information
about the density of the phases, better detailed morphology and topography, higher resolution.
The main disadvantages of SEM are that the process takes longer than OM, it is a more expensive
setup, and the samples that SEM can take in are less versatile when compared with OM.

2.4

Energy Dispersive Spectroscopy Lab

Energy dispersive spectroscopy (EDS) is an additional detector attached to SEM that utilizes Xrays produced by electron beam specimen interaction. High energy electrons hit the sample and
knock out an electron from the inner shell of the element. Next, an electron from a higher energy
shell drops down to fill the vacancy, and in the process emits X-ray radiation detected by EDS. In
most cases this radiation has a unique energy signature, allowing for identification of the element in
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the sample and their relative abundance in the specimen. In some situations there is overlap in the
X-ray spectrum peaks, which can cause trouble distinguishing between elements. This problem can
usually be resolved with the help of X-ray diffraction, which gives information about the crystal
structures of the specimen.
Using EDS, we have determined a lot of information about the composition of our rock. Figures
5, 6, 7 are EDS spectrums of the white, light grey, and dark grey phases, respectively (note, Im
using the colour labels for the phases as seen in Figure 3). The white phase seems to have Lead (II)
sulfide (PbS) in it. The light grey phase seems to be Iron (II) disulfide (FeS2 ), also called pyrite,
or fools gold. The pyrite phase is golden in the OM image (i.e. Figure 1), which is what we would
expect. Lastly, the dark phase seems to have silicon dioxide (SiO2 ) in it. This phase seems to be
silica, but I would expect the silica to be transparent, which it does not seem to be when looked
at with the OM, see Figure 1. This might be explained by the fact that we are seeing the carbon
substrate through the silica, but I am not convinced of this yet. We worked out the stoichiometry
of the molecules using the relative atomic weight information given by the EDS software.

Future Plans

We plan on using X-ray diffraction (XRD) to confirm our EDS results. Our white phase also seem
to detect Molybdenum at zero relative concentration. We need to use XRD to figure out the crystal
structures of the phases, which will help us figure out exactly what the compositions of the phases
are, and eliminate any discrepancies noted earlier.

Appendices

Figure 1: Three phases found in our rock sample (this picture was taken using OM).

(b) lens 2, NA 0.3

(a) lens 1, NA 0.15

(c) lens 3, NA 0.45


(d) lens 4, NA 0.8

Figure 2: comparison of resolution using different objective lenses

Figure 3: BSE overview of the three phases.

(a) SE image

(b) BSE image

Figure 4: comparison of SE and BSE images

Figure 5: white phase EDS spectrum

Figure 6: light grey phase EDS spectrum

Figure 7: dark grey phase EDS spectrum