MATERIALS RESEARCH SOCIETY SYMPOSIUM PROCEEDINGS VOLUME 188 Thin Films: Stresses and Mechanical Properties II Symposium held April 16-19, 1990, San Francisco, California, U.S.A. EDITORS: M. F. Doerner IBM General Products Division, San Jose, California, U.S.A. W. C. Oliver Oak Ridge National Laboratory, Oak Ridge, Tennessee, U.S.A. G. M. Pharr Rice University, Houston, Texas, U.S.A. F. R. Brotzen Rice University, Houston, Texas, U.S.A. IM1RTSI MATERIALS RESEARCH SOCIETY Pittsburgh, Pennsylvania
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Contents PREFACE xi ACKNOWLEDGMENTS xiii MATERIALS RESEARCH SOCIETY SYMPOSIUM PROCEEDINGS xiv PART I: STRESSES: MEASUREMENT AND THEORY STRESSES IN PASSIVATED FILMS 3 Paul A. Flinn FINITE ELEMENT CALCULATIONS OF THERMAL STRESSES IN PASSIVATED AND UNPASSIVATED LINES BONDED TO SUBSTRATES 15 Anne I. Sauter and W.D. Nix DEFLECTION SHAPES DUE TO INTRINSIC STRESS IN THIN FILMS 21 Christine B. Masters, N.J. Salamon, and D.E. Fahnline MEASUREMENT OF STRESSES IN THIN FILMS USING HOLOGRAPHIC INTERFEROMETRY: DEPENDENCE ON ATMOSPHERIC CONDITIONS 29 Michele A. Maden, Kun Tong, and Richard J. Farris A VIBRATIONAL TECHNIQUE FOR STRESS MEASUREMENT IN FILMS 35 A. Jagota, S. Mazur, and R.J. Farris THE IN-SITU MEASUREMENT OF BIAXIAL MODULUS AND RESIDUAL STRESS OF MULTI-LAYER POLYMERIC THIN FILMS 41 Pinyen Lin and Stephen D. Senturia ANALYSIS OF STRESS VARIATIONS IN EPITAXIAL FILMS USING CATHODOLUMINESCENCE MICROSCOPY AND SPECTROSCOPY 47 B.G. Yacobi and P. Sheldon NON-DESTRUCTIVE ASSESSMENT OF THIN FILM STRESSES AND CRYSTAL QUALITY OF SILICON ON INSULATOR MATERIALS WITH RAMAN SPECTROSCOPY 53 Ingrid De Wolf, Jan Vanhellemont, and Herman E. Maes PART II: STRESSES: PROCESSING AND MICROSTRUCTURAL EFFECTS IN SITU STRESS MEASUREMENTS DURING THE FORMATION OF TiSi 2 C49 ON Si WAFERS J.F. Jongste, G.C.A.M. Janssen, and S, Radelaar Invited Paper
IN SITU STUDY OF STRESSES GENERATED DURING THE FORMATION OF COBALT DISILICIDE AND THE EFFECT OF POST SILICIDE PROCESSING 67 A.R. Sitaram, J.C. Kalb, Jr., and S.P. Murarka PLASMA ENHANCED CHEMICAL VAPOR DEPOSITION OF DIELECTRIC FILMS: CORRELATION OF STRESS TO FILM STRUCTURE AND PLASMA CHARACTERISTICS 73 Radhika Srinivasan, B.C. Nguyen, and A.P. Short CORRELATION BETWEEN PROCESSING, COMPOSITION, AND MECHANICAL PROPERTIES OF PECVD-SiN x THIN FILMS 79 D.C.H. Yu and J.A. Taylor INTRINSIC STRESS OF PECVD SILICON OXYNITRIDE FILMS DEPOSITED IN A HOT-WALL REACTOR 85 K. Aite and R. Koekoek STRESSES IN AMORPHOUS Gd-Fe ALLOY THIN FILMS DEPOSITED BY MAGNETRON SPUTTERING 91 Zhi-Feng Zhou, Qi-Gang Zhou, and Yu-Dian Fan INTERNAL STRESSES AND ADHESION PROPERTIES OF FILM/ SUBSTRATE INTERFACES 97 M. Ignat, A. Chouaf, and Ph. Normandon TEMPERATURE DEPENDENCE OF STRESS FOR COPPER, COPPER-SILVER AND COPPER-TIN FILMS 103 Richard Haynes PART III: MICROINDENTATION *THE INFLUENCE OF ION IMPLANTATION ON THE NEAR-SURFACE MECHANICAL PROPERTIES OF CERAMICS 111 C.J. McHargue, M.E. O'Hern, and D.L. Joslin MECHANICAL PROPERTIES OF CARBON-IMPLANTED NIOBIUM 121 S.J. Zinkle and J.S. Huang MECHANICAL PROPERTIES OF COATINGS