ENG ME306 Professor Harold Park

Microstructural Analysis by X-Ray and S.E.M.
Section C4, February 7th, 2012

Bonnassieux, Alexandre, Pierre U03371989

the process of scanning electron microscopy. 2. the repetition of group of atoms that exists throughout a crystal forms a three-dimensional grating which can diffract a beam of xrays. These ejected electrons from the samples surface are picked up by a detector. as well as space groups. and the analysis that can be done with these procedures. In crystals.1 X-Ray Diffraction Similarly to the way that an optical grating diffracts light beams.000X whilst maintaining a .2 Scanning Electron Microscope Typical microscopes use a visible light wave source. Another advantage of such a machine is the production of high resolution images. and measurements of residual and applied stress. crystallization. the preferred orientation in a polycrystalline specimen. the condition for the x-ray’s reflection from these planes is (1) Where λ is the wavelength of the x-rays. X-ray diffraction can also provide information concerning the effect on the lattice of plastic deformation. which uses a source of electrons. age hardening and precipitation. mechanism. The underlying principle for all x-ray diffraction application is Bragg’s Law. the pictures formed by the x-ray diffractions can help in determining the spacing of the lattices contained inside the structure. Diffraction will also indicate the orientation of a single crystal. of deposition. The main advantage of an SEM is that it had a much greater depth of focus compared to traditional optical microscopes. in comparison to a scanning electron microscope (SEM). n the order of the reflection. 2 Theory 2. Given a parallel set of planes of atoms which repeat through a crystal (spaced at intervals of d). A beam of x-rays aimed at a specific structure will show a “finger print” of the structure with its diffracted rays. and the constitution of organic and inorganic systems. An SEM can achieve magnifications of 10. transformation. An electron accelerated towards a conductive sample will knock another electron off of the atoms on that surface. and θ the angle of incidence of the beam on the planes . leading to quality images at very high magnifications.Bonnassieux |1 1 Introduction The purpose of this lab is to introduce the basics of x-ray diffraction. The electron beam used by the microscope scans across the sample and the detector is able to transfer the information to a screen. and positions of atoms in the unit cell. the dimensions of the unit cell. This allows for much larger areas to be in focus at the same time.

the data is displayed directly on the nearby computer. After the machine is run. but not used.1 X-Ray Diffraction During the lab demo. 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 an optical microscope generally does not go above 1000X magnification. 3 Methods 3. which is housed behind safety glass. where closer analysis can be made. an x-ray diffraction machine was visited. The reflection rules of xray diffraction for common structures are as follows Table 1 .Bonnassieux |2 relatively good quality focused image.

Some examples of images of fracture surfaces of tensile bars produced by the scanning electron microscope are . but were not actually performed by the lab group.Bonnassieux |3 3. 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.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.

Bonnassieux |4 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 Bragg’s 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 .

Part A To identify the materials that are represented by the charts (found in appendix I-IV).Bonnassieux |5 Figure 2 Two parallel incident rays (1 and 2) make an angle theta with the planes of the crystal. it is necessary to use Bragg’s Law. Solving for the lattice spacing. A reflected beam with maximum intensity will only result if the waves reflected are in phase. This constructive interference will be determined by the unit cell’s dimensions. Braggs Law becomes . so that the crystal structure can be described. This only happens at certain angles that the beams are reflected from the crystal structure as the machine moves around the sample. Question Two Identifying materials from x-ray diffraction graphs is the very important in understanding the functioning of this process. This will only happen is the difference in path lengths is an integer number of wavelength. we can see how the angle values of the reflection relate to the crystal structure of the sample. Using the reflection rules of x-ray diffraction. Braggs law can be manipulated to give (for a cubic unit cell) √ So that the measured value of θ can be related to the cell parameters and the distance between atomic layers in a crystal.

034 3 65 1. For the first graph.4 can also be manipulated to find the spacing of the materials that were analyzed using x-ray diffraction.251 8 77 1.237 9 82 1.434 4 78 1.5 2.174 10 87 1.27 Table 3: Scan #2 Results Radiation (nm) Peak Number Peak Location (2θ) d (A) 1. Radiation (nm) Peak Number Peak Location (2θ) d (A) 1. scan #2. in appendix V.065 2 65 1.157 .540598nm) which is used for λ.25 4 53 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.366 3 40 2. the locations of the peaks were found.079 2 51 1. and then manipulated using the formula above to find the spacing of the crystal structure Radiation (nm) Peak Number Peak Location (2θ) d (A) 1. Similarly.5 1.540598 1 38.434 3 83.224 5 83.3.789 3 74.157 Table 4: Scan #3 Results Radiation (nm) Peak Number Peak Location (2θ) d (A) 1.454 6 71 1. The charts given in the lab (found in appendix V-VIII) give the wavelength of the radiation that was used (1.5 2.540598 1 44 2.56 2 38 2. we can see the Scan#1 fits best with the Titanium.236 2 44.5 1.540598 1 43. we must divide these angles by 2 when plugging them into this equation.540598 1 35 2.326 7 76 1.35 2.726 5 64 1.Bonnassieux |6 Since the angle scale is in 2-theta. We also assume that n=1.5 1.

224 311 5 83.366 200 3 40 2.119 202 Table 6: Scan #1 Results with crystal planes Radiation (nm) Peak Number Peak Location (2θ) d (A) (hkl) 1.35 2. appendix VIII).540598 1 38. The material used in Scan#2 is Austenite (Fe.434 220 4 78 1.726 102 5 64 1.326 103 7 76 1.237 112 9 82 1.5 1. comparing these values to the charts enables us to identify the unknown materials.034 200 3 65 1.Bonnassieux |7 Table 5: Scan #4 Results From the data obtained in the tables above.174 400 10 87 1.157 222 Table 8: Scan #3 Results with crystal planes Radiation (nm) Peak Number Peak Location (2θ) d (A) (hkl) 1. Scan#3 is Aluminum (appendix VII).5 1.C.540598 1 35 2.56 100 2 38 2.25 101 4 53 1.789 200 3 74. appendix VI).251 200 8 77 1.540598 1 43.454 110 6 71 1. and Scan#4 is Iron (Fe.5 2.27 220 Table 7: Scan #2 Results with crystal planes Radiation (nm) Peak Number Peak Location (2θ) d (A) (hkl) 1.157 211 .065 110 2 65 1.434 200 3 83. 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 (2θ) d (A) (hkl) 1.540598 1 44 2.5 1.236 111 2 44.079 111 2 51 1.5 2.

Although the S. which proves to be challenging when trying to magnify small samples with this method. 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. Scan#2 is Austenite and has a face-centered cubic crystal. the limit of the magnification is found in the wave length of the light that is used. and I know feel that I have a basic knowledge of x-ray diffraction as well as the working of a scanning electron microscope. Therefore. we received a good theoretical and visual explanation (using video) of the working of the machine. Scan#1 Titanium. has a hexagonal crystal structure. .M. 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. Since the device magnifies the light reflected on an object. The results of x-ray diffraction were used to identify the unknown metals that were tested. with an optical microscope. 6 Conclusion The objectives of the lab were clearly completed. was not actually used during the lab. 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. and the crystal planes and structure associated with those samples. Scan#3 is Aluminum and has a face-centered cubic crystal structure.E.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.

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

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