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Handbook of physical vapor deposition (PVD) processing : film formation, adhesion, surface preparation and contamination control PDF

943 Pages·1998·7 MB·English
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HANDBOOK OF PHYSICAL VAPOR DEPOSITION (PVD) PROCESSING Film Formation, Adhesion, Surface Preparation and Contamination Control by Donald M. Mattox Society of Vacuum Coaters Albuquerque, New Mexico NOYES PUBLICATIONS np Westwood, New Jersey, U.S.A. Copyright © 1998 by Noyes Publications No part of this book may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying, recording or by any information storage and retrieval system, without permission in writing from the Publisher. Library of Congress Catalog Card Number: 97-44664 ISBN: 0-8155-1422-0 Printed in the United States Published in the United States of America by Noyes Publications 369 Fairview Avenue, Westwood, New Jersey 07675 10 9 8 7 6 5 4 3 2 1 Library of Congress Cataloging-in-Publication Data Mattox, D. M. Handbook of physical vapor deposition (PVD) processing / by Donald M. Mattox. p. cm. Includes bibliographical references and index. ISBN 0-8155-1422-0 1. Vapor-plating--Handbooks, manuals, etc. I. Title. TS695.M38 1998 671.7'35--dc21 97-44664 CIP Dedication To my wife Vivienne Without Vivienne’s constant support, encouragement, and editorial assistance, this book would not exist. Her wide spectrum of contacts within the vacuum equipment and PVD technology industries has made the accumulation of information in some sections of this book possible. v NOTICE To the best of our knowledge the information in this publication is accurate; however the Publisher does not assume any responsibil- ity or liability for the accuracy or completeness of, or consequences arising from, such information. This book is intended for informational purposes only. Mention of trade names or commercial products does not constitute endorsement or recommendation for use by the Publish- er. Final determination of the suitability of any information or product for use contemplated by any user, and the manner of that use, is the sole responsibility of the user. We recommend that anyone intending to rely on any recommendation of materials or procedures mentioned in this publication should satisfy himself as to such suitability, and that he can meet all applicable safety and health standards. Preface The motivation for writing this book was that there was no single source of information which covers all aspects of Physical Vapor Deposition (PVD) processing in a comprehensive manner. The properties of thin films deposited by PVD processes depend on a number of factors (see Sec. 1.2.2), and each must be considered when developing a reproducible process and obtaining a high product throughput and yield from the production line. This book covers all aspects of PVD process technology from characterizing and preparing the substrate material, through the deposition process and film characterization, to post deposition processing. The emphasis of the book is on the aspects of the process flow that are critical to reproducible deposition of films that have the desired properties. The book covers both neglected subjects, such as film adhesion, substrate surface characterization, and the external processing environment, and widely discussed subjects, such as vacuum technology, film properties and the fundamentals of individual deposition processes. In this book, the author relates these subjects to the practical issues that arise in PVD processing, such as contamination control and substrate property effects on film growth, which are often not discussed or even mentioned in the literature. By bringing these subjects together in one book, the author has made it possible for the reader to better understand the interrelationships between various aspects of the processing and the resulting film properties. The author draws upon his long experience in developing PVD processes, teaching short courses on PVD processing, to not only present the basics but vi Preface vii also to provide useful hints for avoiding problems and solving problems when they arise. Some examples of actual problems and solutions (“war stories”) are provided as foot notes throughout the text. The organization of the text allows a reader who is already knowledgeable in the subject to scan through a section and find subjects that are of particular interest. Extensive references allow the reader to pursue subjects in greater detail if so desired. An important aspect of the book is the useful reference material presented in the Appendices. A glossary of over 2500 terms and acronyms will be especially useful to those individuals that are just entering the field and those who are not fully conversant with the English language. Many of the terms are colloquialisms that are used in the field of Surface Engineering. The author realizes that covering this subject is a formidable task, particularly for one person, and that this effort is incomplete at best. He would like to elicit comments, corrections, and additions, which may be incorporated in a later edition of the book. In particular, he would like to elicit “war stories” of actual problems and solutions. Credit will be given for those which are used. Please contact the author at (ph.) 505-856-6810, (fax) 505- 856-6716, or e-mail [email protected]. Albuquerque, New Mexico Donald M. Mattox August, 1997 Table of Contents ix Table of Contents 1 Introduction ..........................................................................29 1.1 SURFACE ENGINEERING..........................................................29 1.1.1 Physical Vapor Deposition (PVD) Processes..................31 Vacuum