AND INTERFACES 127 B.D. Fabes and W.C. Oliver MECHANICAL PROPERTIES OF SILICA COATINGS 133 Kenneth D. Cornett, B.D. Fabes, and W.C. Oliver THE HARDNESS AND ELASTIC MODULUS OF TiN FILMS AS DETERMINED BY ULTRA-LOW LOAD INDENTATION 139 M.E. O'Hern, W.C. Oliver, C.J. McHargue, D.S. Rickerby, and S.J. Bull PART IV: TIME DEPENDENT DEFORMATION DETERMINATION OF ELASTIC CONSTANTS AND VISCOSITY OF AMORPHOUS THIN FILMS FROM SUBSTRATE CURVATURE 147 Ann Witvrouw and Frans Spaepen *Invited Paper
X-RAY STRESS STUDIES OF PASSIVATED AND UNPASSIVATED NARROW ALUMINUM METALLIZATIONS 153 C.A. Paszkiet, M.A. Korhonen, and Che-Yu Li MEASUREMENT OF STRESS RELAXATION IN THIN ALUMINUM METALLIZATIONS BY CONTINUOUS INDENTATION AND X-RAY TECHNIQUES 159 M.A. Korhonen, W.R. LaFontaine, C.A. Paszkiet, R.D. Black, and Che-Yu Li INDENTATION LOAD RELAXATION EXPERIMENTS ON Al-Si METALLIZATIONS 165 W.R. LaFontaine, B. Yost, R.D. Black, and Che-Yu Li CREEP BEHAVIOR OF SPUTTERED TiN FILMS USING INDENTATION TESTING 171 V. Raman and R. Berriche MECHANICAL PROPERTIES OF THIN FILM ALUMINUM FIBERS: GRAIN SIZE EFFECTS 177 James E. Steinwall and H.H. Johnson STUDYING MECHANICAL PROPERTIES OF THIN FILMS UNDER HIGH PRESSURES 183 B.C. Cai, D. Kuhlmann-Wilsdorf, and R.B. Nelson PART V: TRIBOLOGY *MICROSCRATCH TEST FOR ULTRA-THIN FILMS 191 T.W. Wu MICROSCRATCH TEST ON CARBON FILMS AS THIN AS 20 nm 207 T.W. Wu, A.L. Shull, and J. Lin MECHANICAL PROPERTIES OF CARBON FILMS FOR THIN FILM DISKS 213 Richard L. White, Mary F. Doerner, and George W. Walker NANOTRIBOLOGY OF DIAMOND FILMS STUDIED BY ATOMIC FORCE MICROSCOPY 219 Gabi Neubauer, Sidney R. Cohen, Gary M. McClelland, and Hajime Seki ION BEAM ANNEALING OF VAPOR-DEPOSITED CARBON FILM 225 Kazuo Higuchi, Shoji Noda, Sumiko Iritani, Tomoji Ishiguro, and Osami Kamigaito DIAMOND-LIKE FILMS AS OPTICAL AND PROTECTIVE COATINGS 231 D. Das Gupta, F. Demichelis, R. Spagnolo, and A. Tagliaferro EXPERIMENTS ON, AND A TWO-COMPONENT MODEL FOR, THE BEHAVIOR OF WATER NANO-FILMS ON METALS 237 Chao Gao and D. Kuhlmann-Wilsdorf Invited Paper vii
PART VI: FRACTURE AND ADHESION MEASUREMENT OF INTERFACE STRENGTH BY LASER PULSE INDUCED SPALLATION 245 V. Gupta and A.S. Argon COMPRESSIVE STRESSES, BUCKLING AND SPALLING OF TUNGSTEN LPD FILMS 251 Aidan Borer and Brian Derby CRACKING AND DELAMINATION OF VAPOUR-DEPOSITED TANTALUM FILMS 257 R.M. Fisher, J.Z. Duan, and J.B. Liu INDENTATION FRACTURE OF BRITTLE MATERIALS 263 Barry N. Lucas, W.C. Oliver, and J.J. Wert MOLECULAR DYNAMICS COMPUTER SIMULATION OF THE RUPTURE OF THE TWO-DIMENSIONAL LENNARD-JONES FILM 269 John F. Maguire and Chun-Pok Leung FRACTURE-EXAFS: A NEW METHOD FOR THE STUDY OF INTERFACES IN THIN FILMS AND POLYCRYSTALLINE MATERIALS 275 E.V. Barrera, Benji Maruyama, and S.M. Heald PROPERTIES OF A SUBMICRON-HONEYCOMB THIN FILM 281 R.C. Furneaux, J.S. Crompton, and D.J. Fitchett PART VII: MULTILAYERS MECHANICAL PROPERTIES OF COMPOSITIONALLY MODULATED Au-Ti THIN FILMS USING INDENTATION AND MICROBEAM DEFLECTION TECHNIQUES 289 Shefford P. Baker, Alan F. Jankowski, Soonil Hong, and William D. Nix MECHANICAL