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Vacuum Microbalance Techniques: Volume 8 Proceedings of the Wakefield Conference, June 12–13, 1969 PDF

253 Pages·1971·9.27 MB·English
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Preview Vacuum Microbalance Techniques: Volume 8 Proceedings of the Wakefield Conference, June 12–13, 1969

VACUUM MICROBALANCE TECHNIQUES VOLUME 8 VACUUM MICROBALANCE TECHNIQUES Volume 1 Volume 5 Fort Monmouth Conference-1960 Princeton Conference-1965 Edited by Max J. Katz Edited by Klaus H. Behrndt Volume 2 Volume 6 Washington,D.C., Conference-1961 Newport Beach Conference-1966 Edited by Raymond F . Walker Edited by A. W. Czanderna Volume 7 Volume 3 Eindhoven Conference-1968 Los Angeles Conference-1962 Edited by C. H. Massen Edited by Klaus H. Behrndt and H. J . van Beckum Volume 4 Volume 8 Pittsburgh Conference - 1964 Wakefield Conference-1969 Edited by Paul M. Waters Edited by A. W. Czanderna VACUUM MICROBALANCE TECHNIQUES VOLUME 8 Proceedings of the Wakefield Conference June 12-13. 1969 Edited by A. W.Czanderna Clarkson College of Technology Potsdam, New York <:f? PLENUM PRESS • NEW YORK-LONDON • 1971 Library of Congress Catalog Card Number 61-8595 ISBN 978-1-4757-0135-7 ISBN 978-1-4757-0133-3 (eBook) DOl 10.1007/978-1-4757-0133-3 © 1971 Plenum Press, New York Soft cover reprint of the hardcover 1st edition 1971 A Division of Plenum Publishing Corporation 227 West 17th Street, New York, N.Y. 10011 United Kingdom edition published by Plenum Press, London A Division of Plenum Publishing Corporation, Ltd. Da.vis House (4th Floor), 8 Scrubs Lane, Harlesden, NW10 6SE, England All rights reserved No part of this publication may be reproduced in any form without written permission from the publisher. Introduction This volume contains the proceedings of the Eighth Conference on Vacuum Microbalance Techniques held at Wakefield, Massachusetts on June 12 and 13, 1969. The tenth anniversary of the first confer- ence will be registered as this volume passes through the typeset- ting and proofreading stages. The eight volumes that have spawned from this continuing series of conferences now contain a total of 125 papers. Thus, these volumes serve as a major repository of the world's literature on vacuum microbalance techniques. The Ninth and Tenth Conferences will be held in West Germany in June 1970 and in Texas in 1971. Each of the eight meetings has served as a forum where new developments in this rapidly advancing fie ld can be presented and discussed constructively within a conference atmosphere of cordial informality. The interaction of the participants at the conferences has led to the first treatise on ultra mlcrogravtmetry;' edited by S. P. Wolsky and E. J. Zdanuk, with most of the fourteen chapters written by steady contributors to the volumes on Vacuum Micro- balance Techniques. The number of research investigations and published works in which a vacuum microbalance is utilized con- tinues to expand r apldly.f This is a direct result of several types of automatic recording balances that are now available commercial- ly.3 The Eighth Conference was held to bring together again re- search scientists and engineers who exploit the measurement of mass as a means of studying physical and chemical phenomena. IS. P. Wolsky and E. J. Zda nuk, Ultra Mic ro Weight Determi nat ion in Controlled En- vironments. Intersci ence, New York, 1969. 2 A. W. Czanderna, "Utramicrobalance Review. " in: Wolsky and Zdanuk , op. cit• •p. 7. 3 D. Fox and M. Katz. "The Availability of Commerci a l Microbalances and Quar tz Crystal Oscillators, " in: Wolsky and Zdanuk , op. cit• •p. 465. v vi INTRODUCTION Support for the conference was provided by the Army Research Of- fice - Durham.! Clarkson College of Technology, P, R. Mallory and Co., Inc., and the Cahn Division of Ventron Instruments. Over 1500 users of microbalances were contacted by mail announcing the con- ference. In addition, the meeting was announced in the Journal of Vacuum Science and Technology.! Chemical and Engineering News,6 and Research/Development. 