Microelectronics-Photonics Graduate Program Research Experience for Undergraduates Summer 2007 Final Research Report Metal Induced Crystallization of Amorphous Silicon Using an Electron Beam Benjamin Newton Dr. Hameed Naseem, Electrical Engineering Dr. Husam Abu Safe, Electrical Engineering Mrs. Dorinne Bower, Microeletronics-Photonics July 26, 2007 This work was supported by National Science Foundation award EEC-0097714. Any opinion, findings, and conclusions or recommendations expressed in this Material are those of the author and do not necessarily reflect the views of the National Science Foundation. 1 Benjamin Newton, University of Arkansas Pine Bluff Faculty Mentor: Dr. Hameed Naseem, Electrical Engineering Post doc Mentor: Dr. Husam Abu Safe, Electrical Engineering Graduate Student Mentor: Mrs. Dorinne Bower Metal Induced Crystallization of Amorphous Silicon using an Electron Beam Activities: Amorphous silicon is commonly used in the production of photovoltaic cells and thin film transistors. We investigated the effectiveness of using an electron beam in the process of metal induced crystallization. Various annealing times, spot sizes and accelerating voltages, were used to find the most effective method of using an electron beam to induce crystallization. Findings We found that the electron beam did change the morphology of the surface of the substrate, but that the source we used for our electron beam may not be powerful enough to give us more defined results. The crystals that may have been produced were on the order of nanometers and the substrate was at least a square meter of surface area. We believe this may be the reason the XRD could not detect any crystallization although we saw a definite change in the surface of the material. We find that an electron beam can be used for metal induced crystallization, but the spot size of the beam or an area of multiple spots needs to be crystallized in order for the XRD to detect crystallization. Planned Publications 1. No planned journal publications at this time 2. Student presentation for Microelectronics and photonics on July 25,2007 Key Illustration /Figure Figure 1 Four spots 10 microns apart created by an electron beam from top to bottom they were 30 kv spot size 5 ,20 kv spot size 5, 10 kv spot size 4, 30 kv spot size 1. All of the annealin times were for 30 minuts except for the last which was an hour. 2 Table of Contents 3 List of Figures 4 Abstract 10 Introduction and Background 11 Research goals 11 Description of Experiment 11 Experimental Results and Conclusions 12 Future Research Suggested by this Research 12 Appendix A: List of References 12 Appendix B: Intellectual Property-Commercialization Value 12 Appendix C: Impact of Reu on Personal Goals and Plans 12 Acknowledgements 13 3 Figure 1 Four dots 10 microns apart created by an electron beam from top to bottom their beam strengths and spot size are 30 kv spot size 5, 20 kv spot size 5, 10 kv spot size 4, 30 kv spotsize 1. 4 Figure 2 This is the 30 kv dot spot size 5 for 30 minutes. Definite change in the surface. 5 Figure 3 This is the 20kv dot spot size 4 for 30 min. There appears to be some formation of a substance at the center of the spot. 6 Figure 4 This is the 10 kv dot spot size 4 for 30 min. There appears to be a formation of some substance at the center of the spot. Figure 5 The first site annealed on the surface of the copper transmission electron microscope grid. It was annealed for 15 minutes at 20kv spot size 4. 7 Figure 6 Closer picture of first annealing site . Figure 7 Second annealing site was annealed for 15 minutes at 30 kv spot size 4 8 Figure 8 On the left is the crystallization and on the right is an uncrystallized portion of the substrate from the TEM grid. 9 Abstract Amorphous silicon is commonly in the production of photovoltaic cells and thin film transistors. The process we incorporated was aluminum induced crystallization. We tested the effectiveness of using an electron beam in the process of aluminum induced crystallization. Using an Environmental scanning electron microscope as our source of electrons and incorporating various annealing times, accelerating voltages and spot sizes, we tested the electron beam’s ability to induce crystallization. 10 Introduction and Background Metal induced crystallization (MIC) is a process used to create polycrystalline silicon from amorphous silicon at relatively low temperatures. The process of MIC consist of an amorphous silicon thin film that are deposited onto a substrate. The substrate is usually glass. Then the film covered substrate is capped with a metal most likely aluminum. This entire structure is then annealed at temperatures between 150 and 400 degrees Celsius. This causes the amorphous silicon to change into polycrystalline silicon. Annealing in material science is a heat treatment wherein a material is altered, causing a change in its properties. In this instance it is a change in electrical properties. Because of rising interest in alternate renewable forms of energy, Metal induced crystallization is now receiving much more attention from researchers. The main application of polycrystalline silicon prepared by MIC is in the fabrication of thin film transistors and photovoltaic cells. “ For thin film solar cells polycrystalline silicon is the most promising material to reduce the production