дткдтюм #р СИМШП CRVSTAL MIGiOBAlLANCiS С LU A.W. CZANDERNA Edited by

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1 дткдтюм #р СИМШП CRVSTAL MIGiOBAlLANCiS Edited by С LU Xinix, Incorporated 3350 Scott Boulevard, Building 31, Santa Clara, CA 95051, U.S.A. A.W. CZANDERNA Editor, Methods and Phenomena P.O. Box 27209, Denver, CO 80227, U.S.A. Volume 7 of Methods and Phenomena Their Applications in Science and Technology ELSEVIER Amsterdam - Oxford - New York - Tokyo 1984

CONTENTS Preface vii Chapter 1. Introduction, History, and Overview of Applications of Piezoelectric Quartz Crystal Microbalances, A. W. Czanderna and C. Lu 1 I. Introduction 1 П.

2 CONTENTS Preface vii Chapter 1. Introduction, History, and Overview of Applications of Piezoelectric Quartz Crystal Microbalances, A. W. Czanderna and C. Lu 1 I. Introduction 1 П. History of piezoelectric quartz crystal microbalances 2 A. Piezoelectric effect 2 B. Frequency control with quartz crystals 4 C. Relating changes in mass to frequency measurements 5 1. Theoretical developments, 5 2. Experimental progress, 5 3. Initial applications, 6 Ш. Overview of applications of piezoelectric quartz crystal microbalances... 7 A. Chapter 2, Theory and practice of the quartz crystal microbalance B. Chapter 3, Applications of quartz crystal microbalances for thin film deposition process control 8 C. Chapter 4, Stress effects in quartz crystal microbalances 9 D. Chapter 5, Simultaneous measurement of mass and temperature using quartz crystal microbalances 10 E. Chapter 6, Applications of quartz crystal microbalances in surface science 12 F. Chapter 7, Quartz crystal microbalances for plasma-assisted etching studies and applications 13 G. Chapter 8, Applications of quartz crystal microbalances in analytical chemistry 14 H. Chapter 9, Application of the quartz crystal microbalance to space system contamination studies 15 I. Chapter 10, Applications of quartz crystal microbalances in aerosol mass measurement 16 References 17 Chapter 2. Theory and Practice of the Quartz Crystal Microbalance, С Lu 19 I. Introduction 19 П. Piezoelectric quartz crystal resonators 20 A. Modes of vibration 20 B. Crystallographic orientation 21 C. Temperature dependence of the resonant frequency 23 D. Equivalent circuit 24 Ш. Theory of the piezoelectric quartz crystal microbalance 26 A. A linear frequency-to-mass equation for small mass loads 27 B. A linear period-to-mass approximation for extended mass loads 34 C. A general formula for mass determination by a quartz crystal microbalance 37 IV. The role of acoustic impedance in a quartz crystal microbalance 41 A. Experiments with different materials 41 B. Computation and estimation of acoustic impedance 46 C. Accumulated layers of different materials 49

X V. Design considerations for a quartz crystal microbalance 51 A. The quartz crystal and its supporting structures 51 B. Limit of mass load on a quartz crystal microbalance 54 C.

