What Is in it for Us?
This book is divided into 12 Sections. Section 1 is on contact mechanics. It comprises two chapters. Chapter 1 deals with contact issues in brittle solids, while Chapter 2 concentrates more upon the mechanics of elastic and elastoplastic contact. The importance of elastoplastic contact is well rec-ognized in the case of brittle solids in general, and glass and ceramics in particular.
Section 2 begins with a journey toward the main topic of this book, that is the science and technology of nanoindentation, especially in the backdrop or purview of brittle solids. This section consists of 7 chapters. Chapter 3 gives a brief history of indentation. In Chapter 4, we have discussed the con-cepts of hardness and elastic modulus of a material. Next in Chapter 5, the basic ideas of nanoindentation have been put forward, with a special empha-sis on why it is necessary and where its applications lie altogether. But it is also important to know about the nanoindentation data analysis methods which have been discussed in Chapter 6. The various nanoindentation tech-niques are elaborated in Chapter 7. But one can recognize that it is not only important to know theoretically how the whole technique works; it is also important to understand how it actually translates to real life practice. For instance, what are the basic components of a nanoindentation machine and how do the different components work? It is also important to know about the ranges of different commercially available machines and their resolu-tions. These issues are briefly discussed in Chapter 8. Now, in this book we have discussed results obtained from the nanoindentation experiments con-ducted on a truly wide variety of brittle solids, e. g. , glass, ceramics, shock-loaded ceramics, different types of ceramic matrix composites, structural and functional ceramics, bioactive thick ceramic coatings as well as hard thin ceramic films. We have also included nanoindentation results from our recent research on natural biomaterials like tooth, bone and fish scale materi-als. These aspects are briefly dealt within Chapter 9.
Section 3 discusses the static contact behaviour of glass. It actually comprises three chapters; namely 10, 11, and 12. In Chapter 10, we have discussed the nanoindentation response if the contact is made too quickly in glass. Chapter 11 actually poses the question of whether if it is possible to enhance the nanohardness of glass. To the best of our knowledge this is the very first such attempt. Chapter 12 discusses the energy issues related to the nanoindentation of glass.
Section 4 deals with the dynamic contact behaviour of glass spanning Chapters 13 to 15. What happens if a specimen like glass is damaged in microscale dynamic contact events? This issue is discussed in Chapter 13 The next question that naturally appears is how it matters whether such a microscale contact is slow or fast. As elaborated in Chapter 14, it really mat-ters very much for dynamic damage evolution in glass. When the speed of the dynamic contact is varied, the consequences are portrayed in Chapter 14 We also wanted to ask how much is the damage inside a scratch groove in glass? How can we quantify the damage in terms of the nanomechanical properties evaluated at the local microstructural length scale? To the best of our knowledge, this is the very first such attempt. The results of our related experimental observations are summarized in Chapter 15.
Section 5 that spans Chapters16 to 18 concentrates mainly on the nanoscale static contact behaviour of atypical brittle ceramic like alumina. Chapter 16 not only describes the nanoindentation response of a coarse grain alu-mina, it also questions how relevant the grain size is as far as the intrinsic capability against contact-induced damage of a ceramic is concerned. The results depicted in Chapter 17raise two very important questions, e.g., if the energy dissipation rate from the loading train into the microstructure of a given ceramic really matters in its response against contact induced deformation and/or micro damage evolution and if it does, what will be the mechanisms of real relevance? To the best of our knowledge, this is the very first such attempt. In a kind of self-motivated manner, we have tried in Chapter 18 to devise a rational picture that addresses the issues raised in Chapter 17, but admittedly it opens up possibly more areas of concern for future research than were possible to be addressed in our humble effort made in this book.
Coming up to Section 5 we had somewhat learnt about the very inter-esting aspects of an interaction triangle that possibly exists between the microstructural units, e.g., grain size, the probe length scale and the rate of probing the load and the loading rate and the most important one, the spa-tial extent of interaction between these two factors on the one hand and the length scales of the naturally present pre-existing defects on the other hand. Now we wanted to pose another very important constraint on this scenario, i.e., what happens to its nanoindentation response, if the ceramic is already highly damaged; say, due to very high strain rate or high pressure impact from a projectile!
