VACUUM MICROBALANCE TECHNIQUES VOLUME 7 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 VolumeS Pittsburgh Conference -1964 Wakefield Conference-1969 Edited by Paul M. Waters Edited by A. W. Czanderna VACUUM MICROBALANCE TECHNIQUES VOLUME 7 Proceedings of the Eindhoven Conference June 17-18,1968 Edited by c. H. Massen and H. J. van Beckum Eindhoven University of Technology Eindhoven, Netherlands g:> PLENUM PRESS • NEW YORK-LONDON • 1970 Library of Congress Catalog Card Number 61-8595 ISBN 978-1-4757-0727-4 ISBN 978-1-4757-0725-0 (eBook) DOI 10.1007/978-1-4757-0725-0 © 1970 Plenum Press, New York Softcover reprint of the hardcover 1st edition 1970 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. Donington House, 80 Norfolk Street London W.C. 2, England All rights reserved No part of this publication may be reproduced in any form without written permission from the publisher. At the Seventh Vacuum Microbalance Techniques Con ference one member was unfortunately absent whom all his colleagues would have been glad to meet again. He was our friend Lee Cahn, the initiator and driving force of these conferences. whose sudden death de prived the field of microbalance research of a most enthusiastic collaborator. Cahn's inventive faculty has always inspired young research workers all over the world and has led to the extension of our knowledge, the improvement of vacuum m icrobala nce techniques. and the expansion of their fields of application. Lee Cahn will be especially remembered for his ac tive part in the conference discussions, which re sulted in many novel views. It was Cahn's practical mind that turned them into improvements of hIs prod ucts. In fact, Lee Cahn was a link between science and engineering, and he will be sorely missed. Editors' Note The Seventh Vacuum Microbalance Techniques Conference at the Eindhoven University of Technology, Netherlands, was the first to be held outside the U.S.A. The great number of participants and the lively discussions reflected the broad interest in this field in Europe. The Conference also demonstrated that the development of techniques persists in being the subject of many varied investi gations. Of the 23 papers presented at the Conference 21 have been in corporated in the present volume in alphabetical order of first auth ors' names. Contributions include descriptions of developments of unconventional weighing techniques (Gast and Poulis et aU and papers dealing with the simultaneous use of different weighing sys tems (Hillecke et aI.). The techniques of calibration (Schmider et aU and the different techniques used to eliminate weighing errors (Cutting, Kuhn et aI., Moret et aI., Pebler, and Robens et al.) are reported together with experimental data and theoretical discus sions. The multifarious applications of vacuum microbalances in scientific research are shown in papers concerning such fields as magnetic phenomena (Van den Bosch, Bransky et al., and Cini et aU and chemical reactions (Boudeulle et al., Cameron et aI., Clough et aI., Dovaston et aI., and Gulbransen et aI.) under widely diverging experimental conditions, e.g., temperature and gas pres sure. Other contributions - more or less of a synoptical nature - deal with vacuum system evaluation and the use of vacuum micro balances (Kollen et aI., Gregg, and Wiedemann), one paper (Dijkema et aU describing the microgravimetrical determination of diffusion coefficients in vapors. vii viii EDITORS' NOTE The editors are very grateful to Mrs. F. Duifhuis-Van Ton geren for her secretarial work and to Miss M. Gruyters for her share in the preparation of the graphic work. c. H. Massen H. J. van Beckum Contents Conference Participants. . . • . . . . . • . • . . • . . . . . . . . xiii Use of a Microbalance for the Determination of the Mass of Oxygen Reacting during the Oxidation of Thin Films of Binary Alloys. • . • • . • • . . • . . • • . . . . 1 M. Boudeulle, D. Durand, and p. Michel Static Magnetic Susceptibility Measurements on Small Solid Sample s . . • • • • • . • • • • • . • . • • • • • • . . • 9 A. Van den Bosch Measurements of Magnetic Thin-Film Parameters by the Use of an Automatic Microbalance ..•••.••.•• 19 Judith Bransky, I. Bransky, and A. A. Hirsch Activation Energies of the Decomposition of Poly(methyl O!-phenylacrylate) from Static and Dynamic TGA . . 27 G. G. Cameron and G. P. Kerr Apparatus for the Accurate Measurements of Magnetic Susceptibility with the Help of a Vacuum Electro- balance .••••.•.•.•....•.•.••..•••..• 37 R. Cini and M. Torrini Reduction Characteristics of Certain Oxides of Nickel and Uranium •..•••••.•••..• 51 0 • • • • • • • • • • P. S. Clough and Do Dollimore A Temperature Error in the Gravimetric Determina- tions of Adsorption Isotherms .••••••..•.••• 71 P. A. Cutting Determination of the Diffusion Coefficient of Vapors by Means of a Microbalance .••••••••.••••••• 79 K. M. Dijkema and J. C. Stouthart ix x CONTENTS Activation of Cellulose-Triacetate Carbon by Reaction with Carbon Dioxide: A Microgravimetric Study. 91 N. G. Dovaston and B. McEnaney Microweighing in Vacuo with the Aid of Vibrations of a Thin Band .•.•••.•.•....••...••••••.• 105 Th. Gast Some Uses of Wire-Suspended Microbalances 109 S. J. Gregg Oxidation in Flow-Reaction Systems . • • . . • • • • • . • • • 121 Earl A. Gulbransen, Fred A. Brassart, and Kenneth F. Andrew UHV Microbalance and Quartz Oscillator at Low Temperature s • . • • • . • • . . • • . . • • • . . . . • • . • 135 D. Hillecke and H. Mayer Dynamic Vacuum in Microbalance Chambers 145 W. Kollen and A. W. Czanderna Methods for the Elimination of Weighing Troubles Due to Convection in a Microbalance. • • • • • . . • • • • . 161 W. Kuhn, E. Robens, G. Sandstede, and G. Walter Comments on the Applications and Improvement of a UHV Microbalance. • • . . • • • • • • • . • . • • • • • • . 173 H. Moret, E. Louwerix, and E. Sattler A New Microbalance Technique for Kinetic Studies of Gas - Metal Reactions at High Temperatures . • • . 181 A. Pebler A Moving-Table Balance. • . . • • • • . • • • • • • • . . • • • • 187 J. A. Poulis, M. Verduin, J. P. de Mey, and C. H. Massen Fluctuations of the Weight Indicated by a Microbalance in the Pressure Range Between 1 and 103 torr with the Sample at a Lower Temperature than the Beam. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 195 E. Robens, G. Sandstede, G. Walter, and G. Wurzbacher