ENG ME306 Professor Harold Park

Microstructural Analysis by X-Ray and S.E.M.

Section C4, February 7th, 2012

Bonnassieux, Alexandre, Pierre U03371989

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1 Introduction
The purpose of this lab is to introduce the basics of x-ray diffraction, the process of scanning electron microscopy, and the analysis that can be done with these procedures.

2 Theory
2.1 X-Ray Diffraction
Similarly to the way that an optical grating diffracts light beams, the repetition of group of atoms that exists throughout a crystal forms a three-dimensional grating which can diffract a beam of xrays. A beam of x-rays aimed at a specific structure will show a finger print of the structure with its diffracted rays. In crystals, the pictures formed by the x-ray diffractions can help in determining the spacing of the lattices contained inside the structure, as well as space groups, and positions of atoms in the unit cell. Diffraction will also indicate the orientation of a single crystal, the preferred orientation in a polycrystalline specimen, the dimensions of the unit cell, and measurements of residual and applied stress. X-ray diffraction can also provide information concerning the effect on the lattice of plastic deformation, mechanism, of deposition, crystallization, transformation, age hardening and precipitation, and the constitution of organic and inorganic systems. The underlying principle for all x-ray diffraction application is Braggs Law. Given a parallel set of planes of atoms which repeat through a crystal (spaced at intervals of d), the condition for the x-rays reflection from these planes is (1) Where is the wavelength of the x-rays, n the order of the reflection, and the angle of incidence of the beam on the planes .

2.2 Scanning Electron Microscope

Typical microscopes use a visible light wave source, in comparison to a scanning electron microscope (SEM), which uses a source of electrons. An electron accelerated towards a conductive sample will knock another electron off of the atoms on that surface. These ejected electrons from the samples surface are picked up by a detector. The electron beam used by the microscope scans across the sample and the detector is able to transfer the information to a screen. The main advantage of an SEM is that it had a much greater depth of focus compared to traditional optical microscopes. This allows for much larger areas to be in focus at the same time. Another advantage of such a machine is the production of high resolution images, leading to quality images at very high magnifications. An SEM can achieve magnifications of 10,000X whilst maintaining a

Bonnassieux |2 relatively good quality focused image, which an optical microscope generally does not go above 1000X magnification.

3 Methods
3.1 X-Ray Diffraction
During the lab demo, an x-ray diffraction machine was visited, but not used. The machine is fairly simple to operate, using a computer to start the process after placing the sample into the correct place on the machine, which is housed behind safety glass. After the machine is run, the data is displayed directly on the nearby computer, where closer analysis can be made. The reflection rules of xray diffraction for common structures are as follows

Table 1

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3.2 Scanning Electron Microscope

We were not able to use the SEM in the main demonstration of the lab, as the machines are used by faculty and other researchers to perform experiments and obtain information on microstructure for various samples. The following is a general diagram of the workings of a standard SEM:

Figure 1

4 Results
The results of x-ray diffraction and SEM imaging were given in the lab report, but were not actually performed by the lab group. Some examples of images of fracture surfaces of tensile bars produced by the scanning electron microscope are

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The results of the x-ray diffraction are in forms of graphs, and are attached in appendix I-IV.

5 Analysis
Question One
The basis for x-ray diffraction is governed by Braggs Law (equation 1). A diagram of x-ray diffraction usually looks like the following where it is easy to see why we only get peaks at certain values of theta

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Figure 2 Two parallel incident rays (1 and 2) make an angle theta with the planes of the crystal. A reflected beam with maximum intensity will only result if the waves reflected are in phase. This will only happen is the difference in path lengths is an integer number of wavelength. This only happens at certain angles that the beams are reflected from the crystal structure as the machine moves around the sample. This constructive interference will be determined by the unit cells dimensions. Using the reflection rules of x-ray diffraction, we can see how the angle values of the reflection relate to the crystal structure of the sample. Braggs law can be manipulated to give (for a cubic unit cell) So that the measured value of can be related to the cell parameters and the distance between atomic layers in a crystal, so that the crystal structure can be described.

Question Two
Identifying materials from x-ray diffraction graphs is the very important in understanding the functioning of this process.

