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Shape-Preserving Physical and Chemical Transformations of Si and Sio2 Nano- and Microstructures a Dissertation Presented To Shape-Preserving Physical and Chemical Transformations of Si and SiO2 Nano- and Microstructures A Dissertation Presented to The Academic Faculty by Ari Gordin In Partial Fulfillment Of the Requirements for the Degree Doctor of Philosophy in Materials Science and Engineering Georgia Institute of Technology August, 2014 Copyright © Ari Gordin 2014 Shape-Preserving Physical and Chemical Transformations of Si and SiO2 Nano- and Microstructures Approved by: Dr. Kenneth H. Sandhage, Advisor Dr. Michael A. Filler School of Materials Science School of Chemical and and Engineering Biomolecular Engineering Georgia Institute of Technology Georgia Institute of Technology Dr. Thomas H. Sanders, Jr. Dr. Lawrence Bottomley School of Materials Science School of Chemistry & Biochemistry and Engineering Georgia Institute of Technology Georgia Institute of Technology Dr. Angus P. Wilkinson School of Materials Science and Engineering Georgia Institute of Technology Date Approved: June 30, 2014 Acknowledgements My advisor, Dr. Sandhage, for never accepting mediocre work, for giving me the freedom and encouragement to explore my own ideas (which rarely worked as planned), for sharing his seemingly limitless knowledge, and, it must be said, for making sure my paychecks cleared. My committee members, including Dr. Bottomley (who taught the first class I ever took at Georgia Tech nearly a decade ago), Dr. Wilkinson (who taught the first inorganic chemistry class I ever took, which convinced me to pursue a career in solid state chemistry), and Dr. Sanders (who taught the first materials science class I ever took). My coworkers, all of whom I consider personal friends (except Ben), for putting up with my personality, humor, complaints, and making my daily work-life enjoyable and fun, even when the work itself may not have been. My hair-stylist, David Zecca; my personal trainer, Kafka; and my personal shopping assistant, Lucky Yates. My parents, whose immeasurable support more often than not went unthanked (but never unappreciated). The partner and love of my life, my wife Paulina, whose enduring support and personal sacrifices cannot be put into words. I don’t know where we will go next, but I know we will get there together. ii Table of Contents Acknowledgements ii List of Tables iv List of Figures v Summary x Part I: Shape-Preserving Physical Transformation of Silicon Nano- and Microstructures Chapter 1: Design of a Porosification Process for Si nano- and Micro-structures 1 1.1 Summary 1 1.2 Motivation 1 1.3 Background of Anodized p-Si Films 4 1.4 Metal Assisted Chemical Etching 7 1.5 Formation of Porous Materials via Selective Leaching 9 1.6 Design of Selective Leaching Method for Silicon 12 1.7 Conversion of Si-Nanowires into Group II Silicide Replicas 20 1.8 Experimental 22 1.9 Results and Discussion 23 1.10 Selective Extraction of Magnesium from Mg2Si 28 1.11 Halide-Based Selective Leaching of Mg from Mg2Si 29 1.12 Selective Oxidation of Magnesium in Mg2Si 40 1.13 Discussion & Limitations of Selective Oxidation 50 1.14 Conclusion 55 1.15 References 56 Part II: Shape-Preserving Chemical Transformations of SiO2 Photonic Structures Chapter 2: Conversion of SiO2 Photonic Crystals into High-Index Mg2Si Replicas 66 2.1 Summary 66 2.2 Background of Photonic Crystals and Photonic Bandgaps 66 2.3 Motivation and Approach 70 2.4 Experimental Methods 78 2.5 Results and Discussion 80 2.6 Conversion of Biologically Derived SiO2 Photonic Structures 87 2.7 Limitations and Future Direction 93 2.8 Conclusions 97 2.9 References 97 Chapter 3: Conversion of SiO2 Photonic Crystal Fibers into IR-Transparent Replicas 103 Summary 103 Background of Photonic Crystal Fibers 103 Motivation and Approach 107 Experimental Methods 112 Results 114 Limitations and Future Directions 125 Conclusion 128 References 129 Chapter 4: Kinetic Study of Magnesium Silicide Growth 136 4.1 Summary 136 4.2 The Silicidation Reaction 136 4.3 In-situ Observation via Grazing Angle, HT-XRD 141 4.4 Experimental Setup 143 4.5 Results 144 4.6 Quantitative Analysis of HT-XRD Patterns 151 4.7 Discussion 169 4.8 Conclusion 177 4.9 References 177 iii List of Tables Table 1: Published applications involving porous silicon nanostructures. ...................................................... 3 Table 2: Overview of porous-materials which have been prepared using selective leaching techniques. ... 11 Table 3: Relevant properties of selected alkaline earth metal silicides ........................................................ 20 Table 4: Possible reactions in the oxidation of Mg2Si ................................................................................... 40 Table 5: Overview of Previously Reported Shape Preserving Gas / SiO2 Reactions ...................................... 