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Stoichiometric and Compositional Effects in Cryochemically Processed Barium Ferrite Ceramics

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Stoichiometric and Compositional Effects in Cryochemically Processed Barium Ferrite Ceramics 70 - 19,345 MILLER, Robert James, 1944- STOICHIOMETRIC AND COMPOSITIONAL EFFECTS IN CRYOCHEMICALLY PROCESSED BARIUM FERRITE CERAMICS. The Ohio State University, Ph.D., 1970 Engineering, chemical University Microfilms, A XEROX Company, Ann Arbor, Michigan THIS DISSERTATION HAS BEEN MICROFILMED EXACTLY AS RECEIVED STOICHIOMETRIC AND COMPOSITIONAL EFFECTS IN CRYOCHEMICALLY PROCESSED BARIUM FERRITE CERAMICS DISSERTATION Presented in Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the Graduate School of The Ohio State University By Robert James Miller, B. Cer. E ., M.S. * * * * * * The Ohio State University 1970 Approved by Adviser Department of Ceramic Engineering ACKNOWLEDGMENTS The author wishes to express his sincere appreciation to his adviser, Dr. Ralston Russell, J r ., for his advice and guidance throughout the course of this investigation. His consultation and suggestions proved, a great asset in planning and carrying out this investigation. The advice of Dr. Morris Berg and Dr. Rodney Tettenhorst in vari­ ous aspects of this study proved very helpful. The technical assistance of Dr. Michael Komarmy, Robert Winberg, Sam Matarella, David Achey, Steven Miele, Roger Brown, Carl Schaefer, Arthur Somers, and Robert Carol is gratefully recognized. They have helped to make this investigation more meaningful and complete. In addition, the author wishes to take this opportunity to express his gratitude to the AC Spark Plug Division of General Motors, who sponsored this investigation, and especially to Dr. Karl Schwartzwalder, whose efforts made the entire program possible. His guidance, advice, and even prodding were greatly appreciated. The author e g resses his gratitude to his wife, Marilyn, for her de­ votion and understanding during the last several months of this endeavor. Finally, the author wishes to somehow convey his utmost gratitude to Mrs. Ruth Wick for all her help in preparing this manuscript. Without her assistance, it could never have been completed at this time. li VITA June 27, 1944 . Born — Uhrichsville, Ohio 1967 ........................ B. of Cer. E ., The Ohio State University, Columbus, Ohio 1967 ........................ M. S c., The Ohio State University, Columbus, Ohio 1967-1969 .... General Motors Fellow, Department of Ceramic Engineering, The Ohio State University, Columbus, Ohio 1967-1969 .... Research Engineer, General Motors Corporation, Flint, Michigan PUBLICATION "BaO Glasses in High Alumina Ceramics," Bull. Am. Cer. Soc., 1969. ill TABLE OF CONTENTS Page ACKNOWLEDGMENTS............................................................................ il VITA ........................................................................................................ Hi LIST OF T A B L E S.................................................................................... vl LIST OF ILLUSTRATIONS.................................................................... vil INTRODUCTION........................................................................................ 1 LITERATURE REVIEW ........................................................................ 5 I. Material P reparation....................................................... 5 n. Calcination ...................................... 17 III. Sintering....................................................................... • . 18 IV. Composition............................ ....................................... 28 MODE OF INVESTIGATION.................................................................... 34 EXPERIMENTAL PROCEDURE............................................................ 36 I. Materials........................................................................... 36 n. Ferrite Preparation........................................................... 39 in. Specimen Preparation....................................................... 51 IV. Specimen Composition............................................... 52 V. Property Measurement................................................... 56 a. Magnetic P ro p erties............................................ 56 b. Fired Density........................................................ 61 c. Microstructure................................................... 61 iv RESULTS AND DISCUSSION............................................ I. Material P reparation................................ II. Compositional Evaluation . .................... a. BaO • 6 FegOg Materials .... b. BaO • 6Fe2Og + 2% Si02 Materials c. Varied BaO: Fe2Og Ratio Materials d. BaO -5 .5 Fe2Og Materials . e. BaO -5 .5 Fe2Og Additive Study . f. Dual Additive Materials .... III. Hot Pressing Evaluation............................ SUMMARY. ............................................................ CONCLUSIONS.................................................................... APPENDIX.............................................................................. BIBLIOGRAPHY................................................................ LIST OF TABLES Table Page 1. Barium Acetate Lot A n a ly s is...................................................... 36 2. Bismuth Trioxide Lot A n a ly s is .................................................. 37 3. Titanium Oxide Lot A n a ly s is............................. 38 4. Calcium Oxide Analysis, Maximum Im p u r itie s...................... 38 5. Lead Oxide Analysis, Maximum Im purities.............................. 39 6. Chemical S y s te m s.......................................................................... 43 7. Batch C om p osition s ..................................................................... 45 8. Calcination Results ..................................................................... 48 9. B inders............................................................................................. 48 10. Binder E valuation......................................................................... 50 11. Compositions for BaO • 6 FegOg with A d d itiv e s ...................... 53 12. Compositions with BaO • 6 Fe O, + Si09 as Base M a teria l...........................7 . ........................... 54 13. Compositions for Evaluation of BaO: Fe2Og R a tio.................. 55 14. Final Additive Evaluation, BaO • 5.5 Fe_0„ Base M a teria l............................................... 57 vl LIST OF ILLUSTRATIONS Figure Page 1. Cold Bath for Freezing and Pelletizing ........................................ 12 2. Schematic Diagram of Freeze D ryer............................................ 14 3. Phase Diagram................................................................................ 15 4. Pelletizing Apparatus.................................................................... 40 5. Hysteresigraph Electromagnet.................................................... 58 6. Hysteresis Loop Measurement T ech niqu e................................ 60 7. Remanence Values for BaO • 6 FegOg + A d d itives-I................ 66 8. Remanence Values for BaO • 6 Fe^Og + Additives-II................ 67 9. Coercive Force Values for BaO ■ 6 FegOg + Additives-I . 68 10. Coercive Force Values for BaO • 6 FegOg + Additives-II . 69 11. Energy Product vs. Intrinsic Coercive Force; BaO • 6 Fe2Og + A d ditives-I .................................................... 70 12. Energy Product vs. Intrinsic Coercive Force; BaO • 6 FegOg + Additives-II .................................................... 71 13. Fracture Surfaces of BaO • 6 Fe2O g ............................................ 73 14. Fracture Surfaces of BaO • 6 Fe2Og + 2% Si02 ........................ 75 • 15. Remanence Values for BaO * 6 Fe2Og + 2% Si02 + AlgOg . 76 16. Coercive Force Values for BaO • 6 Feo0 Q + 2% SiO« + 77 AV>3............ ............................... ... ................ ? ................... i7 . Energy Product vs. Intrinsic Coercive Force; BaO • 6 Fe2Og + 2% SiOg + AlgOg . ........................................ 78 18. Remanence Values for BaO • 6 Fe2Og + 2% SiOg + BlgOg . 79 viii Figure Page 19. Coercive Force Values for BaO • 6 Fe00„ + 2% Si09 + Bi20 3 ............................................-2 .3 ------------ ? ................... 80 20. Energy Product vs. Intrinsic Coercive Force; BaO • 6 Fe2Og + 2% S102 + B igO g............................................ 81 21. Remanence Values for BaO • 6 FegOg + 2% SiOg + CaO .... 82 22. Coercive Force Values for BaO • 6 FegOg + 2% SiOg + CaO . 83 23. Energy Product vs. Intrinsic Coercive Force; BaO • 6 Fe2Os + 2% SiOg + CaO ............................................ 84 24. Remanence Values for BaO* 6 FegOg + 2% SiOg + PbO .... 85 25. Coercive Force Values for BaO • 6 FegOg + 2% SiOg + PbO . 86 26. Energy Product vs. Intrinsic Coercive Force; BaO • 6 FegOg + 2% SiOg + PbO................................................ 87 27. Remanence Values for BaO • 6 FegOg + 2% SiOg + TiOg . 88 28. Coercive Force Values for BaO • 6 Fe00„ + 2% Si09 + T i O g ............................................ ...... 7 .................... 89 29. Energy Product vs. Intrinsic Coercive Force; BaO • 6 FegOg + 2% SiOg + TiOg ............................................ 90 30. Remanence Values for Various BaO: FegOg R a tio s................. 93 31. Coercive Force Values for Various BaO: FegOg Ratios . 94 32. Energy Product vs. Intrinsic Coercive Force; Various BaO: FegOg R a tio s.................................................................... 95 33. Remanence Values for Various BaO: Fe90„ Ratios with 2% S iO g ............................................... .
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