cost”[1]. Polycrystalline can be formed without the use of metal but the temperature requirements are much higher and thus more costly. “ Reduced processing temperature is the key to low cost devices”[2]. “For Al, as low as 150 degrees Celsius crystallization temperature can be used”[3]. The common method of inducing crystallization is to anneal the entire sample. In this experiment we hope to only anneal sections of the sample touched by the electron beam. Research Goals Our goal was to prove that an electron beam could be utilized to induce crystallization in amorphous silicon in specific spots touched without inducing crystallization in surrounding areas. This process might require less heat might make photovoltaic cells much cheaper in the future. According to the Department of Energy it currently cost 6.25/watt of produced energy. We want this much lower. Description of Experiment A 1 cm^2 glass substrate was covered in 200 nm of amorphous silicon and then 10 nm of aluminum. The glass substrate was then placed in a scanning electron microscope (SEM) at high vacuum and the electron beam of the SEM was then use to anneal specific sections of the surface. The specific heat formula (c = Q/mΔT) and a spot size vs. diameter chart from the SEM manual were used to determine the heat present at the surface where the electron beam touched. The first annealing was sixteen specific spots at 30 kv accelerating voltage and spot size 3 for 5 minutes per spot. The second annealing consisted of four different spots in which 3 of the spots were for 30 minutes and the last spot for an hour. The first three spots were 30 kv spot size 5, 20 kv spot size 5 and 10 kv spot size 4. The last spot was 30 kv spot size 1. Both the samples were then taken to the XRD to be tested at 28.5 degrees for the existence of polycrystalline silicon and viewed in the SEM for a change in the morphology of the surface. After this the substrate was changed. The new substrate consisted of a copper transmission electron microscope grid covered in 500 nm of amorphous silicon and 300 nm of aluminum. This substrate was annealed twice. The first spot was annealed for 15 minutes at 20 kv spot size 4. The second spot was annealed for 15 minutes at 30 kv spot size 4. The last substrate consisted of a carbon transmission electron microscope grid covered in 500 nm of amorphous silicon and 300 nm of aluminum. The first spot was annealed for 15 11 minutes 30kv spot size 4. The remaining two spots were annealed for 30 minutes at spot size 4. Experimental Results and Conclusions The sample with the sixteen spots showed no signs of a change in the morphology of the surface or the detection of polycrystalline silicon by the XRD. The second sample showed a definite signs of change in the morphology of the surface but did not show any signs of polycrystalline silicon in the XRD. The third sample showed more definite signs of a change in morphology but was still insufficiently large enough to be detected by XRay Diffraction (XRD). The transmission electron microscope substrates did show signs of crystallization in the TEM, and they did show definite signs of change in the morphology of the surface of the substrate. Through the research of electron beam welding it has been found that electron beams can exceed 25,000 degrees Celsius. We also believe that if an electron beam with a much higher current were used it would take the beam less time to produce a change in the surface and induce crystallization. Future Research Suggested by this Research We believe that if an electric gun with a high enough current were used with multiple filaments or a mesh screen of filaments it could be used to cover the entire surface of the substrate with these crystallized spot and dendritic trees beneath creating highways for the electrons produced in photovoltaic reactions. Secondly, increasing the annealing time and using the TEM beam for crystallization and immediate measurement would be an invaluable asset. Appendix A: List of References 1. J.H. Werner, R Bergmann, R. Brendel, Adv. Solid State Phys. 34(1995) 115 2. Maruf Hossam, Husam Abu-Safe, Hameed Naseem, Technical Digest of the International PVSEC-14, 2004 P-33 3. M. Shahidul haque, H. A. Naseem and W. D. Brown, J. Applied Physics, vol.95 p. 3928 1994 Appendix B: Intellectual Property-Commercialization Value The process of annealing would improve the performance of existing photovoltaic technology and would be highly valuable. Therefore if accomplished we would seek a patent. Appendix C: of REU on Personal Goals and Plans This summer has given me experience in another area of research. I now know what area of research I would like to do for my graduate education. I also learned many new pieces of test equipment and procedures. The past two summers in this program has given me a real insight into graduate education. I will definitely be putting my application in for graduate school. 12 Acknowledgements: I would like to acknowledge Mr. Vickers, Ms. Karla Clark, Dr. Husam Abu-Safe, Dr. Hameed Naseem , Dr. Mansour Mortazavi and the micro-electronics and photonics program for the opportunity to allow to study here for a second summer. My knowledge and skills have been improved. Last of all, I would like to thank the National Science Foundation for providing the funding which allows us to be able to come to this university each summer. 13