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Application of the X-Ray Photoelectron Spectroscopy for Development of the Niobium Chemical Mechanical Process, Photomodificatio

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Application of the X-Ray Photoelectron Spectroscopy for Development of the Niobium Chemical Mechanical Process, Photomodificatio Application of the X-ray Photoelectron Spectroscopy for Development of the Niobium Chemical Mechanical Process, Photomodification of Silicon for the Field Release Mass Spectrometer, and Analysis of the Multifunctional Oxide Heterostructures A Thesis Presented by Natalia Maximova to The Department of Chemical Engineering in partial fulfillment of the requirements for the degree of Master of Science in Chemical Engineering Northeastern University Boston, Massachusetts April 17, 2008 ABSTRACT X-ray photoelectron spectroscopy (XPS) provides information about the elemental chemical composition of a surface and the bonding states of those elements. This information is critical to diverse applications where the surface of the material determines its functionality such as tuned catalysts, engineered polymer coatings, and nanoelectronic heterostructures. For this thesis, XPS has been applied in both traditional and novel ways to niobium surface polishing, silicon surface modification, and electronic structure measurement. The current method for fabricating niobium superconducting cavities produces rough and defective surfaces. A proof-of-concept project to develop a niobium Chemical Mechanical Polishing (CMP) process used XPS to monitor surface composition and structure under varying CMP parameters. XPS confirmed rapid oxidation of the niobium with a self-limiting surface oxide of 5.0±0.8 nm. CMP surface effects were explored and a smooth (24 nm average roughness) niobium wafer with an ordered surface was produced. Current methods of detecting complex airborne toxins such as anthrax are time consuming and often give false positives [1]. A modified field release mass spectrometer (FRMS) will enable specific and selective real-time detection of air toxins through utilization of the modified silicon surfaces for the capture and release of these analytes. Photomodification of the silicon surface with undecylenic acid resulted in 42±1 % monolayer coverage as determined from the XPS and angle resolved XPS (ARXPS) data ii using an adapted method from Haber et al. in [2]. Carbon contamination was shown to be detrimental to the formation of the monolayers. Determination of the valence band offsets in multifunctional oxide heterostructures provided a tool for insight in the electronic properties of these materials. The valence band offset for magnesium oxide grown epitaxially on silicon carbide was found to be 1.13±0.12 eV which is consistent with expected offsets based on the band gaps of the two materials. Future work will focus on determining repeatability and accuracy of the valence band offset measurements in various heterostructures. iii ACKNOWLEDGEMENT A great number of people assisted me in completion of this work. I would not be writing this if it was not for my family, my friends, fellow students at Northeastern, and last but not least faculty. Let me start by acknowledging the Northeastern crowd. I would like to thank my advisor Dr. Katherine S. Ziemer who let me work in her laboratory, guided me through these three years at Northeastern, and secured financial aid to allow me to concentrate on studies and research. My gratitude goes to my committee members, Dr. Shashi K. Murthy, Dr. Daniel Burkey, and Dr. Sinan Muftu for help with my thesis. In addition to being on my committee, Dr. Shashi K. Murthy allowed me to use a chemical hood in his lab for silicon cleaning experiments. His students helped me with set up my equipment, especially Brian Plouffe. It was a pleasure working with Dr. Sinan Muftu and George Calota who performed CMP experiments on the niobium wafers. Throughout three years at Northeastern, I worked as a Connections lab manager under leadership of Rachelle Reisberg. I would like to thank Rachelle for giving me an opportunity to work at Connections and helping me through tough times. Dr. Ronald Willey allowed me to use his lab space for purging of the reagent for photomodification in the silicon project. Between Christmas and New Year’s of 2006 when most people are on a break, he came in to change the pressure gauge to make sure that nothing blew up during my purging procedure. I look forward to meeting him at AIChE meetings and while geocaching. His graduate students, James Minicucci and Edward Viveiros helped me with setup of my experiment in their lab. iv My boyfriend, Jonathan Meade, deserved acknowledgement with the University folks as he helped me build a photoreactor. He put all pieces together and wired it. He has been a great support since the time I joined Northeastern. Thanks to the in-network minutes we stayed close and grew our relationship