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PART Ⅰ:PREPARATION AND MATERIALS3

LANGMUIR-BLODGETT FILMS3

1.1 Introduction3

1.2 L-B Films of Long-Chain Compounds6

Fatty Acids6

Amines8

Other Long-Chain Compounds8

1.3 Cyclic Compounds and Chromophores9

1.4 Polymers and Proteins10

1.5 Polymerization In Situ11

1.6 Alternation Films(Superlattices)12

1.7 Potential Applications13

SELF-ASSEMBLED MONOLAYERS21

2.1 Introduction21

2.2 Monolayers of Fatty Acids22

2.3 Monolayers of Organosilicon Derivatives22

2.4 Monolayers of Alkanethiolates on Metal and Semiconductor Surfaces24

2.5 Self-Assembled Monolayers Containing Aromatic Groups27

2.6 Conclusions28

PART Ⅱ:ANALYSIS OF FILM AND SURFACE PROPERTIES35

SPECTROSCOPIC ELLIPSOMETRY35

3.1 Introduction and Overview35

3.2 Theory of Ellipsometry36

3.3 Instrumentation38

3.4 Determination of Optical Properties40

Analysis of Single Ellipsometric Spectra:Direct Inversion Methods40

Analysis of Single Ellipsometric Spectra:Least-Squares Regression Analysis Method42

Analysis of Multiple Ellipsometric Spectra44

3.5 Determination of Thin Film Structure46

Thickness Determination for Monolayers46

Microstructural Evolution in Thick Film Growth50

3.6 Future Prospects53

INFRARED SPECTROSCOPY IN THE CHARACTERIZATION OF ORGANIC THIN FILMS57

4.1 Introduction57

Specific Needs for Characterizing Organic Thin Films58

General Principles and Capabilities of Infrared Spectroscopy for Surface and Thin Film Analysis59

4.2 Quantitative Aspects64

Spectroscopic Intensities64

Electromagnetic Fields in Thin Film Structures65

4.3 The Infrared Spectroscopic Experiment71

General Instrumentation71

Experimental Modes71

Additional Aspects80

4.4 Examples of Applications81

Self-Assembled Monolayers on Gold by External Reflection81

Octadecylsiloxane Monolayers on SiO2 by Transmission82

Langmuir-Blodgett Films on Nonmetallic Substrates by External Reflection83

RAMAN SPECTROSCOPIC CHARACTERIZATION OF ORGANIC THIN FILMS87

5.1 Introduction87

5.2 Fundamentals of Raman Spectroscopy88

5.3 Instrumental Considerations90

5.4 Raman Spectroscopic Approaches for the Characterization of Organic Thin Films92

Integrated Optical Waveguide Raman Spectroscopy(IOWRS)92

Total Internal Reflection Raman Spectroscopy94

Surface Enhanced Raman Scattering95

Normal Raman Spectroscopy96

Resonance Raman Spectroscopy97

Plasmon Surface Polariton Enhanced Raman Spectroscopy97

Fourier Transform Raman Spectroscopy98

Waveguide Surface Coherent Anti-Stokes Raman Spectroscopy(WSCARS)99

5.5 Selected Examples of Thin Film Analyses99

Raman Spectral Characterization of Langmuir-Blodgett Layers of Arachidate and Stearate Salts99

Raman Spectral Characterization of Self-Assembled Monolayers of Alkanethiols on Metals104

Surface Enhanced Resonance Raman Spectral Characterization of Langmuir-Blodgett Layers of Phthalocyanines107