3 X V. Design considerations for a quartz crystal microbalance 51 A. The quartz crystal and its supporting structures 51 B. Limit of mass load on a quartz crystal microbalance 54 C. Quartz crystal microbalances for special environments 56 D. Associated electronics 57 VI. Conclusion 60 References 61 Chapter 3. Applications of Quartz Crystal Microbalances for Thin Film Deposition Process Control, H. K. Pulker and J. P. Decosterd 63 I. Introduction 63 П. Quartz crystal microbalances 64 A. Fundamentals 64 B. Differential mass sensitivity 68 C. Limiting factors to the accuracy and mass load Temperature, Mechanical stress and damping, Environmental influences, 78 Ш. Thin film monitoring with quartz crystal microbalances 79 A. Formation of films with reproducible characteristics Accuracy of measurement, Optical characteristics, Electrical characteristics, 84 B. Reliable measures for depositing films with correct and reproducible characteristics General considerations, Parameters for the production of optical films, Multilayer optical film systems, Quartz crystal monitor controlled deposition of optical multilayer systems, Quartz crystal monitor controlled deposition of electrical films, 103 C. Conclusions and measures to increase the reproducibility of film characteristics 109 IV. Control of an automatic deposition system using a quartz crystal monitor.. Ill A. General principles Ill 1. Principle steps of a thin film deposition process, Automation concept, 113 B. Realization of an automatic coating system Basic description, Quartz crystal monitor, 117 C. Final remarks 120 Acknowledgments 121 References 122 Chapter 4. Stress Effects in Quartz Crystal Microbalances, Errol P. EerNisse 125 I. Introduction 125 П. Origin of the stress effects 126 Ш. Magnitude of the stress effect for microbalance applications 129 IV. Simultaneous mass and stress measurements using the double resonator technique 134 A. Development of equations for Sf (df^, dfg) and Mj (dfд, dfg) 136 B. Sf and Mf for Au films bombarded with 45 kev Kr ions 137 C. Lateral stress in Si films bombarded with 220 kev Kr ions 140 V. Generalization of the double resonator technique 143 VI. Thermal shock effects in quartz resonator microbalances 146 Vn. The SC-cut as a microbalance 147 References 149 Chapter 5. Simultaneous Measurement of Mass and Temperature Using Quartz Crystal Microbalances, E. C. van Ballegooijen 151 I. Introduction 1S1

xi П. Electrode-tab resonator 153 Ш. Experimental equipment 159 A. Determination of the resonant frequencies 159 B. Determination of the mass 160 C. Determination of the temperature 162 IV.

4 xi П. Electrode-tab resonator 153 Ш. Experimental equipment 159 A. Determination of the resonant frequencies 159 B. Determination of the mass 160 C. Determination of the temperature 162 IV. Accuracy of the method 162 A. Reduction of errors Theoretical considerations, Experimental conditions, 167 Б. Experimental results 168 V. Optimized crystal cut 175 A. Mass coefficients a n and a B. Temperature coefficients a 12 and a a 177 C. The inaccuracies of 6aj; and 6WJ 178 VI. Summary 191 Glossary of definitions 193 References 194 Chapter 6. Applications of Quartz Crystal Microbalances in Surface Science, Leonard L. Levenson 197 I. Introduction 197 П. Chemisorption on single element thin films 198 Ш. Chemisorption and decomposition properties of compound thin films 203 IV. Physical adsorption and environmental applications 206 V. Molecular beam measurements 208 VI. Vapor pressure and outgassing studies 215 Vn. Summary 217 References 217 Chapter 7. Quartz Crystal Microbalances for Plasma-Assisted Etching Studies and Applications, J. W. Coburn 221 I. Introduction 221 П. In situ plasma studies 223 A. Plasma-assisted etching apparatus and terminology 223 B. Experimental aspects of operating a quartz crystal microbalance in a plasma environment Quartz crystal microbalance at ground potential with no energetic ion bombardment, Quartz crystal microbalance subjected to high energy ion bombardment, 227 C. Quartz crystal microbalance measurements in reactive gas plasmas Etch rate measurements, Polymerization rate measurements, 234 Ш. Nonplasma studies of plasma-related phenomena 235 A. Apparatus 235 Б. Ion-assisted gas-surface chemistry - an example of a quartz crystal microbalance application 238 C. Transient-like studies using the quartz crystal microbalance 240 D. Calibration of SIMS using a quartz crystal microbalance 247 Acknowledgments 248 References 249 Chapter 8. Applications of Quartz Crystal Microbalances in Analytical Chemistry, George G. Guilbault 251 I. Introduction 251 П. Experimental apparatus 252 Ш. Sorption detector 253 IV. Piezoelectric crystal detector for water 253 V. Detector for gas Chromatograph 255

Xll VI. Detector for liquid chromatography 257 Vn. Piezoelectric crystal detector for detection and determination of air pollutants 260 A. Detector for sulfur dioxide 260 B. Ammonia detectors 264 C.