Thus, Section 6 that spans Chapters 19 to 22 tries to put forward a criti-cal look in this complicated scenario. To the best of our knowledge this is the very first such attempt. Through these chapters we have shown how the nanoscale contact deformation resistance of atypical coarse grain ceramic, e.g., 10 μm grain size alumina would be affected under such a scenario, whether the process will be load-and loading rate-dependent and how the interaction picture changes, as a function of the nanoindentation zone of influence and the extent of pre-shock history that the sample has gone through.
Section 7 spans Chapters 23 to 25 and asks what happens to the nanoin-d entation response in different kinds of ceramic matrix composites (CMCs), e. g. , C/C and C/C-SiC composites, HAp-based biological-composites, tape cast multilayered composites as well as particulate reinforced CMCs. Similarly, the nanoindentation behaviour of a wide variety of functional ceramics is covered in Chapters 26 to 31 of Section 8. Chapter 26 concen-t rates on the nanoindentation study on silicon that phase transforms under nanoindentation-induced pressure, while Chapter27 elaborates on the nanomechanical behaviour of ZTA where the tetragonal zirconia can phase transform under appropriate stress to the monoclinic phase. In Chapter 28 we have tried to address the nanoindentation responses of two actuator ceramics, e.g., (Pb0. 88Ba0.12) [(Zn1/3Nb2/3) 0.88Ti0.12)]O3; (PZN-BT) and (Pb0.8Ba0.2)[(Zn1/3Nb2/3)0.8Ti0.2)]O3, (PZN-BT-PT) ceramics and show how the results cor-relate with the hysteresis loop measurements in the polar region of these two actuator materials. Probably the very first results ever obtained on nanoin-dentation response of sol-gel derived, green compacted nano bismuth ferrite multiferroic ceramics are depicted in Chapter 29. Encouraged by the interest-ing results obtained for many functional materials as depicted above, it was decided to extend the efforts to the realm of materials for renewable energy or greener energy sources. It is in this perspective that the nanoindentation experiments were conducted on all three components—anode, electrolyte and cathode of a ceramic solid oxide fuel cell (SOFC) and also on the glass-ceramic sealants used to connect the different components of a SOFC stack in a condition that prevents leakage of any kind. To the best of our knowledge, these are the very first such efforts made in this field and the results are depicted in Chapters 30 and 31.
Section 8, spread across Chapters 32 to 37, actually puts forward the ques-tion of whether it is possible to utilize the nanoindentation technique to investigate the nanoscale contact deformation behaviour of ceramic coat-ings which are thick, porous, and highly micro-cracked and hence pos-sess truly heterogeneous microstructures. It has been shown that the same really can be achieved. Two coatings were investigated. One is a bioactive ceramic microplasma sprayed hydroxyapatite (MIPS-HAp). The other is a protective ceramic oxide coating formed on magnesium alloy by micro arc oxidation (MAO) coatings. Thus, Chapter 32 studies the nanoindentation on MIPS-HAp coatings, while the Weibull modulus of nanohardness and elas-tic modulus of the same has been discussed in Chapter 33. Keeping in mind the anisotropic microstructure of the MIPS-HAp coatings, the anisotropy in nanohardness has been examined in Chapter 34. To the best of our knowl-edge, in Chapter 36 the very first attempt to evaluate the microstructural scale relevant fracture toughness of the same MIPS-HAp coatings has been explored. Next in Chapter 36, the nanomechanical efficacy of the same was critically examined after immersion in simulated body fluid. Further, the nanoscale contact response of the important protective MAO coatings was examined in Chapter 37.
The cases of the soft Mg(OH)2 and hard TiN, Al2O3 and metal doped as well as undoped DLC thin ceramic thin films in terms of nanoindentation behavior as well as their nano tribological behavior have been briefly exposed in Chapters 39 to 41 which comprise Section 10.
So far we have discussed nanoindentation responses of glass, ceramics, different types of CMCs, functional ceramics, thick coatings as well as soft and hard ceramic thin films of tremendous biological, functional, structural, industrial, tribological as well as commercial importance. But one point has not been explored. That is the aspect of structure and nanomechanical property relationships of the natural biomaterials, e.g., human teeth, bone, fish scales etc. developed by mother nature over the ages in such a way that they possess nanoscale to macroscale functionally graded microstructure. Thus, Section 11 spanning Chapters 42 to 45 focuses on the nanoindentation behaviour of ceramic based natural hybrid nanocomposites.
In Chapters 46 to 51 in Section 12 the global, yet unresolved issues like the forward and reverse indentation size effect (ISE, RISE), pop-in, loading rate, substrate and residual stress effects, as well as the data reliability in brittle solids have been touched upon. A brief note on scope and direction for future research in this exciting, ever growing field of the science and tech-nology of nanoindentation in general, and brittle materials in particular has been sketched in Chapter 52. Finally, the bookends with a summary of the major findings that emerge out of the results presented in this compendium of our research results.

