Scanning Probe Microscopy¿in Industrial Applications Nanomechanical Characterization

Describes new state-of-the-science tools and their contribution to industrial R&D

With contributions from leading international experts in the field, this book explains how scanning probe microscopy is used in industry, resulting in improved product formulation, enhanced processes, better quality control and assurance, and new business opportunities. Readers will learn about the use of scanning probe microscopy to support R&D efforts in the semiconductor, chemical, personal care product, biomaterial, pharmaceutical, and food science industries, among others.

Scanning Probe Microscopy in Industrial Applications emphasizes nanomechanical characterization using scanning probe microscopy. The first half of the book is dedicated to a general overview of nanomechanical characterization methods, offering a complete practical tutorial for readers who are new to the topic. Several chapters include worked examples of useful calculations such as using Hertz mechanics with and without adhesion to model a contact, step-by-step instructions for simulations to guide cantilever selection for an experiment, and data analysis procedures for dynamic contact experiments.

The second half of the book describes applications of nanomechanical characterization in industry, including:

• New formulation development for pharmaceuticals
• Measurement of critical dimensions and thin dielectric films in the semiconductor industry
• Effect of humidity and temperature on biomaterials
• Characterization of polymer blends to guide product formulation in the chemicals sector
• Unraveling links between food structure and function in the food industry

Contributions are based on the authors' thorough review of the current literature as well as their own firsthand experience applying scanning probe microscopy to solve industrial R&D problems.

By explaining the fundamentals before advancing to applications, Scanning Probe Microscopy in Industrial Applications offers a complete treatise that is accessible to both novices and professionals. All readers will discover how to apply scanning probe microscopy to build and enhance their R&D efforts.

Contributors List xiii

Preface xv

Acknowledgments xix

1. Overview of Atomic Force Microscopy 1
Dalia G. Yablon

1.1 A Word on Nomenclature 2

1.2 Atomic Force Microscopy—The Appeal to Industrial R&D 2

1.3 Mechanical Properties 5

1.4 Overview of AFM Operation 6

1.5 Nanomechanical Methods Surveyed in Book 11

1.6 Industries Represented 13

Acknowledgments 14

References 14

2. Understanding the Tip–Sample Contact: An Overview of Contact Mechanics from the Macro- to the Nanoscale 15
Tevis D. B. Jacobs, C. Mathew Mate, Kevin T. Turner, and Robert W. Carpick

2.1 Hertz Equations for Elastic Contact 15

2.2 Adhesive Contacts 22

2.3 Further Extensions of Continuum Contact Mechanics Models 29

2.4 Thin Films 34

2.5 Tangential Forces 37

2.6 Application of Continuum Mechanics to Nanoscale Contacts 42

Acknowledgments 44

Appendix 2A Surface Energy and Work of Adhesion 44

References 45

3. Understanding Surface Forces Using Static and Dynamic Approach–Retraction Curves 49
Sudharsan Balasubramaniam, Daniel Kiracofe, and Arvind Raman

3.1 Tip–Sample Interaction Forces 53

3.2 Static F–Z Curves 58

3.3 Dynamic Amplitude/Phase–Distance Curves 69

3.4 Brief Guide to VEDA Simulations 78

3.5 Conclusions 90

Glossary 91

References 93

4. Phase Imaging 95
Dalia G. Yablon and Greg Haugstad

4.1 Introduction 95

4.2 Bistability: Attractive and Repulsive Mode 97

4.3 Complications in Phase Quantification 107

References 113

5. Dynamic Contact AFM Methods for Nanomechanical Properties 115
Donna C. Hurley and Jason P. Killgore

5.1 Introduction 115

5.2 Force Modulation Microscopy (FMM) 121

5.3 Contact Resonance (CR) Techniques 125

5.4 Comparison of FMM and CR-FM 136

5.5 Other Dynamic Contact Approaches 138

5.6 Summary and Conclusions 140

Acknowledgments 141

Appendix 5A Data Analysis Procedure for Contact Resonance Spectroscopy Measurements 141

