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Information to Users INFORMATION TO USERS While the most advanced technology has been used to photograph and reproduce this manuscript, the quality of the reproduction is heavily dependent upon the quality of the material submitted. For example: • Manuscript pages may have indistinct print. In such cases, the best available copy has been filmed. • Manuscripts may not always be complete. In such cases, a note will indicate that it is not possible to obtain missing pages. • Copyrighted material may have been removed from the manuscript. In such cases, a note will indicate the deletion. Oversize materials (e.g., maps, drawings, and charts) are photographed by sectioning the original, beginning at the upper left-hand corner and continuing from left to right in equal sections with small overlaps. Each oversize page is also filmed as one exposure and is available, for an additional charge, as a standard 35mm slide or as a 17”x 23” black and white photographic print. Most photographs reproduce acceptably on positive microfilm or microfiche but lack the clarity on xerographic copies made from the microfilm. For an additional charge, 35mm slides of 6”x 9” black and white photographic prints are available for any photographs or illustrations that cannot be reproduced satisfactorily by xerography. 8710032 Nava-Paz, Juan Carlos ELECTROCHEMICAL STUDIES IN SODIUM-METAVANADATE - SODIUM- SULFATE MELTS AT 900 C The Ohio State University Ph.D. 1987 University Microfilms International300 N. Zeeb Road, Ann Arbor, Ml 48106 Copyright 1987 by Nava-Paz, Juan Carlos All Rights Reserved PLEASE NOTE: In all cases this material has been filmed in the best possible way from the available copy. Problems encountered with this document have been identified here with a check mark V . 1. Glossy photographs or p a g e s ______ 2. Colored illustrations, paper or print _______ 3. Photographs with dark background 4. Illustrations are poor copy _______ 5. Pages with black marks, not original co p y _______ 6. Print shows through as there is text on both sides of page _______ 7. Indistinct, broken or small print on several pages _ 8. Print exceeds margin requirem ents_______ 9. Tightly bound copy with print lost in sp in e ________ 10. Computer printout pages with indistinct print _______ 11. Page(s) _____________ lacking when material received, and not available from school or author. 12. Page(s) seem to be missing in numbering only as text follows. 13. Two pages numbered . Text follows. 14. Curling and wrinkled pages 15. Dissertation contains pages with print at a slant, filmed as received 16. Other University Microfilms International ELECTROCHEMICAL STUDIES IN NaVO^-NaJSO. MELTS AT 900 C d 2 4 DISSERTATION Presented in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy in the Graduate School of The Ohio State University By Juan Carlos Nava-Paz, B.S., M.S. ***** The Ohio State University 1987 Dissertation Committee: Approved by R. A. Rapp G. R. St.Pierre Adviser Department of Metallurical B. E. Wilde Engineering ©1987 JUAN CARLOS NAVA-PAZ All Rights Reserved To my family, for their love, encouragement, and inspiration. ii ACKNOWLEDGMENTS The author expresses his sincere appreciation to Dr. Robert A. Rapp for his support and guidance during the course of this research, for many interesting and stimulating discussions and for his assistance in "the preparation of this manuscript. A word of thanks is indeed in order to CEPET of Venezuela for its invaluable support. Aknowledgment is granted to my friends and colleagues Yie Shing Hwang, Dianne Shi, Ravi Vilupanur, Yun Shu Zhang and Chong Ook Park for their encouragement and moral support. VITA September 26, 19b9 ......... Born - Maracaibo.Venezuela 1982 .......................... B. S. , Universidad del Zulia Maracaibo, Venezuela 1983 .......................... Scholarship Awarded by CEPET of Venezuela 198b .......................... M.S. , The Ohio State University, Columbus, Ohio FIELDS OF STUDY Ma.ior Ptield: Metallurgical Engineering Corrosion Drs. W. Johnson, S.Smialowska and R. Rapp Electroohemi stry Dr. T. Kuwana Chemical Metallurgy Drs. G. St.Pierre, W. Johnson, R. Rapp, J . Hirth Physical Metallurgy Drs. P. Shewmon, G. Powell, G. Meyrick, W. Clark Mechanical Metallurgy Drs. J. Hirth, R. Wagoner, R. Hoagland Electron Microscopy Dr. W. Clark Solidification Dr. Carroll Mobley iv TABLE OF CONTENTS ACKNOWLEDGMENTS .......................................... iii VITA ......................................................... iv LIST OF TABLES ............................................ vi LIST OF FIGURES ........................................... ix CHARTER page I . INTRODUCTION ................................. 1 I I. ELECTROANALYTICAL TECHNIQUES .............. 12 Cyclic Voltammetry ......................... 