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Processing by Centrifugation Processing by Centrifugation Edited by Liya L. Regel William R. Wilcox and Clarkson University Putsdam, New York Springer Science+Business Media, LLC Library of Congress Cataloging-in-Publication Data Processing by centrifugationledited by Liya Regal and William R. Wilcox. p. cm. Inc1udes bibliographical references. ISBN 978-1-4613-5195-5 ISBN 978-1-4615-0687-4 (eBook) DOI 10.1007/978-1-4615-0687-4 1. Materials-Effect of high gravity on-Congresses. 1. Regel', L. L. II. Wilcox. William R. III. International Workshop on Materials Processing in High Gravity (4th: 2000: Potsdam, N.Y.) TA417.7.H53 C47 2001 620.1 , 12-dc21 2001038547 Proceedings of the Fourth International Workshop on Materials Processing at High Gravity, held May 29-June 2, 2000, at Clarkson University, Potsdam, New York ISBN 978-1-4613-5195-5 ©2001 Springer Science+Business Media New York OriginaIly published by Kluwer AcademiclPlenum Publishers, New York in 2001 Softcover reprint ofthe hardcover Ist edition 2001 http://www.wkap.nl \0987654321 A C.I.P. record for this book is available from the Library of Congress AII rights reserved No part of this book may be reproduced, stored in a retrieval system, or transmitted in any form or by any means, electronic, mechanical, photocopying, microfilming, recording, or otherwise, without written permission from the Publisher "We judge ourselves by what we feel capable of doing, while others judge us by what we have already done." (Henry Wadsworth Longfellow) PREFACE Advances in every field of science and technology are no longer measured in centuries or decades, but in years and even months. They seem to surpass in attainments and scope anything that Man has achieved in the past. In the last decade of the 20th century we witnessed an upsurge in our knowledge of the important role played by gravity in materials processing. This knowledge was gained by experiments in orbiting spacecraft (microgravity) and on centrifuges (macrogravity), as well as by theoretical modeling. Our emphasis here is on research done on centrifuges and other rotating systems. The interest in centrifugal materials processing was largely stimulated by the mysterious results of the first experiments in 1987 with my colleague and friend Huguette Rodot from CNRS in Meudon. From the beginning, we both realized the attractive opportunity presented by the availahility of large centrifuges in Russia and in France for crystal growth and other materials processing. We both found it difficult to deal with the skeptical criticism from some of our colleagues, but that didn't deter us. Others began to find high gravity research interesting. Those of like mind gathered to discuss their results and thoughts in 1991 at the First International Workshop on Materials Processing at High Gravity at Dubna in Russia. Subsequently, three other workshops have been held at Clarkson University. I am also proud to mention here that the proceedings of the Third International Workshop on Materials Processing at High Gravity, published in book form as "Centrifugal Materials Processing" in 1997 by Plenum, received the Best Book Award from the International Academy of Astronautics in 1998 in Melbourne. This was wonderful recognition for all the researchers who have been contributed to this fascinating field. The present volume constitutes the proceedings of the exciting Fourth International Workshop on Materials Processing at High Gravity, held at Clarkson University May 29 to June 2, 2000. There were more than 75 attendees from 16 countries. Since the topics extended well beyond materials processing, it was felt appropriate to name this proceedings "Processing by Centrifugation." It includes applications of the traditional bench-scale centrifuges, but also all rotating systems utilizing the centrifugal and Coriolis forces to provide unique performance. Centrifugation on a bench-scale apparatus led to the formation of sticky, porous Teflon membranes, as well as improved v polymeric solar cells. Centrifugation on large equipment improved the chemical vapor deposition of diamond films, influenced the growth