References 145

6. Guide to Best Practices for AFM Users 150
Greg Haugstad

6.1 Force–Distance Measurements—Instrumental Sources of Nonideality 151

6.2 Force–Distance Measurements—Physical Sources of Nonideality 157

References 161

7. Nanoindentation Measurements of Mechanical Properties of Very Thin Films and Nanostructured Materials at High Spatial Resolution 162
Steve J. Bull

7.1 Introduction 162

7.2 Bulk Materials 163

7.3 Coatings 176

7.4 Conclusions 188

Acknowledgments 188

References 188

8. Scanning Probe Microscopy for Critical Measurements in the Semiconductor Industry 190
Johann Foucher

8.1 Introduction 190

8.2 Critical Dimension in the Semiconductor Industry 191

8.3 CD Metrology Techniques for Production 192

8.4 Obtaining Accurate CD in the Semiconductor Industry 194

8.5 Hybrid Metrology as a Final Solution to Overcome CD-AFM, CD-SEM, and Scatterometry Intrinsic Limitations 203

8.6 Conclusion 208

References 208

9. Atomic Force Microscopy of Polymers 210
Andy H. Tsou and Dalia G. Yablon

9.1 Introduction 210

9.2 Tapping Phase AFM 213

9.3 Nanoindentation 217

9.4 Force Modulation 218

9.5 Pulsed Force Imaging 219

9.6 Force–Volume AFM 220

9.7 HarmoniX and Peak Force QNM Imaging 222

9.8 Summary 227

References 229

10. Unraveling Links between Food Structure and Function with Probe Microscopy 232
A. Patrick Gunning and Victor J. Morris

10.1 Introduction 232

10.2 Gels and Thickeners: Molecular Networks 236

10.3 Emulsions and Foams: Protein–Surfactant Competition 238

10.4 Interfacial Structure and Digestion: Designer Interfaces 241

10.5 Force Spectroscopy: Model Emulsions 244

10.6 Force Spectroscopy: Origins of Bioactivity 247

10.7 Conclusions 248

References 249

11. Microcantilever Sensors for Petrochemical Applications 251
Alan M. Schilowitz

11.1 Introduction 251

11.2 Background 252

11.3 Applications 257

11.4 Conclusion 266

References 267

12. Applications of Scanning Probe Methods in Cosmetic Science 270
Gustavo S. Luengo and Anthony Galliano

12.1 Introduction 270

12.2 Substrates of Cosmetics 271

12.3 Mechanical Properties and Modifications by Cosmetic Products 274

12.4 Scanning Probe Technologies Adapted to Cosmetic Science 275

12.5 Conclusions 285

References 285

13. Applications of Scanning Probe Microscopy and Nanomechanical Analysis in Pharmaceutical Development 287
Matthew S. Lamm

13.1 Introduction 287

13.2 Applications of SPM Imaging 288

13.3 SPM as a Screening Tool 291

13.4 Applications of Nanoindentation 293

13.5 Conclusion 299

Acknowledgments 299

References 300

14. Comparative Nanomechanical Study of Multiharmonic Force Microscopy and Nanoindentation on Low Dielectric Constant Materials 302
Katharine Walz, Robin King, Willi Volksen, Geraud Dubois, Jane Frommer, and Kumar Virwani

14.1 Introduction 302

14.2 Experimental 308

14.3 Results and Discussions 311

14.4 Conclusions 319

Acknowledgments 320

References 320

15. Nanomechanical Characterization of Biomaterial Surfaces: Polymer Coatings That Elute Drugs 323
Klaus Wormuth and Greg Haugstad

15.1 Introduction 323

15.2 Materials and Methods 325

15.3 Dexamethasone in PBMA or PBMA–PLMA Polymer Blends 327

15.4 Simvastatin in PEO–PBT Copolymers 337

15.5 Concluding Comments 340

Acknowledgments 341

References 341

Index 342

DALIA G. YABLON, PhD, developed and led a state-of-the-art scanning probe microscopy facility for more than ten years in Corporate Strategic Research, the flagship R&D center of ExxonMobil Corporation. Under her direction, scanning probe microscopy was used to characterize, conduct failure analysis, and probe structure-property relationships across all sectors of the vast petroleum business including areas of polymers, tribology, corrosion, geochemistry, and metallurgy. She currently leads SurfaceChar, a characterization consulting company.