5.6 Prospects for Raman Spectroscopic Characterization of Thin Films110

SURFACE POTENTIAL113

6.1 Introduction113

6.2 Origins of the Contact Potential Difference and Surface Potential114

The Work Function114

Contact Potential Difference and Surface Potential115

Surface Potential Changes Induced by Adsorbates116

6.3 Measurement of Surface Potential117

Capacitance Techniques117

Ionizing-Probe Technique119

6.4 Surface Potentials of Organic Thin Films121

Air-Water Interface:Surface Potential of Langmuir Monolayers121

Air-Solid Interface:Surface Potential of L-B and Related Films124

6.5 Conclusions129

X-RAY DIFFRACTION133

7.1 Introduction133

7.2 Basic Principles134

7.3 Structure Normal to Film Plane135

7.4 Structure Within the Film Plane139

7.5 Summary145

HIGH RESOLUTION EELS STUDIES OF ORGANIC THIN FILMS AND SURFACES147

8.1 Introduction147

8.2 The Scattering Mechanism148

Dipole Scattering149

Impact Scattering149

Resonance Scattering150

8.3 The Spectrometer151

8.4 EELS Versus Other Techniques:Advantages and Disadvantages153

8.5 Examples153

Resolution Enhancement153

Linearity155

Depth Sensitivity157

Molecular Orientation159

Local Versus Long-Range Interactions160

Surface Segregation161

8.6 Conclusions162

WETTING165

9.1 Introduction165

9.2 Contact Angles166

9.3 Techniques for Contact Angle Measurements171

Axisymmetric Drop Shape Analysis-Profile(ADSA-P)171

Axisymmetric Drop Shape Analysis-Contact Diameter(ADSA-CD)173

Capillary Rise Technique175

9.4 Phase Rule for Moderately Curved Surface Systems175

9.5 Equation of State for Interfacial Tensions of Solid—Liquid Systems179

9.6 Drop Size Dependence of Contact Angle and Line Tension182

9.7 Contact Angles in the Presence of a Thin Liquid Film184

9.8 Effects of Elastic Liquid-Vapor Interfaces on Wetting187

SECONDARY ION MASS SPECTROMETRY AS APPLIED TO THIN ORGANIC AND POLYMERIC FILMS193

10.1 Introduction and Background193

Overview of the SIMS Method and Experiment193

Ion Formation Mechanisms196

Comparisons to Other Surface Analysis Techniques196

The Motivation for Thin Organic Films as Model Systems196

10.2 Qualitative Information:Mechanisms of Secondary Molecular Ion Formation197

Structure-Ion Formation Relationships197

Applications to Self-Assembled Film Chemistry199

10.3 The Study of Sampling Depth in the SIMS Experiment200

10.4 Quantitation in SIMS203

Development of Quantitation Methods203

Application of Quantitative Schemes to Thin Film Chemistry205

10.5 Imaging Applications208

10.6 Summary and Prospects208

X-RAY PHOTOELECTRON SPECTROSCOPY OF ORGANIC THIN FILMS213

11.1 Introduction213

11.2 Experimental Considerations214

11.3 Binding Energy Shifts215

11.4 XPS of Molten Films215

11.5 Angular Dependent XPS216

11.6 ETOA XPS of Self-Assembled Monolayers218

11.7 Conclusions223

MOLECULAR ORIENTATION IN THIN FILMS AS PROBED BY OPTICAL SECOND HARMONIC GENERATION227

12.1 Introduction227

12.2 Experimental Considerations228

12.3 Molecular Nonlinear Polarizability Calculation232

12.4 Measurements of the Surface Nonlinear Susceptibility236

12.5 Molecular Orientation Calculation239

Case 1:βZZZ only240

Case 2:βZXX only241

Case 3:βXXZ(=βXZX)only241

Case 4:βZZZ and βZXX241

Case 5:βZXX and βXXZ(=βXZX)242

12.6 Absolute Molecular Orientation Measurements243

12.7 Summary and Conclusions244

APPENDIX:TECHNIQUE SUMMARIES251

1 Auger Electron Spectroscopy(AES)251

2 Dynamic Secondary Ion Mass Spectrometry(Dynamic SIMS)252

3 Fourier Transform Infrared Spectroscopy(FTIR)253

4 High-Resolution Electron Energy Loss Spectroscopy(HREELS)254

5 Low-Energy Electron Diffraction(LEED)255

6 Raman Spectroscopy256

7 Scanning Electron Microscopy(SEM)257

8 Scanning Tunneling Microscopy(STM)and Scanning Force Microscopy(SFM)258

9 Static Secondary Ion Mass Spectrometry(Static SIMS)259

10 Transmission Electron Microscopy(TEM)260

11 Variable-Angle Spectroscopic Ellipsometry(VASE)261

12 X-Ray Diffraction XRD)262

13 X-Ray Fluorescence(XRF)263

14 X-Ray Photoelectron Spectroscopy(XPS)264

Index265