and LUMINOUS CHEMICAL VAPOR DEPOSITION INTERFACE ENGINEERING HirotsuguYasuda University of Missouri-Columbia Columbia, Missouri, U.S.A.

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1 LUMINOUS CHEMICAL VAPOR DEPOSITION and INTERFACE ENGINEERING HirotsuguYasuda University of Missouri-Columbia Columbia, Missouri, U.S.A. MARCEL MARCEL DEKKER. NEW YORK DEKKER

2 Contents Preface iii Part I. Fundamentals of LCVD Chapter 1. Introduction 1 References 6 Chapter 2. Domain of Luminous Chemical Vapor Deposition 7 1. Terminology 7 2. Parylene Polymerization and Plasma Polymerization 8 3. Plasma-Induced Polymerization Plasma Surface Modiflcation of Polymers 11 References 12 Chapter 3. Luminous Gas Phase Luminous Columns in DC Discharge of Argon Electron Temperature and Electron Density Plasma and Luminous Gas Glow Discharge of Argon and of Acetylene Negative Glow in DC Discharge of Argon Cathode Glow in Glow Discharge of Trimethylsilane Dissociation of Molecule vs. Ionization Onion Layer Structure of Luminous Gas Phase Mode of Discharge and Onion Layer Structure 31 References 32 Chapter 4. Creation of Chemically Reactive Species in Luminous Chemical Vapor Deposition Polymerizable Species vs. Photon-Emitting Species LCVD on Electrode and in Gas Phase 36

3 vi Contents 3. Change of Gas Phase Composition with Discharge Time Change of Dissociation Glow and lonization Glow with Reaction Time Mixture of Polymerizable and Nonpolymerizable Gases Influence of Frequency of Power Source Polymerizable Species Created in DC Cathode Glow Polymerizable Species Created in Jet Stream of Luminous Gas Role of Free Radicals in Luminous Chemical Vapor Deposition 54 References 55 Chapter 5. Growth and Deposition Mechanisms Growth Mechanisms of Polymer Formation in Luminous Gas Polymerization in Vacuum Initiator and Polymerizable Species Growth Mechanisms of LCVD Deposition Mechanism in LCVD 71 References 81 Chapter 6. Dangling Bonds Free Radicals and Dangling Bonds Free Radicals in Plasma Polymer and Free Radicals in Substrate Dangling Bonds in Plasma Polymer Decay of the TMS Signal Ex Situ Estimation of Dangling Bonds and Polymer Free Radicals 111 References 112 Chapter 7. Chemical Structures of Organic Compounds for Luminous Chemical Vapor Deposition Hydrocarbons and Their Derivatives Perfluorocarbons Incorporation of Nonpolymerizable Gases in Plasma Polymers Derivatives of Silane and Siloxane 145 References 149 Chapter 8. Deposition Kinetics Mass Balance for Deposition in a Flow System Deposition in Luminous Gas Phase (Deposition G) Deposition on Electrode Surface (Deposition E) Partition Between Deposition E and Deposition G Properties of Plasma Polymers and Deposition Kinetics Deposition Kinetics in Low-Pressure Cascade Are Torch Powder Formation in Gas Phase 166 References 177 Chapter 9. Ablation by Luminous Gas (Low Pressure Plasma) Physical Sputtering and Chemical Etching Ablation of Polymers Simultaneous Sputter Coating and LCVD 187

4 Contents vii 4. Ablation-Influenced LCVD 192 References 195 Chapter 10. Competitive Ablation and Polymerization Chemical Etching and Material Formation Classification of Gases for Glow Discharge Plasma Sensitivity of Elements CAP Principle Effect of Consecutive Plasma Polymerizations Multistep Glow Discharge Treatment of Polymer Surface 216 References 219 Chapter 11. Internal Stress in Material Formed by Luminous Chemical Vapor Deposition Cause of Internal Stress in Plasma Polymer Curling of Bilayer Internal Stress in Glow Discharge Polymers Internal Stress in Plasma Polymers Prepared by LPCAT Internal Stress as a Function of Normalized Energy Input Parameter Correlation Between Internal Stress and Refractive Index 233 References 237 Part II. Operation of LCVD and LCVT Chapter 12. Modes of Operation and Scale-up Principle Modes of Overall Processing Pressure of a Steady-State Flow System (Without Pressure Control) System Pressure Under a Glow Discharge (Without Pressure Control) Factors That Determine Pressure Under a Glow Discharge in Flow Monomer Flow Rate Meaning of Flow Rate in an LCVD System Adsorption of Monomer on Substrate and Reactor Wall Surfaces Continuous LCVD Scale-up Principle 259 References 260 Chapter 13. Direct Current and Alternating Current Discharge Cathodic Polymerization vs. Plasma Polymerization in Negative Glow Role of Anode in DC Cathodic Polymerization TMS Deposition on Multiple Cathodes Without Anode Assembly DC LCVD in a Closed Reactor System 272 References 277