65 107,108 Table 6: Molar Volumes of Relevant Materials ..................................................................................... 72 Table 7: Overview of rate limiting steps and growth characteristics of various silicides. ........................... 137 Table 8: Thickness of Mg-coating at randomly selected areas of the wafer. .............................................. 146 Table 9: SEM determined thickness of Mg2Si after complete reaction. ...................................................... 149 Table 10: Slopes of best-fit lines in log(Mg2Si thickness) vs log(time) plots. ............................................... 166 Table 11: Experimentally determined growth data. ................................................................................... 169 iv List of Figures Figure 1: Number of publications/year showing simultaneous surge in interest in porous silicon and in silicon nanostructures (from Web of Science). ............................................................................... 2 Figure 2: Schematic for Fabrication of Porous Silicon via Anodic Etching ..................................................... 5 Figure 3: Characteristic Potential vs. current density curve for anodization of Si, showing regimes of pore- formation and electropolishing. ...................................................................................................... 6 Figure 4: Fabrication of freestanding por-Si particles via liftoff and fracture of anodized film. .................... 7 Figure 5: A variety of silicon micro- and nanostructures have been fabricated including nanowires, nanospheres, and waveguides. ....................................................................................................... 7 Figure 6: Overview of typical MACE process. ................................................................................................. 8 Figure 7: Mechanism of porous nanowire fabrication via metal assisted chemical etching. Porosity is only observed for highly doped silicon22. ................................................................................................ 9 Figure 8: Cross-section and top-down view of porous gold film formed via selective ................................ 10 Figure 9: Schematic of post-growth porosification process based on successive silicidation and selective leaching. In the first step, conversion of a dense Si-structure into a silicide with a larger volume results in volume expansion. In the second step, selective extraction of the metal from the silicide will either result in generation of porosity or shrinkage back to the original size. ........... 13 Figure 10: After some initial reaction, a dense metal silicide film forms on the Si surface. For further reaction to proceed, either (a) metal atoms must diffuse inward, in which case a direct replica may be expected, or (b) Si atoms must diffuse outward, in which case an inverse replica is possible. ........................................................................................................................................ 16 Figure 11: Schematic of (a) a solid/solid silicidation reaction, and (b) a gas/solid silicidation reaction. ...... 21 Figure 12: XRD of reaction product of reaction between silicon and calcium and 790oC for 6 hours, confirming the growth of multiple silicide phases. ....................................................................... 23 Figure 13: Binary phase diagrams for the Si –Mg, Si-Ca, and Si-Sr systems. ................................................. 24 Figure 14: (a) SEM and EDX of as-fabricated Si nanowires before reaction; (b) SEM and EDX of nanowires o after reaction with Mg-vapor at 500 C for 6 hours to form Mg2Si; (c) TEM image of a single nanowire showing polycrystalline nature of nanowires; (d) Electron diffraction pattern confirming Mg2Si as the only crystalline phase; and (e) XRD pattern of the reacted nanowires consistent with Mg2Si. Scalebars shown for (a) and (b) are 1 µm. ................................................ 26 Figure 15: High resolution TEM of grain boundary region in a single Mg2Si nanowire. ................................ 27 Figure 16: Magnesium silicide (Mg2Si) nanospheres (left) and microspheres (right), fabricated via gas/solid silicidation of silicon templates. A 10:1 molar ratio of Mg:Si was utilized, and the reaction was o carried out at 575 C for 8 hours. Scalebars are 1 µm. ................................................................. 28 Figure 17: XRD of gray product produced via reaction of Mg2Si in 1M HCl for 20 minutes; reaction produced visible sparks. ................................................................................................................ 30 Figure 18: (a) SEM and (b) EDX of residual
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