5 Xll VI. Detector for liquid chromatography 257 Vn. Piezoelectric crystal detector for detection and determination of air pollutants 260 A. Detector for sulfur dioxide 260 B. Ammonia detectors 264 C. Detector for hydrogen sulfide 266 D. Detector for hydrogen chloride gas 266 E. Detector for organophosphorus compounds and pesticides 267 F. Detector for aromatic hydrocarbons 270 G. Detector for mercury in air 272 H. Detector for mononitrotoluene 272 I. Carbon monoxide detector 273 Vin. Determination of compounds in water 274 IX. Other applications 275 A. Microweighing with the quartz crystal detector 275 B. Piezoelectric crystals for residues in liquid and hydrogen 275 C. Miscellaneous applications 276 X. Instrumentation available commercially 277 XI. Conclusions 279 Acknowledgment 279 References 279 Chapter 9. Application of the Quartz Crystal Microbalance to Space System Contamination Studies, A. P. M. Glassford 281 I. Introduction 281 П. Evaluation of a commercial space-qualified quartz crystal microbalance A. System description 283 B. Evaluation experiments 287 С Data reduction Predicted evaporation rate of water, Quartz crystal microbalance sensitivity, Flow resistance of quartz crystal microbalance housing, Temperature measurement, 292 D. Comparison of experimental and predicted evaporation rate 293 Ш. Measurement of outgassing rate by the quartz crystal microbalance collection method 294 A. Introduction 294 B. The quartz crystal microbalance collection technique Test procedure, Measurement capability, 296 C. Measurement of diffusion properties Basic theory, Experimental procedure, Verification of the approach, 306 IV. Analysis of the species by heating the quartz crystal microbalance 308 A. Practical considerations Quartz crystal microbalance heating rate, Liquefaction of deposit, Loss of adhesion, Resolution problems in multispecies deposits, Deposit thickness, 315 B. Applications of the method Water/phenol/cresol mixtures, RTV 560 silicone adhesive, RTV 602 silicone potting compound, 323 V. Response of the quartz crystal microbalance to liquid deposits 325 A. Theoretical analysis Quartz crystal microbalance sensitivity considerations, Velocity distribution in the deposit, Derivation of response factor, 330 B. Experimental measurements Constant-deposit variable-temperature tests, Constant-temperature variable-deposit tests, 338 C. Discussion 340

Xlll VI. Condensation kinetics 341 Vn. Mass measurement on optical and thermal control surfaces 347 Acknowledgments 349 References 350 Chapter 10.

6 Xlll VI. Condensation kinetics 341 Vn. Mass measurement on optical and thermal control surfaces 347 Acknowledgments 349 References 350 Chapter 10. Applications of Quartz Crystal Microbalances in Aerosol Mass Measurement, Mat H. Ho 351 I. Introduction 351 П. Principles 353 A. Mass concentration of aerosol 353 B. Particle adhesion 356 Ш. Instrumentation 359 A. General description 359 B. Particle collection and deposition Impaction, Electrostatic Precipitation, Sampling, 364 C. Piezoelectric quartz crystal mass detector Piezoelectric crystal, Electronic system, Cleaning the sensing crystal, 366 IV. Performance characteristics of the piezoelectric quartz crystal microbalance for aerosol measurements 366 A. Mass response 367 B. Linear response 370 C. Collection and deposition of aerosol particles 373 D. Effects of temperature 376 E. Effects of humidity Effects on the crystal, Moisture affinity of deposited aerosols, 379 F. Effects of pressure 380 G. Calibration 381 V. Applications 382 VI. Conclusions 384 Acknowledgment 386 References 386 Index 389

PHYSICAL VAPOR DEPOSITION OF THIN FILMS

PHYSICAL VAPOR DEPOSITION OF THIN FILMS JOHN E. MAHAN Colorado State University A Wiley-Interscience Publication JOHN WILEY & SONS, INC. New York Chichester Weinheim Brisbane Singapore Toronto CONTENTS