Part A
To identify the materials that are represented by the charts (found in appendix I-IV), it is necessary to use Braggs Law. Solving for the lattice spacing, Braggs Law becomes

Bonnassieux |6 Since the angle scale is in 2-theta, we must divide these angles by 2 when plugging them into this equation. The charts given in the lab (found in appendix V-VIII) give the wavelength of the radiation that was used (1.540598nm) which is used for . We also assume that n=1. For the first graph, the locations of the peaks were found, and then manipulated using the formula above to find the spacing of the crystal structure Radiation (nm) Peak Number Peak Location (2) d (A) 1.540598 1 35 2.56 2 38 2.366 3 40 2.25 4 53 1.726 5 64 1.454 6 71 1.326 7 76 1.251 8 77 1.237 9 82 1.174 10 87 1.119 Table 2: Scan #1 Results Comparing the results obtained for the spacing of the sample with the charts that were given in the lab, we can see the Scan#1 fits best with the Titanium, in appendix V. Similarly, scan #2,3,4 can also be manipulated to find the spacing of the materials that were analyzed using x-ray diffraction. Radiation (nm) Peak Number Peak Location (2) d (A) 1.540598 1 43.5 2.079 2 51 1.789 3 74.5 1.27 Table 3: Scan #2 Results Radiation (nm) Peak Number Peak Location (2) d (A) 1.540598 1 38.35 2.236 2 44.5 2.034 3 65 1.434 4 78 1.224 5 83.5 1.157 Table 4: Scan #3 Results Radiation (nm) Peak Number Peak Location (2) d (A) 1.540598 1 44 2.065 2 65 1.434 3 83.5 1.157

Bonnassieux |7 Table 5: Scan #4 Results

From the data obtained in the tables above, comparing these values to the charts enables us to identify the unknown materials. The material used in Scan#2 is Austenite (Fe,C, appendix VI), Scan#3 is Aluminum (appendix VII), and Scan#4 is Iron (Fe, appendix VIII).

Part B
The crystal planes (hkl) associated with each peak can be identified for each scan using the charts provided and tables 2-5 Radiation (nm) Peak Number Peak Location (2) d (A) (hkl) 1.540598 1 35 2.56 100 2 38 2.366 200 3 40 2.25 101 4 53 1.726 102 5 64 1.454 110 6 71 1.326 103 7 76 1.251 200 8 77 1.237 112 9 82 1.174 400 10 87 1.119 202 Table 6: Scan #1 Results with crystal planes Radiation (nm) Peak Number Peak Location (2) d (A) (hkl) 1.540598 1 43.5 2.079 111 2 51 1.789 200 3 74.5 1.27 220 Table 7: Scan #2 Results with crystal planes Radiation (nm) Peak Number Peak Location (2) d (A) (hkl) 1.540598 1 38.35 2.236 111 2 44.5 2.034 200 3 65 1.434 220 4 78 1.224 311 5 83.5 1.157 222 Table 8: Scan #3 Results with crystal planes Radiation (nm) Peak Number Peak Location (2) d (A) (hkl) 1.540598 1 44 2.065 110 2 65 1.434 200 3 83.5 1.157 211

Bonnassieux |8 Table 9: Scan #3 Results with crystal planes

Part C
The crystal structures can be determined with the help of the reflection rules of x-ray diffraction found in table 1 and the charts given. Scan#1 Titanium, has a hexagonal crystal structure. Scan#2 is Austenite and has a face-centered cubic crystal, Scan#3 is Aluminum and has a face-centered cubic crystal structure, and Scan#4 is Iron and has a Body-centered cubic crystal structure.

Question Three
Optical microscopes must have a perfectly flat surface to get a food focused image at high magnifications, which proves to be challenging when trying to magnify small samples with this method. The limitation of light microscopes, and the reason why we cannot use a light microscope to look at the microstructure at very high magnifications is because of its use of light. Since the device magnifies the light reflected on an object, the limit of the magnification is found in the wave length of the light that is used. Therefore, with an optical microscope, it is not possible to magnify objects that are smaller than the shortest wavelength of visible light (around 400 nanometers) since the object cannot reflect the visual light due to its size and will consequently be virtually invisible to the microscope.

6 Conclusion
The objectives of the lab were clearly completed, and I know feel that I have a basic knowledge of x-ray diffraction as well as the working of a scanning electron microscope. The results of x-ray diffraction were used to identify the unknown metals that were tested, and the crystal planes and structure associated with those samples. Although the S.E.M. was not actually used during the lab, we received a good theoretical and visual explanation (using video) of the working of the machine.

Bonnassieux |9 Sources: http://web.pdx.edu/~pmoeck/phy381/Topic5a-XRD.pdf