Image Enhancement of Polycrystalline Aluminum Electron Diffraction Patterns Paul Larsen William Stratton ECE 533 Final Project December 12, 2003 Introduction Transmission electron microscopy (TEM) is an essential part of materials characterization. Following L. de Broglie’s dual character theory, stating that particles can be considered as waves, it was discovered the electron has a wavelength one hundred thousand times smaller than visible light for an accelerating potential of 60 kV [1,2]. This smaller wavelength of the electron meant that electrons could image a specimen at a much smaller resolution than any form of visible light. In 1931, Knoll and Ruska, working at the Electrotechnical Institute of the Technological University-Berlin, developed the first two-lens electron microscope. Siemens and Halske Company in Germany first commercially manufactured this new invention in 1938. Today’s TEMs work very similarly to the earlier versions. Using an electron source (usually either a tungsten wire or a LaB6 crystal filament), electrons are boiled off and accelerated to ~70% the speed of light along an optic axis of column under high vacuum. These accelerated electrons are focused by a series of positive acting magnetic lenses (figure 1), and coherently sent through an electron transparent Optic Axis sample. Electron transparency Ray 1 Ray 2 usually refers to specimens being hundreds of Å thick. The electrons interact with the sample and are Lens 1 projected onto a viewing screen. Imaging electrons can either be viewed in imaging or diffraction Back Focal Plane mode. Imaging mode in a TEM is probably the first type of sample viewing thought of by most people. Lens 2 The electrons pass through the specimen producing an image Ray 2 Ray 1 similar to an image of a broken bone taken by x-rays at a doctor’s office. Crystals, impurities, and dislocations Figure 1: Simplified ray diagram of a typical in the sample all interact with the TEM. The specimen would be placed above electrons differently, therefore lens 1. Electrons travel through the positive generating an image with both high lens 1, crossover at the back focal plane, and and low contrast areas. Using then continue through lens 2 to a viewing images made by basic scattering, screen. Diffraction patterns of specimens are one can determine crystal size, viewed at the back focal plane. defect type, and defect size. Diffraction mode can be thought of as the frequency domain representation of the aforementioned projected image. Formed at the back focal plane of the TEM, the diffraction pattern can give information on crystal structure, basic composition, and lattice parameters. Various diffraction patterns can be seen in figure 2. Single crystal samples generate a symmetric array of spots, polycrystalline samples generate an array of concentric circles, and amorphous samples generate concentric fuzzy rings. In a single 2 crystal diffraction pattern, the angle between the spots and the central beam (central beam being at the vertex of the angle) is the angle that is between those reflecting planes. While the distance from the center spot of the pattern to a feature, either a spot or ring is proportional to the inverse of the distance between atomic planes of that feature. For example, if a spot or ring corresponds to the {111} set of planes in a crystal lattice and the distance from the spot to the feature is 2 cm, the spacing between the {111} planes will be ξ * (1/2) cm-1, where ξ is the camera constant for the microscope [2,3]. Figure 2: Diffraction patterns of an A1 single crystal, polycrystalline gold, and amorphous carbon respectively [3]. Diffraction patterns are generated in accordance with Bragg’s Law (equation 1 and figure 3). n 2d sin (1) Where n is an integer, λ is the wavelength of the electron used for imaging, d is the distance between two rows of atoms, and θ is the angle of reflection for the electron waves. When a group of atoms is oriented at a Bragg condition (meaning the electrons are reflected coherently), a bright spot will appear in the diffraction pattern, compared to no generated spot when aligned out of the Bragg condition. This is how the various rings and spots are generated in the diffraction patterns in figure 2. Incoming coherent electron waves (λ) d Outgoing coherent electron waves θ Figure 3: Visual representation of Bragg’s Law, the dotted lines represents electron wave paths while solid lines represent rows of atoms. Incoming electron waves scatter coherently off columns of atoms, this coherence generates a bright spot in the diffraction pattern. Generally, the intensity of the diffraction patterns is proportional to the number of electrons that can pass through the specimen. Hence, the intensity is dependent upon the 3 thickness of the sample, assuming constant electron brightness. Thicker samples allow only the central spot and a few other features to be visible, while thinner specimens allow for more detail to be shown in the diffraction pattern. In both cases, however, the outermost features are often lost due to the drastic difference in intensity between the central spot and the outer features (rings or spots). The resulting loss of information creates a problem for the analysis and presentation of the diffraction patterns. Approach Kirkland has suggested using digital image enhancement to make the lower intensity portions of the diffraction patterns more visible and thereby extract as much data as possible [4]. Researchers having little image processing background often apply standard techniques in a trial-and-error fashion, which is often both ineffective and timeconsuming. For this project, we propose to develop a more concrete methodology for digital enhancement of diffraction patterns. By applying image enhancement techniques to a plethora of digitally captured diffraction patterns, we will identify those techniques that are generally most effective for a given diffraction pattern, thereby assisting researchers to apply image enhancement in a more systematic fashion. Experimental Digital diffraction images were obtained with the LEO 912 EFTEM at the Materials Science Center at the University of Wisconsin – Madison. The TEM was operated with an accelerating voltage of 120 kV, and has a spatial resolution of 16 Å. Images were acquired in 8-bit TIFF format by AnalySIS ESIvision image acquisition software. A polycrystalline aluminum standard diffraction pattern manufactured by Ted Pella Incorporated was used for the diffraction patterns. This type of polycrystalline sample generates a diffraction pattern with multiple concentric rings about a bright central spot. A beam blocker was used as to not damage the CCD camera from the high intensity electrons traveling down the optic axis. Multiple images at varying exposure times were taken, some with the bright central spot in the center, and some with the image shifted to allow some of the dimmer rings of the diffraction pattern to be imaged. Table 1 gives the combinations of exposure time and shift level for which images were acquired. Exposure Time Table 1. Combinations of Exposure Time and Shift Level for which Images were Acquired. 