5 VIII Contents Chapter 14. Magnetron Discharge for Luminous Chemical Vapor Deposition Applicability of Magnetrons in LCVD Profile of Magnetic Field Effect of Magnetic Field on the Breakdown Voltage Effect of Magnetic Field on Voltage-Current Diagram Effect of Magnetic Field on the Sputtering of Electrode Materials Effect of Magnetic Field on the Deposition Rate of Plasma Polymer Significance of Magnetron Discharge in LCVD 305 References 306 Chapter 15. Anode Magnetron Discharge Cathode and Anode Magnetrons Electron Temperature and Electron Density Sputter Cleaning of Cathode Surface Anode Magnetron for Cathodic Polymerization 326 References 333 Chapter 16. Low-Pressure Cascade Are Torch Cascade Are Cascade Are Generator and Low-Pressure Cascade Are Torch Reactor Luminous Gas in Cascade Are Torch Deposition in Cascade Are Torch Characteristic Features of LPCAT Processing 357 References 361 Chapter 17. Anode Magnetron Torch Anode Magnetron Torch Structure of Anode Magnetron Torch Distribution of Anode Magnetic Field Strength A Comparison of AT and AMT Glow Discharge Effects of Physical Parameters in AMT Glow Discharge Infiuence of Various Parameters on the CDST in AMT Glow Discharge Infiuence of Operating Parameters on Sputter Cleaning 377 References 387 Chapter 18. Primary, Secondary and Pulsed Discharges Primary Plasma and Secondary Plasma "Secondary Plasma" Reactor Comparison of In-Glow and Off-Glow Treatments In-Glow and Off-Glow Treatment Without Ion and Electron Bombardment Surface Morphology of Treated PTFE Pulsed Glow Discharge 403 References 405

6 Contents ix Chapter 19. Reactor Size Tubulär Reactors with Different Diameters Deposition Characteristics Polymer Composition Change of Domain by Size of Reactor 417 References 422 Chapter 20. Flow Pattern Flow and Luminous Gas Volume Deposition of Fast-Polymerizing Monomer in Tubulär Reactor Deposition of Slowly-Polymerizing Monomer in Tubulär Reactor Effect of Flow Pattern Combined Effect of Flow Pattern and Energy Input Deposition on Electrode in a Bell Jar Type of Reactor Pinching of Luminous Gas Phase 443 References 447 Chapter 21. Composition-Graded Transition Phase Metal-Polymer Interface Transitional Buffering Film Deposition of Metal-Containing Polymer Films Activation of Nonconducting Surfaces for Electroless Plating Direct Electroplating onto Composition-Graded Composite Films Composition-Graded Transitional Buffering Film/Electrocopper Adhesion Durability Structure and Stability of Composition-Graded Transitional Buffering Phase 462 References 465 Chapter 22. Tumbler Reactor Needs for Tumbler Reactor Powder Surface Treatment or Coating Reactor with Basketlike Tumbler Electrodes for Basketlike Tumbler Reactor 470 Part III. Fundamentals of Surface and Interface Chapter 23. Surface Configuration Molecular Configuration vs. Surface Configuration Surface Characteristics of Gelatin Gel and of Agar-Agar Gel Oxygen Atoms Near the Top Surface of Ethylene-Vinyl Alcohol Copolymer O Atoms Detectable by XPS in Teflon PFA Film Localized Surface Configuration Change Under a Sessile Droplet of Water 482 References 486