PROPERTIES OF MULTILAYERED COPPER-NICKEL THIN FILMS MEASURED BY INDENTATION TECHNIQUES 295 T.E. Schlesinger, R.C. Cammarata, C. Kim, S.B. Qadri, and A.S. Edelstein TRIBOLOGICAL AND MECHANICAL PROPERTIES OF Fe/Ti MULTILAYERED FILMS 301 M. Nastasi, J-P. Hirvonen, T.R. Jervis, and S.N. Basu THE MECHANICAL PROPERTIES OF Cu/TiB 2 MULTILAYER STRUCTURES 307 Kevin M. Hubbard, S.N. Basu, J-P. Hirvonen, T.R. Jervis, and M. Nastasi PART VIII: MICROSTRUCTURE AND DEFECTS MECHANISMS AND KINETICS OF MISFIT DISLOCATION FORMATION IN HETEROEPITAXIAL THIN FILMS 315 W.D. Nix, D.B. Noble, and J.F. Turlo *Invited Paper viii
MECHANICAL PROPERTIES OF NANOCOMPOSITE COATINGS FABRICATED BY SPUTTERING 331 G.M. Chow, R.L. Holtz, C.Cm. Wu, A.S. Edelstein, T.E. Schlesinger, and R.C. Cammarata *HARD COATINGS 337 S.J. Bull and D.S. Rickerby PHOTOREFLECTANCE CHARACTERIZATION OF SILICON FILMS ON INSULATOR 349 Adriana Giordana, R. Glosser, Joseph G. Pellegrino, S. Qadri, M.E. Twigg, E.D. Richmond, Keith Joyner, and Gordon Pollack STRUCTURAL DEPENDENCE OF THE ELASTIC CONSTANTS OF POLYMERIC LANGMUIR-BLODGETT FILMS STUDIED USING BRILLOUIN SCATTERING 355 Sukmock Lee, J.R. Dutcher, B. Hillebrands, G.I. Stegeman, W. Knoll, G. Duda, G. Wegner, and F. Nizzoli AUTHOR INDEX 361 SUBJECT INDEX 363 MATERIALS RESEARCH SOCIETY SYMPOSIUM PROCEEDINGS 365 *Invited Paper
Preface This volume is a compilation of papers presented at the 1990 Spring Meeting of the Materials Research Society in a symposium entitled "Thin Films: Stresses and Mechanical Properties II". As indicated by the title, the symposium was the second in a series, the first of which was held at the Fall Meeting in 1988. Interest in thin film mechanical properties continues to grow. The symposium was attended by a large international audience representing universities, national laboratories and industry who presented basic and applied research results in fields such as semiconductor technology, magnetic recording technology, and hard coating technology. The importance of thin film mechanical properties in these fields is now recognized to the extent that basic characterization techniques such as microindentation and thin film stress measurement are performed routinely, and new characterization techniques are being developed on a daily basis. Many of the papers in the symposium dealt with the developments in these characterization methods and their application to a broad spectrum of materials such as compositionally modulated structures, ion implanted materials, optical coatings, and the numerous metals, ceramics and organics used in semiconductor device manufacture. The editors are encouraged by the rapidly growing interest in thin film mechanical properties. It is hoped that this volume will be useful to newcomers to the field, as well as stimulate new ideas for those who are already familiar with it. Mary F. Doerner Warren C. Oliver George M. Pharr Franz R. Brotzen June 1990