Deposition....................................................32 Sputter Deposition......................................................33 Arc Vapor Deposition.................................................34 Ion Plating...................................................................34 1.1.2 Non-PVD Thin Film Atomistic Deposition Processes....35 Chemical Vapor Deposition (CVD) and PECVD ......35 Electroplating, Electroless Plating and Displacement Plating......................................................................36 Chemical Reduction ...................................................37 1.1.3 Applications of Thin Films..............................................38 1.2 THIN FILM PROCESSING...........................................................39 1.2.1 Stages of Fabrication.......................................................39 1.2.2 Factors that Affect Film Properties.................................40 1.2.3 Scale-Up and Manufacturabilty ......................................43 1.3 PROCESS DOCUMENTATION...................................................44 1.3.1 Process Specifications.....................................................44 Laboratory/Engineering Notebook.............................46 1.3.2 Manufacturing Process Instructions (MPIs)....................46 1.3.3 Travelers..........................................................................47 1.3.4 Equipment and Calibration Logs.....................................48 1.3.5 Commercial/Military Standards and Specifications........48 1.4 SAFETY AND ENVIRONMENTAL CONCERNS......................50 ix x Handbook of Physical Vapor Deposition (PVD) Processing 1.5 UNITS.............................................................................................50 1.5.1 Temperature Scales .........................................................51 1.5.2 Energy Units....................................................................51 1.5.3 Prefixes............................................................................51 1.5.4 Greek Alphabet ...............................................................52 1.6 SUMMARY....................................................................................52 FURTHER READING................................................................................53 REFERENCES............................................................................................54 2 Substrate (“Real”) Surfaces and Surface Modification....56 2.1 INTRODUCTION..........................................................................56 2.2 MATERIALS AND FABRICATION............................................57 2.2.1 Metals..............................................................................57 2.2.2 Ceramics and Glasses......................................................59 2.2.3 Polymers..........................................................................61 2.3 ATOMIC STRUCTURE AND ATOM-PARTICLE INTERACTIONS........................................................................63 2.3.1 Atomic Structure and Nomenclature...............................63 2.3.2 Excitation and Atomic Transitions..................................64 2.3.3 Chemical Bonding...........................................................66 2.3.4 Probing and Detected Species.........................................67 2.4 CHARACTERIZATION OF SURFACES AND NEAR-SURFACE REGIONS.....................................................69 2.4.1 Elemental (Chemical) Compositional Analysis..............71 Auger Electron Spectroscopy (AES)..........................72 Ion Scattering Spectroscopy (ISS and LEISS)...........73 Secondary Ion Mass Spectrometry (SIMS)................75 2.4.2 Phase Composition and Microstructure ..........................75 X-ray Diffraction........................................................75 Electron Diffraction (RHEED, TEM) ........................76 2.4.3 Molecular Composition and Chemical Bonding.............76 Infrared (IR) Spectroscopy.........................................76 X-ray Photoelectron Spectroscopy (XPS) or Electron Spectroscopy for Chemical Analysis (ESCA)............79 2.4.4 Surface Morphology........................................................80 Contacting Surface Profilometry................................82 Scanning Tunneling Microscopy (STM) and Atomic Force Microscopy (AFM).......................................83 Interferometry.............................................................84 Scanning Near-Field Optical Microscopy (SNOM) and Photon Tunneling Microscopy (PTM)....................84 Scatterometry..............................................................85 Scanning Electron Microscope (SEM).......................85 Replication TEM ........................................................85 Adsorption—Gases and Liquids.................................86 Table of Contents xi 2.4.5 Mechanical and Thermal Properties of Surfaces.............87 2.4.6 Surface Energy................................................................88 2.4.7 Acidic and Basic Properties of Surfaces.........................90 2.5 BULK PROPERTIES.....................................................................91 2.5.1 Outgassing.......................................................................91 2.5.2 Outdiffusion....................................................................92 2.6 MODIFICATION OF SUBSTRATE SURFACES........................92 2.6.1 Surface Morphology........................................................92 Smoothing the Surface................................................92 Roughening Surfaces..................................................95 Vicinal (Stepped) Surfaces.......................................100 2.6.2 Surface