and dissolution of semiconductor crystals, and elucidated the influence of gravity on coagulation of colloidal Teflon. A million-g centrifuge was constructed and used to study sedimentation in solids and to prepare compositionally graded materials and new phases. Rotation of a pipe about its axis allowed the casting of large-diameter metal alloy pipes as well as coating the interior of pipes with a cermet utilizing self-propagating high-temperature synthesis. Such coatings are highly corrosion and erosion resistant. Flow on a rotating disk was shown to be useful for process intensification, e.g. large-scale manufacturing of nano particles, polymerization reactions, and heat & mass transfer. Several theoretical studies dealt with the influence of rotation on fluid convection on surfaces and in pipes, tubes, and porous media. These have applications to integrated-circuit chip manufacturing, alloy casting, oil production, crystal growth, and the operation of rotating machinery. While I was researching, writing, planning, conceptualizing, organizing, and talking to all contributors, many friends were at my side. The close professional association with all contributors provided the most rewarding and the richest experience arising from hosting this successful fourth international conference and following up with this fourth proceedings. In editing the papers, we made every effort to retain the authors' syntactic and verbal texture, while seeking consistency and readability. All authors strove to convey the flavor of their excellent presentations. lowe them a special thanks for their skill and insight, and for making the collaboration such a pleasure. This book is theirs. All aspects of the work on this volume were done equally by Bill Wilcox and me; the order of our names as editors is purely alphabetical. We greatly appreciate the financial support. of the U.S. National Science Foundation, the Petroleum Research Fund of the American Chemical Society, Coming Corporation, and the New York State Center for Advanced Materials Processing at Clarkson University. We are grateful to those at Clarkson University who so competently handled meeting facilities, housing, etc. Our graduate students particularly deserve awards for helping attendees 'With travel, setup of projection equipment, entertainment after the banquet, and innumerable other tasks. Our apologies to those whose contributions we have overlooked. The continual encouragement and support of my family and my friends are deeply and sincerely appreciated. My heartfelt thanks TO my mother for everything she did for me. She was more than the usual patient and understanding parent. I'm very sorry she couldn't see this new book. Liya L. Regel. Chair of Workshops and Co-Editor International Center for Gravity Materials Science and Applications Clarkson University Potsdam NY 13699-5814 USA vi CONTENTS Vibration during Centrifugation ....................................................................................... 1 L.L. Regel, W.R. Wilcox, R. Derebail, and P.V. Skudamov Application of the Spinning-Disc Technology for Process Intensification in the Chemical Process Industry ........................................ 7 K.V.K. Boodhoo and R.J.J. lachuck Synthesis and Application of NanoparticIes by Multiphase Reactive Precipitation in a High-Gravity Reactor: I: Experimental ........................ 19 1. Chen and Y. Wang Synthesis and Application of Nanoparticles by Multiphase Reactive Precipitation in a High-Gravity Reactor: II: Modeling ............................. 29 Y. Wang and 1. Chen Spreading of a Thin Liquid Drop under the Influence of Gravity, Rotation and Non-Uniform Surface Tension ............................................. 37 E. Momoniat Recovery of Diluted Components from Large Aqueous Streams by an Extremely Compact, Centrifugal Countercurrent Adsorption System .............. 45 L.A.M. van der Wielen, M.A.T. Bisschops and K.Ch.A.M. Luyben Gas-Phase Mass Transfer in a Centrifugal Gas-Liquid Contactor with a Stack of Flexible Disks as Packing ........................... 51 R. Mukherjee, D. Deb, P. Sandilya and D. P. Rao Analytical Ultracentrifugation: A Valuable Tool to Recognize Crystallization Conditions of Proteins ..................................... 