12 Chronopotentiometry ........................ 14 Chronoamperometry ........................... 18 AC Impedance ................................. 20 111. EXPERIMENTAL PROCEDURE ..................... 29 IV. RESULTS AND DISCUSSION ..................... 37 Electrochemical Studies in Relatively Basic NaVOg-NagSO^ Solutions.............. 37 Reaction Mechanism ......................... 79 Electrochemical Studies in NaVO„-Na^SO. Solutions Under 0 ^ Gas .................... 94 Reaction Mechanism ......................... 129 Electrochemical Studies in NaVO,-,-Na„S0. Solutions Under 0.1 % SOg-Og Gas .......... 137 Reaction Mechanism ......................... 181 AC Impedance Results on The PtPainted WE 194 AC Impedance Results on The PtFoil WE .. 201 Discussion of AC Impedance Results ..... 208 CONCLUSIONS 213 LIST OF REFERENCES 215 v LIST OF TABLES Table Page 1 . F'eak Potential As a Function Of Scan Rate For a Pure Pt Foil WE Immersed In a NaVO^-Na^SO^ Solution Of Basicity -9.77 At 900 C ......... 41 2. Anodic To Cathodic Peak Current Ratio For Various Scan Rates For a Pure Pt Foil WE Immersed In a NaVO^-Na^SO^ Solution Of Basicity -9.77 At 900 C ....................... 41 3. Peak Potential As a Function Of Scan Rate For a Pure Pt Foil WE Immersed In a Na^SO^ Melt Of Basicity -6.66 At 900 C ................... 57 4. Chronopotentiometric Data For a Pure Pt Foil WE Immersed In a NaVO^-Na^SO^ Solution Of Basicity -9.77 At 900 C ....................... 57 5. Variation Of Peak Potential With Scan Rate For Cyclic Voltammograms On a Pure Pt Foil WE Immersed In a NaV0o-Na,.SO. Solutions Of 3 2 4 Basicity -11.70 At 900 C ....................... 97 6. Thermodynamic Data At 900 C ................. 82 7. Variation Of Anodic To Cathodic Peak Current Ratio With Scan Rate For Cyclic Voltammograms On a Pure Pt Foil WE Immersed In a NaVO,- o v i NaoS0/l Solution Of Basicity -11.70 At 900 C 2 4 8. Criteria For Determining The Reaction Mechanism From Cyclic Voltammetry ........... 101 9. Variation Of Peak Potential With Scan Rate For Cyclic Voltammograms On a Pure Pt Foil WE Immersed in a Na^SO^ Melt At 900 C Under 0^ 121 10. Chronopotentiometric Data On a Pt Foil WE Immersed In a NaVO^-Na^SO^ Solution Of Basicity -11.70 At 900 C ................. 121 11. Variation Of Peak Potential With Scan Rate For Cyclic Voltammograms On a Pure Pt Foil Immersed In a NaVu,-Na,.S0. Solution At 900 C 3 2 4 Under Uncatalyzed 0.1% SOg-Or, Atmosphere ... 139 12. Variation Of Anodic To Cathodic Peak Current Ratio With Scan Rate For Cyclic Voltammograms On a Pure Pt Foil WE Immersed In a NaVO^- NarS0. Solutions Of Basicity -11.72 At 900 C 139 4 13. Chronopotentiometric Data From a Pure Foil WE Immersed In a NaVO,--Nar,SO. Solution Of 3 2 4 Basicity -11.72 At 900 C ...................... 149 14. Variation Of Peak Potential With Scan Rate For a Pure Pt Foil WE Immersed in a NaV0o-Nar.S0. 3 2 4 Solution of Basicity -13.15 At 900 C ....... 149 15. Chronopotentiometric Data From a Pure Pt Foil WE Immersed In a NaVO^-Na^SO^ Solution Of Basicity -13.15 At 900 C ................. 170 vii 16. Variation Of Peak Potential With Scan Rate For a Pure Pt Foil WE Immersed In a NaVO^-NagSO^ Solution Of Basicity -13.85 At 900 C ....... 170 17. Chronopotentiometric Data From A Pure Pt Foil WE Immersed In a NaVO^-NagSO^ Solution Of Basicity -13.85 At 900 C ................. 176 18. Ohmic Resistance From AC Impedance Measurements .................................... 211 vi ii LIST OF FIGURES Figure page 1. Cyclic Voltammetry ......................... 13 2. Chronopotentiometry ........................ lb 3. Chronopotentiometric Diagnostic Plot ... 17 4. Chronoamperometry .......................... 19 b. AC Impedance Representation For a Purely Activation Controlled Interface ......... 22 6. AC impedance Representation B'or a Mixed Controlled Interface ....................... 24 7. Bode Plot B'or An Activation Controlled Interface Reaction ......................... 26 8. Bode Plots For A System With Two Rate Determining Steps .......................... 26 9. Randles Plot ................................. 28 1U. ZR vs ZI/W Plot For an Activation Controlled Interface Equivalent To The Circuit In Fig. b a ........................... 28 11. Experimental Setup For Electrochemical Studies At 900 C ............................ 33 12. Apparatus Arrangement For Cyclic Voltam­ metry and Chronopotentiometry ........... 34 ix 13. Block Diagram For AC Impedance Measurements ................................. 36 14. Cyclic Voltammograms On A Pure Pt WE Immersed In A 10 m/o NaVOg-Na^SO^ Solution Of Basicity -9.77 At 900 C ............. 38 lb. Cyclic Voltammograms At Various Cathodic Switching Potentials Recorded On A Pt WE Immersed In A 10 M/o NaVO^-Na^SO. Solution Of Basicity
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