Prologue xxi

Preface xxv

Acknowledgments xxix

About the Authors xxxiii

Contributors xxxvii

Section 1 Contact Mechanics

1. Contact Issues in Brittle Solids 3

Payel Bandyopadhyay, Debkalpa Goswami, Nilormi Biswas, Arjun Dey, and Anoop Kumar Mukhopadhyay

1.1 Introduction 3

1.2 Elasticity and Plasticity 3

1.3 Stresses 5

1.4 Conclusions 10

References 10

2. Mechanics of Elastic and Elastoplastic Contacts 13

Manjima Bhattacharya, Arjun Dey, and Anoop Kumar Mukhopadhyay

2.1 Introduction 13

2.2 The Different Models 14

      2.2.1 The Elastic Indentation Model 14

      2.2.2 The Rigid Perfectly Plastic Model 16

      2.2.3 The Spherical-Cavity Expansion Model 16

      2.2.4 The Elastic and Perfectly Plastic Model 18

2.3 Conclusions 18

References 19

Section 2 Journey Towards Nanoindentation

3. Brief History of Indentation 23

Nilormi Biswas, Arjun Dey, and Anoop Kumar Mukhopadhyay

3.1 Introduction 23

3.2 How Did It All Happen? 23

3.3 And Then There Was a 23

3.4 Modern Developments: Nineteenth-Century Scenario 24

3.5 Comparison of Techniques 25

3.6 Major Developments beyond 1910 25

3.7 Beyond the Vickers and Knoop Indenters 26

3.8 Conclusions 27

References 27

4. Hardness and Elastic Modulus 31

Nilormi Biswas, Arjun Dey, and Anoop Kumar Mukhopadhyay

4.1 Introduction 31

4.2 Conceptual Issues 31

4.3 Beyond the Hertzian Era: Modern Contact Mechanics 33

4.4 The Experimental Issues 33

4.5 Elastic Modulus 33

4.6 Techniques to Determine Elastic Modulus 34

4.7 Conclusions 36

References 37

5. Nanoindentation: Why at All and Where? 39

Arjun Dey, Payel Bandyopadhyay, Nilormi Biswas, Manjima Bhattacharya, Riya Chakraborty, I. Neelakanta Reddy, and Anoop Kumar Mukhopadhyay

5.1 Introduction 39

      5.1.1 Depth-Control Mode 39

      5.1.2 Location-Control Mode 39

      5.1.3 Phase-Control Mode 41

5.2 In Situ Nanoindentation 42

5.3 Conclusions 43

References 43

6. Nanoindentation Data Analysis Methods 45

Manjima Bhattacharya, Arjun Dey, and Anoop Kumar Mukhopadhyay

6.1 Introduction 45

6.2 Modeling of the Nanoindentation Process 47

      6.2.1 Oliver-Pharr Model 47

      6.2.2 Doerner-Nix Model 49

      6.2.3 Field-Swain Model 49

      6.2.4 Mayo-Nix Model 49

6.3 Conclusions 51

References 52

7. Nanoindentation Techniques

Manjima Bhattacharya, Arjun Dey, and Anoop Kumar Mukhopadhyay

7.1 Introduction 53

      7.1.1 Hardness Analysis 53

7.2 Conclusions 55

References 55

8. Instrumental Details 57

Payel Bandyopadhyay, Arjun Dey, and Anoop Kumar Mukhopadhyay

8.1 Introduction 57

8.2 Nanoindenters: Tip Details and Tip Geometries 57

8.3 Conclusions 62

References 62

9. Materials and Measurement Issues 63

Arjun Dey, Riya Chakraborty, Payel Bandyopadhyay, Nilormi Biswas, Manjima Bhattacharya, Saikat Acharya, and Anoop Kumar Mukhopadhyay