Acknowledgments The editors gratefully acknowledge financial support provided by: Nano Instruments, Inc. Knoxville, Tennessee IBM General Products Division San Jose, California UltraTherm, Inc. Kingston, Tennessee Oak Ridge National Laboratory Oak Ridge, Tennessee The organizational and typing assistance provided by Ms. Gwen Sims, Oak Ridge National Laboratory, is also appreciated. Mary F. Doerner Warren C. Oliver George M. Pharr Franz R. Brotzen June 1990 xiii
MATERIALS RESEARCH SOCIETY SYMPOSIUM PROCEEDINGS Recent Materials Research Society Symposium Proceedings Volume 157 Beam-Solid Interactions: Physical Phenomena, J.A. Knapp, P. Borgesen, R.A. Zuhr, 1989, ISBN 1-55899-045-3 Volume 158 In-Situ Patterning: Selective Area Deposition and Etching, R. Rosenberg, A.F. Bernhardt, J.G. Black, 1989, ISBN 1-55899-046-1 Volume 159 Atomic Scale Structure of Interfaces, R.D. Bringans, R.M. Feenstra, J.M. Gibson, 1989, ISBN 1-55899-047-X Volume 160 Layered Structures: Heteroepitaxy, Superlattices, Strain, and Metastability, B.W. Dodson, LJ. Schowalter, J.E. Cunningham, F.H. Pollak, 1989, ISBN 1-55899-048-8 Volume 161 Properties of II-VI Semiconductors: Bulk Crystals, Epitaxial Films, Quantum Well Structures and Dilute Magnetic Systems, J.F. Schetzina, F.J. Bartoli, Jr., H.F. Schaake, 1989, ISBN 1-55899-049-6 Volume 162 Diamond, Boron Nitride, Silicon Carbide and Related Wide Bandgap Semiconductors, J.T. Glass, R.F. Messier, N. Fujimori, 1989, ISBN 1-55899-050-X Volume 163 Impurities, Defects and Diffusion in Semiconductors: Bulk and Layered Structures, J. Bernholc, E.E. Haller, DJ. Wolford, 1989, ISBN 1-55899-051-8 Volume 164 Materials Issues in Microcrystalline Semiconductors, P.M. Fauchet, C.C. Tsai, K. Tanaka, 1989, ISBN 1-55899-052-6 Volume 165 Characterization of Plasma-Enhanced CVD Processes, G. Lucovsky, D.E. Ibbotson, D.W. Hess, 1989, ISBN 1-55899-053-4 Volume 166 Neutron Scattering for Materials Science, S.M. Shapiro, S.C. Moss, J.D. Jorgensen, 1989, ISBN 1-55899-054-2 Volume 167 Advanced Electronic Packaging Materials, A. Barfknecht, J. Partridge, C-Y. Li, CJ. Chen, 1989, ISBN 1-55899-055-0 Volume 168 Chemical Vapor Deposition of Refractory Metals and Ceramics, T.M. Besmann, B.M. Gallois, 1989, ISBN 1-55899-056-9 Volume 169 High Temperature Superconductors: Fundamental Properties and Novel Materials Processing, J. Narayan, C.W. Chu, L.F. Schneemeyer, D.K. Christen, 1989, ISBN 1-55899-057-7 Volume 170 Tailored Interfaces in Composite Materials, C.G. Pantano, EJ.H. Chen, 1989, ISBN 1-55899-058-5 Volume 171 Polymer Based Molecular Composites, D.W. Schaefer, J.E. Mark, 1989, ISBN 1-55899-059-3 Volume 172 Optical Fiber Materials and Processing, J.W. Fleming, G.H. Sigel, S. Takahashi, P.W. France, 1989, ISBN 1-55899-060-7 Volume 173 Electrical, Optical and Magnetic Properties of Organic Solid-State Materials, L.Y. Chiang, D.O. Cowan, P. Chaikin, 1989, ISBN 1-55899-061-5 Volume 174 Materials Synthesis Utilizing Biological Processes, M. Alper, P.D. Calvert, P.C. Rieke, 1989, ISBN 1-55899-062-3 Volume 175 Multi-Functional Materials, D.R. Ulrich, F.E. Karasz, A.J. Buckley, G. Gallagher-Daggitt, 1989, ISBN 1-55899-063-1 Volume 176 Scientific Basis for Nuclear Waste Management XIII, V.M. Oversby, P.W. Brown, 1989, ISBN 1-55899-064-X Volume 177 Macromolecular Liquids, C.R. Safinya, S.A. Safran, P.A. Pincus, 1989, ISBN 1-55899-065-8 Volume 178 Fly Ash and Coal Conversion By-Products: Characterization, Utilization and Disposal VI, F.P. Glasser, R.L. Day, 1989, ISBN 1-55899-066-6
