Scanning Probe Microscopy for 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 for 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 for 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. 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. 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