X-Ray Diffraction Austin Williams Section 5 Mechanical Engineering Department, Louisiana State University Instructor: Bahador Farshchian ABSTRACT

This lab is important because it shows how different crystal structures in metals respond to x-ray diffraction. By analyzing where peaks occur in the Intensity v. 2theta graph and understanding why these peaks happen, engineers are able to determine lattice constants of the metals and also find defects in the metals. To better understand these properties, an experiment was conducted using samples of Aluminum and Stainless Steel. Both metal samples were placed, individually, in an xray diffractometer and the data from this experiment was used to make calculations and conclusions about each metal. For each sample, an average lattice constant was found and the interplanar spacing for each Miller indices was found as well. Knowing that each peak was a result of constructive interference, the data was analyzed for two different crystal structures: BCC and FCC.

Table of Contents

INTRODUCTION Forensic science in todays world is a very important and studied field. Creating stronger and lighter materials while also being price effective is one of the many challenges forensic scientists face in present time. For any of these studies or research opportunities to happen one must know the properties of the materials being worked with. For an engineer to make decision on using a certain material over another or even to combine separate materials, the structure of the material is key to understanding the process needed and what to expect from this combination. The rest of this lab report will contain the methods used during lab time that resulted in the given data seen in the results section of the report. Each step taken during lab will be documented and detailed so that others may be able to reproduce the experiment exactly the same and get exactly the same results. Once these have been seen, there will be a discussion and a conclusion summarizing the lab and also discussing what the results mean and how this is useful for others.

THEORY Three basic crystal structures encountered in metallic materials are the BodyCentered Cubic (BCC), Face-Centered Cubic (FCC) and Hexagonal Close-Packed (HCP). X-ray diffraction techniques can be utilized to identify the structure of various materials. If the x-rays hit the metal and it reflects rays back then this is called constructive interference at this particular angle. Braggs Law expresses the relationship between the wavelengths of the diffracted light and the interplanar spacing of the crystal planes: n = 2dhkl sin The Interplanar Spacing between two closest parallel planes with the same Miller Indices can be determined as dhkl = a (h2 +l2 +k2)0.5 where "a" is the Lattice Parameter. These equations can be used to represent the wavelength as a function of the lattice parameter; which can be used along with Xray diffraction data to determine if a cubic crystal structure is FCC or BCC. Diffraction occurs only on planes whose Miller indices when added together (h + k + l) total to an even number when dealing with BCC, while for FCC crystal structure, the principal diffracting planes are those whose Miller indices are either all even/odd (zero is considered even).

PROCEDURE There were not many materials required to complete this lab. To fully reproduce the results that will later be displayed there are only four things one must have to successfully do so. The first thing one needs to conduct this experiment is a X-ray diffraction machine. Once this has been procured software must be downloaded onto a computer so that data from the machine can be read. The basis of the experiment lies in the samples used, so one must also have a sample of Aluminum and Stainless Steel to carry out the procedures. Once these materials have been gathered the actual procedural part of the experiment must begin. The first step is to turn on your computer and open the program that runs with the x-ray diffractometer. After this has been done the x-ray diffractometer must then be turned on. After turning on the machine carefully read all instructions given by lab instructors and then take the sample out of its plastic/container. Be sure that the red warning light is not on before you open the door on the machine to ensure that you are not exposed to harmful x-rays. Once you are certain that it is safe to open the door (based on instructions), change whatever settings you need to on the machine and then place the first sample into the machine. Close the door of the machine and turn the x-ray function on. Once this has been done watch the computer program plot the Intensity vs 2theta graph while waiting for the experiment to finish the first sample. After the machine has stopped and the red light is off, open the door and extract the sample. Record the data from the experiment and repeat all these steps over for the second sample.

Results

Intensity Vs. 2
160000 140000 120000

Intensity

100000 80000 60000 40000 20000 0 20 30 40 50 60 70 80 90 100 110 120

Figure 1. Plot of intensity versus 2 for FCC aluminum

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Figure 1. Plot of intensity vs. 2theta for FCC Aluminum Figure 1 shows the plot of Intensity vs 2 for the FCC structured aluminum sample. The diffraction process began at 10 degrees and was stopped at 60 degrees. There were 4 peaks total for the FCC aluminum sample. The sample starts with a small intensity of the diffracted beam that slowly decreases. Next the intensity has a peak at about 19 degrees followed by another peak at about 27.5 degrees. The intensity drops back down and peaks two more times around 41 and 49 degrees.

Intensity Vs. 2
4500 4000 3500 3000 2500 2000 1500 1000 500 0 20 30 40 50 60 70 80 90 100 110 120

Intensity

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Figure 2. Plot of intensity vs. 2theta for BCC stainless steel

Figure 2 shows a plot of Intensity vs. 2theta for the BCC structured stainless steel. There are a total of 5 peaks for stainless steel compared to the 4 for aluminum. Just as with the Aluminum sample, 2theta ranges from 20-120 degrees. The overall behavior of the graph shows the intensity starting at a low value and gradually increasing over 2theta. The first peak occurs at around 22 degrees and after that all of the other 4 peaks have a lot smaller intensity. These four peaks occur at about 32.5, 41, 44.5, and 58 degrees.

Figure 3. Chart showing data collected from FCC Aluminum sample

Figure 4. Chart showing data collected from BCC Stainless Steel sample Figures 3 and 4 are charts that show the exact values for the intensity and 2theta at which the peaks occurred in the FCC aluminum sample and the BCC steel sample. Once the planes that caused the peaks in each sample were determined, other properties such as lattice parameter and interplanar spacing could also be calculated. The average lattice parameter for FCC aluminum is 0.287 nm and the average lattice parameter for BCC stainless steel is 0.406 nm.

Discussion Fully understanding the results of this lab requires one to be able to manipulate the data with equations. The most important equation used was Braggs Law. The key fact to know is that order of diffraction and wavelength are constants throughout the entire experiment. This is the case because n (the order of diffraction) is assumed to be one and the wavelength remained constant. With these two terms constant, one is able to determine where peaks will occur after the first angle of diffraction has been found. Braggs law can also be used to calculate interplanar spacing, and from that one can then calculate a (lattice parameter). The lattice parameter is a good measure of error for this because it must be constant. Therefore if one plane has a different lattice parameter than another one may assume and error was made. Planes that cause the highest peaks will appear more frequently parallel to the surface since the higher the intensity, the more preferred orientation it is. The highest preferred orientation for FCC was the (200) because it was the highest peak, occurring at 44.6 degrees. There was also another high peak for FCC and tht was at 38.2 degrees with the (111) plane. BCC however only had on strong peak and that occurred at 44.6 degrees, making it pair up with the (110) plane. The fact that no other BBC peaks were near the magnitude of the 44.6 degree peak, that make it the 100% preferred orientation.

Conclusion X-ray diffraction is a very useful tool when attempting to learn more about a metals crystal structures. By using the Intensity vs. 2theta graph and the equations given (Braggs law, Interplanar spacing equation), one can calculate what planes in FCC and BCC structures cause diffraction. For each sample, an average lattice constant was found (0.287 nm for FCC aluminum and 0.406 nm for BCC stainless steel) Knowing that each peak was a result of constructive interference the data was analyzed for two different crystal structures, and the interplanar spacing for each Miller indices was found. It was then be concluded that the highest preferred orientation for FCC are the (200) and (111) planes and (110) plane for BCC.