9.1 Introduction 63

9.2 Materials 63

9.3 Nanoindentation Studies 68

      9.3.1 Fischerscope H100-XYp 69

      9.3.2 Triboindenter UBI 700 70

      9.3.3 Nano Indenter G200 71

      9.3.4 The Typical Protocol 71

9.4 The Scratch Tests 72

9.5 Microstructural Characterizations 72

9.6 Conclusions 73

References 73

Section 3 Static Contact Behavior of Glass

10. What If the Contact is Too Quick in Glass? 79

Riya Chakraborty, Arjun Dey, and Anoop Kumar Mukhopadhyay

10.1 Introduction 79

10.2 Effect of Loading Rate on Nanohardness 80

10.3 Damage Evolution Mechanism 81

10.4 Conclusions 85

References 85

11. Enhancement in Nanohardness of Glass: Possible? 87

Riya Chakraborty, Arjun Dey, and Anoop Kumar Mukhopadhyay

11.1 Introduction 87

11.2 Nanomechanical Behavior 87

11.3 Conclusions 90

References 90

12. Energy Issues in Nanoindentation 93

Riya Chakraborty, Arjun Dey, and Anoop Kumar Mukhopadhyay

12.1 Introduction 93

12.2 Energy Models 94

      12.2.1 Lawn-Howes Model 94

      12.2.2 Sakai Model 95

      12.2.3 Cheng-Cheng Model 95

      12.2.4 Malzbender-With Model 95

12.3 Energy Calculation 99

12.4 Conclusions 100

References 101

Section 4 Dynamic Contact Behavior of Glass

13. Dynamic Contact Damage in Glass 105

Payel Bandyopadhyay, Arjun Dey, and Anoop Kumar Mukhopadhyay

13.1 Introduction 105

13.2 Damage Due to Dynamic Contact 106

13.3 Conclusions 115

References 115

14. Does the Speed of Dynamic Contact Matter? 117

Payel Bandyopadhyay, Arjun Dey, and Anoop Kumar Mukhopadhyay

14.1 Introduction 117

14.2 Effect of Speed of Dynamic Contacts and Damage Evolution 118

14.3 Conclusions 122

References 123

15. Nanoindentation Inside the Scratch: What Happens? 125

Payel Bandyopadhyay, Arjun Dey, and Anoop Kumar Mukhopadhyay

15.1 Introduction 125

15.2 Nanoindentation Inside a Scratch Groove 125

15.3 The Model of Microcracked Solids 129

15.4 Conclusions 131

References 131

Section 5 Static Contact Behavior of Ceramics

16. Nanomechanical Properties of Ceramics 135

Riya Chakraborty, Manjima Bhattacharya, Arjun Dey, and Anoop Kumar Mukhopadhyay

16.1 Introduction 135

16.2 Nanoindentation Study 136

16.3 Indentation Size Effect (ISE) in Alumina 137

16.4 Conclusions 138

References 139

17. Does the Contact Rate Matter for Ceramics? 141

Manjima Bhattacharya, Riya Chakraborty, Arjun Dey, and Anoop Kumar Mukhopadhyay

17.1 Introduction 141

17.2 Effect of Loading Rate and "Multiple Micro Pop-in" and "Multiple Micro Pop-out" 141

17.3 Conclusions 145

References 146

18. Nanoscale Contact in Ceramics 147

Manjima Bhattacharya, Riya Chakraborty, Arjun Dey, and Anoop Kumar Mukhopadhyay

18.1 Introduction 147

18.2 Evolutions of Pop-ins 148

18.3 Conclusions 151

References 152

Section 6 Static Behavior of Shock-Deformed Ceramics

19. Shock Deformation of Ceramics 155

Riya Chakraborty, Arjun Dey, and Anoop Kumar Mukhopadhyay

19.1 Introduction 155

19.2 Nanoindentation Study 155

19.3 Occurrence of Pop-ins 157

19.4 Defects in Shock-Recovered Alumina 158

19.5 Conclusions 159

References 160

20. Nanohardness of Alumina 161

Riya Chakraborty, Arjun Dey, and Anoop Kumar Mukhopadhyay

20.1 Introduction 161

20.2 Indentation Size Effect of Shocked Alumina 161

20.3 Deformation of Shocked Alumina 164