7 There were forty-six participants at the conference represent- ing Germany, Great Britain, and all regions of the United States. Roughly, two-thirds of the attendees from the United States came from the northeast, while the four scientists from Western Europe provided an international character to the meeting. The attendees were welcomed by the Conference Chairman, A. W. Czanderna, who provided a brief historical sketch of the conferences and indicated some of the benefits derived by the participants of previous confer- ences. In the technical program which followed, J. W. Whalen, Th, Gast, E. J. Zdanuk, and Pat Gaskins served successively as moder- ators for the four sessions. The first session was opened with an invited paper by E. A. Gulbransen and was followed by two contri- buted papers pertaining to oxidation. An invited paper was presented in the second session by E. Robens on the genera] problem of the mass defect produced by thermal gradients. In the third session, W. H. King presented an invited paper on applications of the crys- tal oscillator microbalance. Of the nineteen papers presented, seventeen are included in the proceedings and an eighteenth was accepted for publication after the conference because of its rele- vance to the other papers in the volume. Discussion questions and answers that followed each presentation are incorporated at the end of each paper. The cooperation of the participants and authors, which made it possible to document this valuable material, is grate- fully acknowledged. The format of the volume, abbreviations, ref- erences, etc., conform to that of previous volumes as outlined by the publisher, Plenum Press. In addition, the editor thanks all the authors for their cooperation in using the definitions developed for 4Gram DA - ARO-D-31-124- G1l57 to Clarkson Coll ege of Technology with A. VI. Czanderna as Principal Investigator. 5Announcements, J . Vac . Sci. Tech. 6 : 277. 1969. 6Chem . Eng. News, Feb. 24. 1969, p. 96; May 19, 1969, p. 46. 7 Research /Development. May 1969. p. 46; June 1969, p. 40. INTRODUCTION vii microbalances 8 and the AVS standard symbols for vacuum sys- tems.i It is a pleasure to thank all the people who contributed to the success of the Eighth Conference. Two complete mailings of the "Call for Papers n were handled by Pat Gaskins and Colin Williams and the staff of the Cahn Division of the Ventron Instruments Com- pany. The papers for the technical program were selected by S. P. Wolsky and A. W. Czanderna on the basis of abstracts submitted. Local arrangements for the meeting at the Colonial Statler Hilton were made by S. P. Wolsky, E. J. Zdanuk, and Mrs. M. Dor andi. The participants enjoyed hospitality provided by the Cahn, Rodder, Sartorius, and Worden Instrument Companies. Considerable typing and secretarial contributions were made by Mrs. A. Hollister from the planning stages to the publication of this volume. The painstak- ing task of copyediting the manuscripts and proofreading the galleys fell on Mrs. A. Czanderna and her assistance is gratefully acknowl- edged. Finally, it is my pleasure to thank Dr. H. M. Davis of the ARO-Durham, Dr . E . E . Anderson, Chairman of Physics at Clark- son College of Technology, and Dr. S. P, Wolsky, Director of Re- search at P, R. Mallory and Son, Inc., whose administrative deci- s ions and / or expertise led to direct financial support that made it possible to hold the E'ighth Conference on Vacuum Microbalance Techniques. Alvin W. Czanderna Potsdam, New York November 1969 8 Czanderna , op. cit. •p. 10-11. These definitions evolved from an. original se t suggested by T. N. Rhodin and were an outgro wth of interaction by S. P. Wolsky. R. L. Schwoebel, E. 1. Zdanuk, and A. W. Czanderna. They are recommended for use by all workers in the field . 