7 X Chapter 24. Surface State Surface, Interface and Surface State Equilibration of Surface State Electrons on Contact Depth of Surface State and Influence of Bulk Phase Influence of the Surface State of Contacting Phase Durability and Breakdown of Surface State Significance of Surface Modification by LCVD 504 References 504 Chapter 25. Surface Dynamics Reference State for Surface Dynamics Incorporation of Tagging Atoms by Plasma Treatment Polymer Surfaces in Dry Condition Immersion of a Dry Polymer in Liquid Water Emersion or Drying of a Wet Surface Factors Involved in an Interface Molecular Interaction vs. Interfacial Interaction Interfacial Tension Between Polymer Surface and Liquid Water Surface Configuration Change When Polymer is Immersed in Water Surface Configuration Change in (Dry) Air Surface Dynamics of Hydrophilic Polymers Hydrophilic Polymers Immersed in Liquid Water Samples Exposed to High Humidity (Instead of Water Immersion) 521 References 523 Chapter 26. Contact Angle and Wettability Energy Balance at Liquid/Solid Interface Static Contact Angle Time Dependence of Sessile Droplet Contact Angle Advancing and Receding Sessile Droplet Contact Angles Dynamic Contact Angle Change of Meniscus Shape During Immersion and Emersion Processes Wilhelmy Dynamic Contact Angles and Wettability Contact Angle Hysteresis Correlation Between Wilhelmy (Dynamic) and Sessile Droplet (Static) Contact Angles Liquid Film on Surface on Wilhelmy Plate Wilhelmy Force Loops and Fluid Holding Time Effect of Wilhelmy Balance Parameters on Fluid Holding Time Meaning of Contact Angle 553 References 557 Chapter 27. Sessile Bubble Formation and Detachment Sessile Droplet Contact Angle vs. Sessile Bubble Contact Angle Force Balance in a Developing Sessile Bubble Bubble Formation from an Inclined Surface 567

8 Contents XI 4. Bubble Detachment from the Hydrophilic Surface Detachment of Drifted Bubbles from the Amphoteric Surface Criteria for Wettability 570 References 572 Part IV. Interface Engineering Chapter 28. System Approach Interface Engineering System Approach Interface Engineering for Corrosion Protection Corrosion Tests and Quantitative Evaluation of Results Pitting Corrosion Beneath Undamaged Coating Steps Involved in SAIE Nonelectrochemical Principle of Corrosion Protection Role of Adhesion in Electrochemical Impedance Spectroscopy Effects of Interfacial Damage on Corrosion Protection 597 References 603 Chapter 29. Creation of an Imperturbable Surface Origin of Surface Dynamical Instability Correlation Between Surface Dynamic Stability and Barrier Characteristics Segmental Mobility of the Substrate Polymer Stability of Top Surface of LCVD Film 618 References 621 Chapter 30. Creating Adhesion to Substrate Surface Modification of Surface Energy of Substrate Parylene C Film LPCAT (Treatment) and LCVD (Deposition) Increasing Adhesion of Inorganic Fillers and Fibers to PMMA Matrix 649 References 658 Chapter 31. Corrosion Protection of Aluminum AUoys SAIE Applied on Aluminum Alloys Pretreatment of Aluminum Alloys Surfaces Polarization Resistance Corrosion Test Results Chromated and Nonchromated Spray Paints on Plasma Polymer Surfaces 676 References 689 Chapter 32. Corrosion Protection of Ion Vapor-Deposited Aluminum Ion Vapor-Deposited Aluminum Cathodic LCVD With Anode Magnetron 694

9 XII Contents 3. Cathodic LCVD Without Anode Assembly Cathodic LCVD in Closed Reactor 707 References 718 Chapter 33. Corrosion Protection of Cold-Rolled Steel and Pure Iron Plasma Cleaning and In Situ Deposition of TMS Polymer on Cold-Rolled Steel Interfacial Chemistry Characterized by XPS and Sputtered Neutral Mass Spectroscopy Corrosion Test Results (Cold-Rolled Steel) Corrosion Protection of Pure Iron 732 References 741 Chapter 34. Membrane Preparation and Modifkation General Principles in Membrane Application of Luminous Chemical Vapor Deposition and Luminous Gas Treatment Luminous Gas Treatment LCVD on Nonporous Membrane LCVD on Nonporous/Porous Composite Membrane LCVD on Porous Membrane Macroporous Membrane for Gas/Liquid Reactions Membrane for Gas Bubbling Oxygenation of Blood Oxygenation of Water 771 References 776 Chapter 35. Application of Luminous Chemical Vapor Deposition in Biomaterials Signiflcance of Imperturbable Surface in Biocompatibility Principle of LCVD Coating for Biomaterials Applications of LCVD Coating on Silicone Contact Lens LCVD on Inner Surface of Polymer Tube LCVD for Blood Compatibility Biocompatibility of Imperturbable Surface 796 References 798 Chapter 36. Economical Advantages of Luminous Chemical Vapor Deposition Environmentally Benign (Green) Processing LCVD to Replace an Existing Hazardous Process LCVD as a New Manufacturing Process 800 Index 805

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