20.4 Micro Pop-ins of Shocked Alumina 166

20.5 Conclusions 166

References 167

21. Interaction of Defects with Nanoindents in Shocked Ceramics 169

Riya Chakraborty, Arjun Dey, and Anoop Kumar Mukhopadhyay

21.1 Introduction 169

21.2 Indentation Size Effect of Alumina Shocked at High Shock Pressure 170

21.3 Deformation Due to Shock at High Pressure 172

21.4 Conclusions 174

References 175

22. Effect of Shock Pressure on ISE: A Comparative Study 177

Riya Chakraborty, Arjun Dey, and Anoop Kumar Mukhopadhyay

22.1 Introduction 177

22.2 Comparison of ISE in Alumina Shocked at 6.5 and 12 GPa 177

22.3 Shear Stress and Micro Pop-ins 179

22.4 Comparison of Deformations in Alumina Shocked at 6.5 and 12 GPa 181

22.5 Conclusions 183

References 183

Section 7 Nanoindentation Behavior of Ceramic-Based Composites

23. Nano/Micromechanical Properties of C/C and C/C-SiC Composites 187

Soumya Sarkar, Arjun Dey, Probal Kumar Das, Anil Kumar, and Anoop Kumar Mukhopadhyay

23.1 Introduction 187

23.2 Nanoindentation Behavior 187

23.3 Energy Calculation 190

23.4 Conclusions 191

References 192

24. Nanoindentation on Multilayered Ceramic Matrix Composites 193

Sadanand Sarapure, Arnab Sinha, Arjun Dey, and Anoop Kumar Mukhopadhyay

24.1 Introduction 193

24.2 Nanomechanical Behavior 194

      24.2.1 Nanoindentation on Lanthanum Phosphate Tape 194

      24.2.2 Nanoindentation on Alumina Tape 196

24.3 Conclusions 198

References 199

25. Nanoindentation of Hydroxyapatite-Based Biocomposites 201

Shekhar Nath, Arjun Dey, Prafulla K Mallik, Bikramjit Basu, and Anoop Kumar Mukhopadhyay

25.1 Introduction 201

25.2 HAp-Calcium Titanate Composite 202

25.3 HAp-Mullite Composite 203

25.4 Conclusions 205

References 206

Section 8 Nanoindentation Behavior of Functional Ceramics

26. Nanoindentation of Silicon 211

Arjun Dey and Anoop Kumar Mukhopadhyay

26.1 Introduction 211

26.2 Nanoindentation Response 212

26.3 Conclusions 215

References 216

27. Nanomechanical Behavior of ZTA 217

Sadanand Sarapure, Arnab Sinha, Arjun Dey, and Anoop Kumar Mukhopadhyay

27.1 Introduction 217

27.2 Nanomechanical Behavior 218

27.3 Conclusions 221

References 222

28. Nanoindentation Behavior of Actuator Ceramics 223

Sujit Kumar Bandyopadhyay, A K Himanshu, Pintu Sen, Tripurari Prasad Sinha, Riya Chakraborty, Arjun Dey, Payel Bandyopadhyay, and Anoop Kumar Mukhopadhyay

28.1 Introduction 223

28.2 Nanoindentation Behavior 224

28.3 Polarization Behavior 225

28.4 Conclusions 226

References 227

29. Nanoindentation of Magnetoelectric Multiferroic Material 229

Pintu Sen, Arjun Dey, Anoop Kumar Mukhopadhyay, Sujit Kumar Bandyopadhyay, and A K Himanshu

29.1 Introduction 229

29.2 Nanoindentation Response 229

29.3 Conclusions 232

References 232

30. Nanoindentation Behavior of Anode-Supported Solid Oxide Fuel Cell 235

Rajendra Nath Basu, Tapobrata Dey, Prakash C Ghosh, Manaswita Bose, Arjun Dey, and Anoop Kumar Mukhopadhyay

30.1 Introduction 235

30.2 Nanomechanical Behavior 236

30.3 Conclusions 240

References 240

31. Nanoindentation Behavior of High-Temperature Glass–Ceramic Sealants for Anode-Supported Solid Oxide Fuel Cell 243

Rajendra Nath Basu, Saswati Ghosh, A Das Sharma, P Kundu, Arjun Dey, and Anoop Kumar Mukhopadhyay