Hardness...........................................................100 Hardening by Diffusion Processes ...........................100 Hardening by Mechanical Working.........................102 Hardening by Ion Implantation ................................102 2.6.3 Strengthening of Surfaces .............................................103 Thermal Stressing.....................................................103 Ion Implantation .......................................................104 Chemical Strengthening ...........................................104 2.6.4 Surface Composition.....................................................104 Inorganic Basecoats..................................................105 Oxidation..................................................................105 Surface Enrichment and Depletion...........................107 Phase Composition...................................................107 2.6.5 Surface “Activation”.....................................................108 Plasma Activation.....................................................108 Corona Activation.....................................................109 Flame Activation ......................................................110 Electronic Charge Sites and Dangling Bonds...........110 Surface Layer Removal............................................111 2.6.6 Surface “Sensitization”..................................................111 2.7 SUMMARY..................................................................................112 FURTHER READING..............................................................................112 REFERENCES..........................................................................................113 3 The Low-Pressure Gas and Vacuum Processing Environment .......................................................................127 3.1 INTRODUCTION........................................................................127 3.2 GASES AND VAPORS...............................................................128 3.2.1 Gas Pressure and Partial Pressure.................................129 Pressure Measurement..............................................131 Identification of Gaseous Species.............................135 xii Handbook of Physical Vapor Deposition (PVD) Processing 3.2.2 Molecular Motion..........................................................136 Molecular Velocity...................................................136 Mean Free Path.........................................................136 Collision Frequency..................................................136 Energy Transfer from Collision and “Thermalization”............................................137 3.2.3 Gas Flow........................................................................138 3.2.4 Ideal Gas Law................................................................140 3.2.5 Vapor Pressure and Condensation.................................141 3.3 GAS-SURFACE INTERACTIONS.............................................143 3.3.1 Residence Time .............................................................143 3.3.2 Chemical Interactions....................................................144 3.4 VACUUM ENVIRONMENT......................................................146 3.4.1 Origin of Gases and Vapors..........................................147 Residual Gases and Vapors......................................147 Desorption ................................................................148 Outgassing................................................................149 Outdiffusion..............................................................151 Permeation Through Materials.................................151 Vaporization of Materials.........................................152 Real and Virtual Leaks.............................................153 “Brought-in” Contamination....................................154 3.5 VACUUM PROCESSING SYSTEMS ........................................155 3.5.1 System Design Considerations and “Trade-Offs”.........157 3.5.2 Processing Chamber Configurations.............................157 Direct-Load System..................................................159 Load-Lock System....................................................159 In-Line System .........................................................161 Cluster Tool System .................................................162 Web Coater (Roll Coater).........................................162 Air-To-Air Strip Coater............................................163 3.5.3 Conductance..................................................................163 3.5.4 Pumping Speed and Mass Throughput .........................165 3.5.5 Fixturing and Tooling....................................................166 Substrate Handling ...................................................171 3.5.6 Feedthroughs and Accessories......................................171 3.5.7 Liners and Shields.........................................................171 3.5.8 Gas Manifolding............................................................172 Mass Flow Meters and Controllers...........................173 3.5.9 Fail-Safe Designs ..........................................................175 “What-If” Game .......................................................178 3.6 VACUUM PUMPING..................................................................179 3.6.1 Mechanical Pumps ........................................................179 Oil-Sealed Mechanical Pumps..................................180 Dry Pumps................................................................181 Diaphragm Pumps ....................................................182

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