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A Report on the Progress of the Research / Thesis Entitled METALLIC CLUSTER FORMATION IN GLASSES BY JOHN S. RICH A THESIS SUBMITTED TO THE FACULTY OF ALFRED UNIVERSITY IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE DEGREE OF DOCTOR OF PHILOSOPHY IN GLASS SCIENCE ALFRED, NEW YORK FEBRUARY, 2011 Alfred University theses are copyright protected and may be used for education or personal research only. Reproduction or distribution in any format is prohibited without written permission from the author. METALLIC CLUSTER FORMATION IN GLASSES BY JOHN S. RICH B.S. ALFRED UNIVERSITY (2006) M.S. ALFRED UNIVERSITY (2008) SIGNATURE OF AUTHOR _____________________________________ APPROVED BY _______________________________________________ JAMES E. SHELBY, ADVISOR ________________________________________________ MATTHEW M. HALL, CO-ADVISOR ________________________________________________ ALEXIS G. CLARE, ADVISORY COMMITTEE ________________________________________________ WILLIAM C. LACOURSE, ADVISORY COMMITTEE ________________________________________________ S.K. SUNDARAM, ADVISORY COMMITTEE ________________________________________________ CHAIR, ORAL THESIS DEFENSE ACCEPTED BY _______________________________________________ DOREEN D. EDWARDS, DEAN KAZUO INAMORI SCHOOL OF ENGINEERING ACCEPTED BY _______________________________________________ NANCY J. EVANGELISTA, ASSOCIATE PROVOST FOR GRADUATE AND PROFESSIONAL PROGRAMS ALFRED UNIVERSITY ACKNOWLEDGMENTS I would like to thank my parents for supporting me throughout this experience. Without you both, this would not have been possible. I would like to thank my friends. You all made my time in Alfred worth remembering. And last, but certainly not least, I would like to thank Dr. Shelby for being there for me when he could. iii TABLE OF CONTENTS Page Acknowledgments ................................................................................................................ iii Table of Contents ................................................................................................................. iv List of Tables ........................................................................................................................ vi List of Figures .................................................................................................................... viii Abstract .............................................................................................................................. xiii 1. INTRODUCTION ................................................................................................... 1 2. LITERATURE REVIEW ....................................................................................... 2 2.1 Introduction ................................................................................................................... 2 2.2 Hydrogen Diffusion ....................................................................................................... 3 2.3 Hydrogen Reaction ........................................................................................................ 4 2.4 Nucleation and Growth Theory ..................................................................................... 8 2.5 Redox Equilibria in Glasses......................................................................................... 15 2.6 Instrumentation Background ....................................................................................... 16 2.6.1 Spectroscopy ..................................................................................................................... 16 2.6.2 Optical Spectroscopy ........................................................................................................ 17 2.6.3 IR Spectroscopy ................................................................................................................ 18 2.6.4 GIXRD .............................................................................................................................. 19 3. EXPERIMENTAL PROCEDURE ...................................................................... 20 3.1 Melting/Annealing ....................................................................................................... 20 3.2 Cutting/Polishing ......................................................................................................... 20 3.3 Hydrogen Reduction .................................................................................................... 20 3.4 Spectroscopy ................................................................................................................ 22 3.5 X-Ray Diffraction ........................................................................................................ 23 4. SODIUM INDIUM SILICATES .......................................................................... 24 4.1 Introduction ................................................................................................................. 24 4.2 Experimental ................................................................................................................ 24 4.3 Results ......................................................................................................................... 25 4.3.1 Microscopy ....................................................................................................................... 25 4.3.1.1 Spectroscopy ............................................................................................................ 40 4.4 Discussion .................................................................................................................... 56 4.4.1 Reaction ............................................................................................................................ 56 4.4.2 Nucleation and Growth ..................................................................................................... 65 iv 5. THE REDUCTION OF 2+ IONS IN SODA LIME SILICA GLASSES ......... 68 5.1 Introduction ................................................................................................................. 68 5.2 Results ......................................................................................................................... 68 5.3 Discussion .................................................................................................................... 88 5.3.1 Reaction ............................................................................................................................ 88 5.3.2 Nucleation/Growth ........................................................................................................... 92 6. THE FORMATION OF NI-CU ALLOYS IN GLASSES THROUGH HYDROGEN REDUCTION ................................................................................ 95 6.1 Introduction ................................................................................................................. 95 6.2 Results ......................................................................................................................... 96 6.3 Discussion .................................................................................................................. 109 7. CONCLUSIONS .................................................................................................. 113 8. FUTURE WORK ................................................................................................ 116 REFERENCES .............................................................................................................. 117 APPENDIX .................................................................................................................... 126 A-1 Background Correction for IR Spectra ...................................................................... 126 v LIST OF TABLES Page Table II. Experimental Treatment Temperatures for the Two Parts of this Chapter ....... 25 Table III. Calculated Backscattered Electron Coefficients and the Contrast Between Them for the Glasses Imaged Assuming Density has a Negligible Effect ............... 26 Table IV. Measurements Depicting Average Sizes of Features in Micrographs with Standard Deviations in Parenthesis ................................................................. 27 Table V. IR Band Locations and Intensity Ratios for the Entire Series of Indium Containing Glasses with Standard Deviations in Parenthesis......................... 42 Table VI. Difference IR Spectra Band Locations and Intensity Ratios for the Entire Series of Indium Containing Glasses Treated at 500°C with Standard Deviations ... 47 Table VII. Comparison between the base spectra intensity ratio to the difference spectra of the reduced glass intensity ratio for various indium containing ................. 47 Table VIII. Collection of the Best Fit Linear Regression of the Change in Absorbance of the 3500-3600 Cm-1 Band Plotted Against the Reduction Time .................... 54 Table IX. Calculated Concentrations of Indium Ions in the Various Glasses and the Respective Hydroxyl Sites Generated by Complete Reduction ..................... 57 Table X. Base Glass Compositions and Composition After Indium Reduction with Tg Values Retrieved from SciGlass ..................................................................... 58 Table XI. Estimated and Measured Properties for Thermal Expansion Mismatch Stresses ......................................................................................................................... 59 Table XII. Estimated Values of TEC for the
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