MATERIALS RESEARCH SOCIETY SYMPOSIUM PROCEEDINGS Volume 179 Specialty Cements with Advanced Properties, H. Jennings, A.G. Landers, B.E. Scheetz, I. Odler, 1989, ISBN 1-55899-067-4 Volume 180 Better Ceramics Through Chemistry IV, C.J. Brinker, D.E. Clark, D.R. Ulrich, B.J.J. Zelinsky, 1990, ISBN: 1-55899-069-0 Volume 181 Advanced Metallizations in Microelectronics, A. Katz, S.P. Murarka, A. Appelbaum, 1990, ISBN: 1-55899-070-4 Volume 182 Polysilicon Thin Films and Interfaces, B. Raicu, T.Kamins, C.V. Thompson, 1990, ISBN: 1-55899-071-2 Volume 183 High-Resolution Electron Microscopy of Defects in Materials, R. Sinclair, DJ. Smith, U. Dahmen, 1990, ISBN: 1-55899-072-0 Volume 184 Degradation Mechanisms in III-V Compound Semiconductor Devices and Structures, V. Swaminathan, SJ. Pearton, O. Manasreh, 1990, ISBN: 1-55899-073-9 Volume 185 Materials Issues in Art and Archaeology II, J.R. Druzik, P.B. Vandiver, G. Wheeler, 1990, ISBN: 1-55899-074-7 Volume 186 Alloy Phase Stability and Design, G.M. Stocks, D.P. Pope, A.F. Giamei, 1990, ISBN: 1-55899-075-5 Volume 187 Thin Film Structures and Phase Stability, B.M. Clemens, W.L. Johnson, 1990, ISBN: 1-55899-076-3 Volume 188, W.C. Oliver, M. Doerner, G.M. Pharr, F.R. Brotzen, 1990, ISBN: 1-55899-077-1 Volume 189 Microwave Processing of Materials II, W.B. Snyder, W.H. Sutton, D.L. Johnson, M.F. Iskander, 1990, ISBN: 1-55899-078-X Volume 190 Plasma Processing and Synthesis of Materials III, D. Apelian, J. Szekely, 1990, ISBN: 1-55899-079-8 Volume 191 Laser Ablation for Materials Synthesis, D.C. Paine, J.C. Bravman, 1990, ISBN: 1-55899-080-1 Volume 192 Amorphous Silicon Technology, P.C. Taylor, M.J. Thompson, P.G. LeComber, Y. Hamakawa, A. Madan, 1990, ISBN: 1-55899-081-X Volume 193 Atomic Scale Calculations of Structure in Materials, M.A. Schluter, M.S. Daw, 1990, ISBN: 1-55899-082-8 Volume 194 Intermetallic Matrix Composites, D.L. Anton, R. McMeeking, D. Miracle, P. Martin, 1990, ISBN: 1-55899-083-6 Volume 195 Physical Phenomena in Granular Materials, T.H. Geballe, P. Sheng, G.D. Cody, 1990, ISBN: 1-55899-084-4 Volume 196 Superplasticity in Metals, Ceramics, and Intermetallics, M.J. Mayo, J. Wadsworth, M. Kobayashi, A.K. Mukherjee, 1990, ISBN: 1-55899-085-2 Volume 197 Materials Interactions Relevant to the Pulp, Paper, and Wood Industries, J.D. Passaretti, D. Caulfield, R. Roy, V. Setterholm, 1990, ISBN: 1-55899-086-0 Volume 198 Epitaxial Heterostructures, D.W. Shaw, J.C. Bean, V.G. Keramidas, P.S. Peercy, 1990, ISBN: 1-55899-087-9 Volume 199 Workshop on Specimen Preparation for Transmission Electron Microscopy of Materials II, R. Anderson, 1990, ISBN: 1-55899-088-7 Volume 200 Ferroelectric Thin Films, A.I. Kingon, E.R. Myers, 1990, ISBN: 1-55899-089-5 Earlier Materials Research Society Symposium Proceedings listed in the back.