50ms 100ms 500ms 1000ms 5000ms 10000ms 20000ms 30000ms _________________Shift Level__________________ _0_ _1_ _2_ _3_ x x x x x x x x x x x x x x x x x x x x x x x 4 The acquired images were each subjected to a power-law transformation, a log transformation, and histogram equalization to enhance the lower intensity portions of the diffraction pattern. The equations for the power-law and log transformations are, respectively, s c r (2) s c log( 1 r ) (3) where c and γ are constants and r is the original pixel value. The value of c is computed by first performing the transformation for c = 1, giving the output values s’, and then letting c = max(s’)-1 such that subsequent application of the transform gives output values that span the entire range of gray values. Histogram equalization is achieved by mapping each original pixel with level rk into a corresponding pixel with level sk using k n j (4) sk j 0 n in which nj is the number of pixels with gray-level rj and n is the total number of pixels in the image. A median filter was also applied to each image to remove salt-and-pepper noise. Finally, the images were visually inspected to determine which transform provided the best contrast to the outer rings generated by the polycrystalline Al standard. All image processing was done with the computer program Matlab. Results Table 2 gives the transformations that resulted in the best image enhancement for each image. Although not mentioned explicitly in the table, there are two operations that should be performed in addition to the power-law and log transformations in Table 2. First, the constant c shown in Equations 2 and 3 should be calculated as explained in the Experimental section. Second, the median filter should always be performed following each transformation. Table 2. Transform Giving the Best Enhancement for Each Image. ___________________________Shift Level_____________________________ _______0______ _______1______ _______2______ _______3______ 50ms Exposure Time 100ms Log or Power-law with γ = 0.3 Log or Power-law with γ = 0.3 500ms 1000ms 5000ms 10000ms 20000ms 30000ms Log or Power-law with γ = 0.3 Power-law with γ = 0.4 Power-law with γ = 0.4 Log or Power-law with γ = 0.3 Log or Power-law with γ = 0.3 Log or Power-law with γ = 0.3 Power-law with γ = 0.5 Power-law with γ = 0.45 Power-law with γ = 0.45 Power-law with γ = 0.4 Power-law with γ = 0.35 Power-law with γ = 0.35 Power-law with γ = 0.35 Power-law with γ = 0.55 Power-law with γ = 0.55 Power-law with γ = 0.55 Power-law with γ = 0.55 Power-law with γ = 0.5 Power-law with γ = 0.4 Power-law with γ = 0.4 Power-law with γ = 0.35 5 The value of γ used for the power-law transformation was determined in a trial-and-error fashion with the objective of minimizing noise without losing information. The result of applying these “best” transformations are given for a few of the images in Figures 4-7. original power-law with median filter, gamma = 0.3 Figure 4. Result of applying power-law transform on image for 50 ms exposure time and zero shift. original power-law with median filter, gamma = 0.4 Figure 5. Result of applying power-law transform on image for 1000 ms exposure time and one shift. 6 original power-law with median filter, gamma = 0.4 Figure 6. Result of applying power-law transform on image for 5000 ms exposure time and two shifts. original power-law with median filter, gamma = 0.4 Figure 7. Result of applying power-law transform on image for 10000 ms exposure time and three shifts. Discussion Median Filter The median filter should be used always because it greatly enhances lower exposure time images and does no harm to higher exposure time images, as shown in Figures 8 and 9. Histogram Equalization Histogram Equalization should not be used because it usually gives results that are considerably less desirable than the log and power-law transformations and never gives results that are noticeably better. This fact is also seen in Figures 8 and 9. 7 a) histogram equalization for 50ms s hift0 b) histogram equalization and median filter c) log transformation for 50ms s hift0 d) log transformation with median filter Figure 8. Effect of median filter for low exposure times (50 ms and zero shift). 8 a) histogram equalization for 1000ms s hift0 b) histogram equalization and median filter c) log transformation for 1000ms s hift0 d) log transformation with median filter Figure 9. Effect of median filter for high exposure times. Log Transformation Log transformations give basically the same results as power-law transformations with γ = 3. The only difference is that the log transformation displays the outer rings with slightly better contrast while the power-law transformation gives better contrast for the inner rings, as seen in Figure 10. The difference is nearly imperceptible, such that there should not ever be a need to apply the log transformation. 9 log transformation for 5000ms s hift1 power-law with gamma = 0.3 Figure 10. Comparison of log transformation and power-law transformation with γ = 0.3. Power-law transformation The foregoing discussion establishes that the power-law transformation achieves either the best or very close to the best enhancement under all circumstances investigated. The focus should therefore be not on the type of transformation to employ, but rather on which value of γ gives the best enhancement. To this end, the values given in Table 2 serve as a guide to the best values of γ for a given exposure time and shift level. References 1. Hall, C. E., Introduction to Electron Microscopy, Robert Krieger Publishing Co., Malabar, Florida, 2nd edition, reprinted, 1983 2. Class Notes for MSAE 748 – Structural Analysis of Materials, Spring 2002, University of Wisconsin – Madison, Dr. Babcock, notes prepared by Dr. T.F. Kelly 3. Williams, David, Carter, C Barry, Transmission electron microscopy, Plenum Press, New York, 1st edition, 1996. 4. Kirkland, Earl, Advanced computing in electron microscopy, Plenum Press, New York, 1st edition, 1998 10 Tasks Planning Experimental & Analysis Writing/Presentation Overall Team Members Percent Contribution William Stratton Paul Larsen 50 50 50 50 50 50 50 50 11