61 1. Behlke and O. Ristau The Effect of Centrifugation on the Composition, Structure and Properties of Ionic Compound Crystals ........................................... 71 S.P. Nikanorov, V.N. Gurin, L.I. Derkachenko, A.P. Nechitailov, LN. Zimkin, Z.L Uspenskaya,V.N. Osipov, M.M. Korsukova, and L.L. Regel vii Alteration of the Chemical Composition of Solid Solutions and Eutectics by Centrifugation ....................................................... 77 V.N. Gurin, S.P. Nikanorov, A.P. Nechitailov, V.N. Osipov, Z.I. Uspenskaya, M.M. Korsukova, and L.L. Regel Dissolution Rate of GaP Crystal on a Centrifuge .............................................................. 83 Y. Inatomi, K Horiuchi, and K Kuribayashi Influence of Centrifugation on the Conductivity of Poly-N-Epoxypropylcarbazole -Copper Phthalocyanine Films Deposited from Solution ......................................... 93 K Karimov, K Akhmedov, M. Mahroof-Tahir, R.M. Gul, and A. Ashurov Physical Vapor Transport of CuPc Organic Thin Films in High Gravity .......................... 99 K Karimov, S. BeIlingeri, and Y. Abe Diamond Synthesized by DC-Plasma CVD at High Gravity ........................................... 107 M. Nakazato, T. Suzuki, Y. Nagasaka, Y. Abe, S. BeIlingeri, and G. Maizza Influence of Centrifugation on Diamond Film Deposition by Chemical Vapor Transport ....................................................... 113 L.L. Regel and W.R. Wilcox Polymer Synthesis in a Centrifugal Field ......................................................................... 121 KG. Kostarev and A.V. Shmyrov Utilization of Microgravity and High Gravity to Prepare Materials with ControIled Properties ...................................................... 127 V.A. Briskman, KG. Kostarev, and A.V. Shmyrov Influence of Centrifugation on Coagulation of CoIloidal Dispersions of Teflon™ .......... 133 J. Simmons, L.L. Regel, W.R. Wilcox, and R. Partch Boundary Conditions in Diffusional Growth and Sedimentation ..................................... 141 V. Privman and 1. Park Simulation of Sedimentation of Atoms in a Binary Alloy in Strong Gravity ................... 149 M. Ono and T. Mashimo Mega-Gravity Experiment on In-Pb Alloy ....................................................................... 155 T. Mashimo, M. Ono, T. Kinoshita and H. Kanegae Molecular Gradation in Glass by Using High Gravity: A Novel Method for Si-Ti Graded-Glass Preparation .............................................. 159 M. Nishihara, H. Ihara, T. Sagawa, R. Nishimura, S. Matsuzaki and T. Mashimo High-Velocity Sedimentation to Determine Conformational and Hydrodynamic Parameters of NitroceIlulose Macromolecules .......................... 163 V.A. Malchevsky viii Mechanical Properties of Nitrocellulose Composite Materials ........................................ 171 V.A. Malchevsky Centrifugal Casting of AI-25%w Cu Alloy with Electromagnetic Stirring and Water Cooling ............................................................ 177 W. Zhang, Y. Yang, and Z. Hu The Influence of High Artificial Gravity on SHS Processes ............................................ 185 V.I. Yukhvid, V.N. Sanin, and A.G. Merzhanov Self-Propagating High-Temperature Centrifugal Processing of Cu 0-Cu-AI and Cu 0-AI Systems .............................. 201 2 2 A.S. Rogachev, V.N. Sanin, A.E. Sytschev, V.1. Yukhvid, E. Medda, R. Orru, and G. Cao Centrifugal-Thermit Process for Production of Composite Pipes of Various Sizes ......... 213 E. Miyazaki and O. Odawara Ceramic-Lined Composite Pipes Produced by the GS-T SHS Process with Mechanical Vibration ................................................. 223 J. Wang, Z. Zhao, M. Ye, X. Du, and J. Wen Directional Solidification of Aluminum and Lead in a Centrifuge .................................. 231 Sh. Mavlonov and H. Shodiev Physico-Chemical Analysis under Conditions of High Gravity ....................................... 235 Sh. Mavlonov and H. Shodiev Defect Formation in Tellurium at Different Gravitational Levels .................................... 