despite living in different states. My fellow students deserve a special thank you as well. Kathleen McCarthy was my comrade in research and job search. During long discussions about research, economy, job search, politics, classes, family, relationships, etc, I feel that we have built a strong friendship. I hope to continue my relationship with Kathleen in my professional life. Trevor Goodrich and Zhuhua Cai taught me how to use XPS and AES, and turned off the instruments on multiple occasions so that I could catch my train. Trevor did most of the SEM analysis of niobium samples, and Zhuhua cleaned silicon carbide and grew magnesium oxide for the valence band offset experiment. Bing Sun, thank you for your encouragement and support. Dr. Albert Sacco Jr. allowed me to move into CAMMP office. Dr. Juliusz Warzywoda and CAMMP students welcomed me and assisted me throughout my stay. Mariam Ismail, Dennis Callahan, and Julo helped me with SEM imaging. Jonathan Leong captured AFM images of the polished niobium surfaces. Dr. Elizabeth Podlaha and her graduate students assisted with determination of the OCP potential for the niobium CMP project. Undergraduate students, Chris McLaughlin, Katie Passino, and Abby Deleault, contributed to the silicon project. v Robert Eagan has built an excellent support for the Barnstead filtering system, so that I could wheel it around. He also assisted with some other projects which were always completed in no time. Now I would like to thank my family in U.S. and in Russia who kept my spirit up throughout my academic career. My mom, her husband, and my sister encouraged and supported me. My mom deserves special thanks for raising me and teaching me discipline and determination. I would have not been here if it was not for her. My aunts in Saint Petersburg and Moscow, and my cousins listened to me complain and provided great support that would have been enough for two degrees. My dear friend TO, who has been my friend since my studies at Saint Petersburg University of Refrigeration and Food Technologies, has listened to me for hours, entertained me with her crazy adventures, and was just the best friend one could ever dream of. My friends from Connecticut believed in me and helped me as well. I especially want to acknowledge my boyfriend’s family, especially his mom, who supplied me with prepared food and Costco products to help me save money and stay healthy. vi TABLE OF CONTENTS LIST OF FIGURES…………………………………………………………………… ix LIST OF TABLES…………………………………………………………………….. xiii 1.0 INTRODUCTION………………………………………………………………1 2.0 BACKGROUND INFORMATION ON X-RAY PHOTOELECTRON SPECTROSCOPY………………………………………………………............6 2.1 Description of the XPS Instrument…………………………………………. 6 2.2 Physics behind XPS………………………………………………………….. 8 2.3 Spectral Interpretation………………………………………………………. 13 2.3.1 Survey Spectra…………………………………………………………. 14 2.3.2 Elemental Spectra………………………………………………………15 2.4 Quantitative XPS Analysis…………………………………………………... 16 2.4.1 Inelastic Mean Free Path and Sampling Depth……………………… 17 2.4.2 Area under the Curve, Sensitivity Factors for Elemental Composition, and Composition of Bonding States……………………………………... 18 2.4.3 Peak Fitting……………………………………………………………. 23 2.4.4 Thickness Calculations………………………………………………... 26 2.4.5 Error Analysis…………………………………………………………. 27 2.5 Beyond Composition…………………………………………………………. 29 2.5.1 Angle Resolved XPS for Depth Profiling and Increased Surface Sensitivity………………………………………………………………… 29 2.5.2 Valence Band Offset Measurements………………………………….. 31 2.6 Experimental Apparatus and Procedures in the Interface Engineering Laboratory…………………………………………………………………… 33 2.7 Applications of XPS………………………………………………………….. 36 3.0 NIOBIUM CHEMICAL MECHANICAL POLISHING……………………….37 3.1 Critical Literature Review: Niobium CMP ………………………………... 40 3.1.1 Surface Requirements for SRF Cavities……………………………… 41 3.1.2 Niobium: Surface Studies……………………………………………... 47 3.1.3 Chemical Mechanical Polishing: Applications to Semiconductors and Metals…………………………………………………………………….. 57 3.1.4 Niobium Chemistry; Pourbaix Diagrams…………………………….. 61 3.1.5 Summary………………………………………………………………. 65 3.2 Experimental: Niobium CMP………………………………………………. 66 3.2.1 Materials……………………………………………………………….. 66 3.2.2 Experimental Procedure: Degrease, BCP, Oxidizing and Etch Treatments, CMP………………………………………………………… 68 3.2.3 XPS: Data Acquisition and Manipulation……………………………. 71 vii 3.2.4 SEM and AFM Analysis………………………………………………. 75 3.3 Results and Discussion: Niobium CMP…………………………………….. 76 3.3.1 Chemical Stability of Niobium in Oxidizing and Etching Aqueous Solutions………………………………………………………………….. 76 3.3.2 Niobium Surface Condition after CMP Process……………………… 87 3.3.2.1. Effect of Starting Surface Condition…………………………88 3.3.2.2. Effect of Slurry Parameters: Type of Abrasive Particle, pH…………………………………………………………………..97 3.3.2.3. Multi-Slurry Process …………………………………………106 3.4 Summary and Conclusions for Nb CMP…………………………………....111 3.5
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