31.1 Introduction 243

31.2 Preparation of the Sealant Glass–Ceramic 244

31.3 Nanomechanical Properties 244

31.4 Conclusions 246

References 247

Section 9 Static Contact Behavior of Ceramic Coatings

32. Nanoindentation on HAp Coating 251

Arjun Dey, Payel Bandyopadhyay, Nil Ratan Bandyopadhyay, and Anoop Kumar Mukhopadhyay

32.1 Introduction 251

32.2 Influence of Load on Nanohardness and Young’s Modulus 251

32.3 Conclusions 254

References 254

33. Weibull Modulus of Ceramic Coating 255

Arjun Dey and Anoop Kumar Mukhopadhyay

33.1 Introduction 255

33.2 Data Reliability Issues in MIPS–HAp Coatings 255

33.3 Conclusions 257

References 258

34. Anisotropy in Nanohardness of Ceramic Coating 261

Arjun Dey and Anoop Kumar Mukhopadhyay

34.1 Introduction 261

34.2 Nanohardness Behavior: Anisotropy 262

34.3 Conclusions 264

References 264

35. Fracture Toughness of Ceramic Coating Measured by Nanoindentation 267

Arjun Dey and Anoop Kumar Mukhopadhyay

35.1 Introduction 267

35.2 Fracture Toughness Behavior 267

35.3 Conclusions 270

References 271

36. Effect of SBF Environment on Nanomechanical and Tribological Properties of Bioceramic Coating 273

Arjun Dey and Anoop Kumar Mukhopadhyay

36.1 Introduction 273

36.2 Nano-/Micro-mechanical Behavior 273

36.3 Tribological Study 274

36.4 Conclusions 277

References 278

37. Nanomechanical Behavior of Ceramic Coatings Developed by Micro Arc Oxidation 279

Arjun Dey, R Uma Rani, Hari Krishna Thota, A Rajendra, Anand Kumar Sharma, Payel Bandyopadhyay, and Anoop Kumar Mukhopadhyay

37.1 Introduction 279

37.2 Nanoindentation Study and Reliability Issue 280

37.3 Conclusions 282

References 283

38. Section 10 Static Contact Behavior of Ceramic Thin Films Nanoindentation Behavior of Soft Ceramic Thin Films: Mg (OH)2 287

Pradip Sekhar Das, Arjun Dey, and Anoop Kumar Mukhopadhyay

38.1 Introduction 287

38.2 Nanoindentation Study 287

38.3 Energy Calculation 289

38.4 Conclusions 290

References 291

39. Nanoindentation Study on Hard Ceramic Thin Films: TiN 293

Arjun Dey and Anoop Kumar Mukhopadhyay

39.1 Introduction 293

39.2 Nanoindentation Study 294

39.3 Depth Dependent Nanomechanical Behavior 295

39.4 Conclusions 296

References 297

40. Nanoindentation Study on Sputtered Alumina Films for Spacecraft Application 299

I. Neelakanta Reddy, N. Sridhara, V. Sasidhara Rao, Anju M Pillai, Anand Kumar Sharma, V R Reddy, Anoop Kumar Mukhopadhyay, and Arjun Dey

40.1 Introduction 299

40.2 Optical Behavior 299

40.3 Nanomechanical Behavior 300

40.4 Conclusions 302

References 302

41. Nanomechanical Behavior of Metal-Doped DLC Thin Films 305

Arjun Dey, Rajib Paul, A K Pal, and Anoop Kumar Mukhopadhyay

41.1 Introduction 305

41.2 Nanoindentation Study 306

41.3 Nanotribological Study 308

41.4 Adhesion Mechanisms 310

41.5 Conclusions 311

References 311

Section 11 Nanoindentation Behavior on Ceramic-Based Natural Hybrid Nanocomposites