241 L.L. Regel, R.V. Parfeniev, 1.1. Farbshtein, I.L. Shulpina, S.V. Yakimov, V.P. Shalimov, and A.M. Turchaninov Influence of Centrifugation on Furnace Temperature Distribution and Freezing Rate of InSb using the Gradient Freeze Technique ............................. 253 I.L. Moskowitz, L.L. Regel, and W.R. Wilcox Effects of Rotation on Transport Processes during Crystal Growth by Solidification ..... 259 C.W.Lan Numerical Modeling and Flow Visualization in the Gradient Freeze Configuration during Centrifugation .............................................. 273 P.V. Skudarnov, L.L. Regel, W.R. Wilcox, and G. Ahmadi Pattern Formation in Natural Convection in a Rotating Container ................................... 287 M. Vargas, E. Ramos, F.Z. Sierra, and A.A. Avramenko Non-Axisymmetric Chimney Convection in a Mushy Layer under a High Gravity Environment .................................................. 295 D.N. Riahi ix Viscous Fingering in a Rotating Porous Medium ............................................................. 303 M.Z. Saghir, H.H. Vaziri and M.R. Islam Magnetohydrodynamic Effects in High Gravity Convection during Alloy Solidification .................................................................... 317 D.N. Riahi Body-Force-Driven Multiplicity and Stability of Combined Free and Forced Convection in Rotating Curved Ducts: Centrifugal Force ............. 325 L. Wang and T. Yang Visualization of Flows in Channels with Curvature and Rotation ................................... 339 L. Wang and K.c. Cheng Effect of High Gravity on the Solid-Liquid Interfacial Free Energy ............................... 361 C. Patuelli and R. Tognato Mechanical Behavior of Energetic Materials at High Acceleration ................................. 367 Y. Lanzerotti and J. Sharma Index ................................................................................................................................. 371 x VIBRATION DURING CENTRIFUGATION Liya L. Regel, William R. Wilcox, Ramnath Derebail,l and Peter V. Skudarnov2 International Center for Gravity Materials Science and Applications Clarkson University, Potsdam, NY 13699-5814, USA INTRODUCTION Vibration is of concern in many experiments. For example, low-frequency acceleration influences buoyancy-driven convection. If there are two fluid phases present, vibration can cause oscillation of the interface between them, thereby pumping the adjacent fluids. High frequency vibrations can be transmitted through the container walls to cause streaming of the fluid and, in addition, move second-phase particles relative to the fluid. There are several sources of vibration in centrifuges. Here, we are concerned with the experiment package on large centrifuges operating in the open atmosphere. We offer as an example our experience on the Clarkson centrifuge HIRB. ,2 A tube furnace was placed in a box, 30.5 cm X 30.5 cm X 25.4 cm, that was attached by a hinge to the centrifuge arm so as to maintain the net acceleration vector approximately aligned with the axis of the furnace. A triaxial accelerometer was placed within this 20 kg package. The attachment hinge was 1.65 m from the center of rotation. At accelerations from 2 to 5 g , vibration was observed mainly at 17 Hz in the direction of rotation, with a maximum amplitude at 5 g. This was most likely due to periodic vortex shedding that became locked-in to the mechanical resonance frequency (17 Hz) of the system. SOURCES OF VIBRATION Laboratory Vibrations Vibrations are present in all laboratories and these can be transmitted through the centrifuge to the experiment package. Figure 1 shows accelerometer readings taken while our centrifuge was stationary. On the left are the raw data for the three axes. The corresponding spectral power densities are on the right. Vibrations of almost 0.1 g occurred in the y and z directions primarily at -225 Hz and secondarily at -420 Hz. J Current address: Agilent Technology, San Jose, CA 95131-1008. 2 Current address: Florida International University, Miami, FL 33174. Processing by Centrifugation, Edited by Regel and Wilcox Kluwer Academic/Plenum Publishers, New York, 2001

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