9Graphic Symbols in Vacuu m Technology AVS Standard 7.1-1 966. J. Vac. Sci. Tech. 4 : 139-142.1967. Contents Conference Participants . . . . . . . . • • . . . • . • . • . . . • xi Interpretation of Vacuum Microbalance Data during the High-Temperature Oxidation of Materials (Invited) 1 E. A. Gulbransen The Simultaneous Use of Mass Spectrometer and Micro- balance Techniques for the Carbon - Oxygen System . .. . . . . . . . . . . . • . • . . . . . . . . . • . • 17 J . Graham Br own, John Dollimore , Clive M. Freedman, and Brian H. Harrison A System for the Determination of Oxidation- Reduction Kinetics in Nonstoichiometr ic Metal Oxides . . • • . 29 I. Bransky and N. M. Ta llan An Automated Bakeable Quartz Fiber Vacuum Ultra- microbalance .. .. . ....... ....... •.••• 43 J. Rodder Adsorption Studies with a Bakeable Quartz Automatic Recording Ultramicrobalance ..•.... .••...• 55 Stanley E. Fink and Robert P. Merrill The Effect of Thermal Gas Motion on Microbalance Measur ements (Invited) ..•.........••...• 73 E. Robens Gravimetric Adsorption Studies of Hydrogen on Granular Metal Surfaces Using a Vacuum Microbalance 97 D. A. Cadenhead and N. J. Wagner Gravimetric Measurement of the Molecular Area of Some Adsorbed Gases .•..•.....••...•••• 111 E. Robens, G. Sandstede , and G. Walter ix x CONTENTS Vapor Adsorption Studies on Low-Energy Solids 121 J. W. Whalen Momentum Artifacts in the Gravimetric Measurement of 131 Fast Desorption .....•..•.......•.....• Robert P. Merrill, Charles R. Arnold, and Andrew J. Robell On the Development of Electromagnetic Balances in Recent Years .....•..•...•.....•••.. 0 • 141 Tho Gast Pressure of Light Used as Restoring Force on a Micro- balance .••. 0 0 0 •• 0 0 0 • 0 • 0 • 0 • 0 0 • 0 • 0 0 0 0 0 147 Karl P. Zinnow and Jens Po Dybwad Vacuum Microbalance Apparatus for Rapid Determination of Low-Temperature Vaporization Rates . 0 • • • • • 155 J, Gordon Davy Wireless Temperature Measurement of a Sample in Vacuum. 0 0 0 • 0 0 0 0 • 0 0 0 0 0 • 0 0 • • • • • • • • • • • 173 G. Richard Blair Applications of the Quartz Crystal Resonator (Invited) 183 Wo H. King, Jr. Thermal Degradation of Piperazine Copolyamides . . . . • 201 Stephen D. Bruck and Ashok Thadani A Thermal Analysis System for Radioactive Materials. . 215 W. J. Kerrigan, J. S. Byrd, and P. Do Holloway Thermal Degradation of an Anhydride-Cured Epoxy Resin by Laser Heating 0 0 •••••• 0 • 0 • 0 0 0 0 0 • 229 A. So Vlastaras Author Index 243 Subject Index 247 Conference Participants Richard M. Alire D. A. Cadenhead Los Alamos Scientific Department of Chemistry Laboratory SUNY at Buffalo P. O. Box 1663 Buffalo, New York 14214 Los Alamos, New Mexico 87544 Peter G. Chamy General Electric Company Warren A. Anderson 6901 Elmwood Avenue Sylvania Ltg. Center 100 Endicott Street Materials Laboratory - 10-779 Danvers, Massachusetts 01923 Philadelphia, Pennsylvania 19142 Edward G. Clarke, Jr. Klaus Behrndt Department of Physics Granville-Phillips Co. Clarkson College of Technology 5675 E. Arapahoe Street Potsdam, New York 13676 Boulder, Colorado 80302 A. W. Czanderna Joseph R. Biegen Department of Physics Department of Physics Clarkson College of Technology Clarkson College of Technology Potsdam, New York 13676 Potsdam, New York 13676 J. Dollimore G. Richard Blair Dept. of Pure and Applied Hughes Aircraft Company Physics Electron Dynamics Division University of Salford Torrance, California 90509 Salford 5, Lancashire,England Jens Peter Dybwad 1. Bransky Space Physics Laboratory Wright-Patterson AFB Air Force Cambridge Research ARL(ARZ) Bldg. 450 Laboratories Ohio 45433 Bedford, Massachusetts 01730 S. D. Bruck Owen Fiet National Heart Institute TRW Systems National Institute of Health 1 Space Park Bethesda, Maryland 20014 Redondo Beach, California 90278 xi

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