42. Orientational Effect in Nanohardness of Tooth Enamel 315

Nilormi Biswas, Arjun Dey, and Anoop Kumar Mukhopadhyay

42.1 Introduction 315

42.2 Nanomechanical Behavior and Energy Issues 316

42.3 Micro Pop-in Events 318

42.4 Conclusions 319

References 319

43. Slow or Fast Contact: Does it Matter for Enamel? 321

Nilormi Biswas, Arjun Dey, and Anoop Kumar Mukhopadhyay

43.1 Introduction 321

43.2 Loading Rate Effect 321

43.3 Evolution of Micro Pop-in Events 323

43.4 Loading Rate versus Micro/Nanostructure 324

43.5 Conclusions 325

References 326

44. Anisotropy of Modulus in Cortical Bone 327

Arjun Dey, Himel Chakraborty, and Anoop Kumar Mukhopadhyay

44.1 Introduction 327

44.2 Microstructure 328

44.3 Nanomechanical Behavior and Anisotropy 329

44.4 Conclusions 331

References 331

45. Nanoindentation of Fish Scale 333

Arjun Dey, Himel Chakraborty, and Anoop Kumar Mukhopadhyay

45.1 Introduction 333

45.2 Microstructure 334

45.3 Nanomechanical Behavior 335

45.4 Conclusions 337

References 337

Section 12 Some Unresolved Issues in Nanoindentation

46. Indentation Size Effect (ISE) and Reverse Indentation Size Effect (RISE) in Nanoindentation 341

Arjun Dey, Devashish Kaushik, Nilormi Biswas, Saikat Acharya, Riya Chakraborty, and Anoop Kumar Mukhopadhyay

46.1 Introduction 341

46.2 ISE in HAp Coating 342

      46.2.1 Nanoindentation at High Load 342

      46.2.2 Nanoindentation at Ultralow Load 343

46.3 ISE and RISE in AlN-SiC Composites 344

46.4 ISE in Dentin 345

46.5 ISE in SLS Glass 346

46.6 Conclusions 347

References 347

47. Pop-in Issues in Nanoindentation 349

Riya Chakraborty, Arjun Dey, Manjima Bhattacharya, Nilormi Biswas, Jyoti Kumar Sharma, Devashish Kaushik, Payel Bandyopadhyay, Saikat Acharya, and Anoop Kumar Mukhopadhyay

47.1 Introduction 349

47.2 What is Known about Pop-ins? 349

47.3 Pop-ins in Nanoindentation of Brittle Solids 350

      47.3.1 Pop-ins in SLS Glass and Alumina 350

      47.3.2 Why Pop-ins in SLS Glass? 353

      47.3.3 Why Pop-ins in Alumina Ceramic? 353

      47.3.4 Pop-ins in AIN-SiC Composites and Other Natural Biocomposites 354

      47.3.5 Pop-ins in Tooth Enamel 356

47.4 Conclusions 356

References 357

48. Effect of Loading Rate on Nanoindentation Response of Brittle Solids 359

Riya Chakraborty, Arjun Dey, Nilormi Biswas, Manjima Bhattacharya, Payel Bandyopadhyay, Jyoti Kumar Sharma, Devashish Kaushik, Saikat Acharya, and Anoop Kumar Mukhopadhyay

48.1 Introduction 359

48.2 Loading Rate Effects in Brittle Solids: SLS Glass and Alumina 359

      48.2.1 Loading Rate Study on SLS Glass 361

      48.2.2 Loading Rate Study on Alumina 361

      48.2.3 Loading Rate Study on inside Scratch Groove in SLS Glass 362

      48.2.4 Loading Rate Study on AIN-SiC Composites 362

      48.2.5 Loading Rate Study on Tooth Enamel 362

48.3 Conclusions 364

References 364

49. Measurement of Residual Stress by Nanoindentation Technique 367

Arjun Dey and Anoop Kumar Mukhopadhyay

49.1 Introduction 367

49.2 Measurement of Residual Stress by Nanoindentation: Concept 368

49.3 Evaluation of Residual Stress by Nanoindentation of HAp Coating 369

49.4 Conclusions 370

References 370

50. Reliability Issues in Nanoindentation Measurements 373

Arjun Dey and Anoop Kumar Mukhopadhyay

50.1 Introduction 373

50.2 The Weibull Statistical Distribution 374

50.3 Weibull Analysis for HAp Coating 375

50.4 Weibull Analysis for C/C and C/SiC Composites 377

50.5 Conclusions 378

References 378

51. Substrate Effect in Thin Film Measurements 381

Arjun Dey, I Neelakanta Reddy, N Sridhara, Anju M Pillai, Anand Kumar Sharma, Rajib Paul, A K Pal, and Anoop Kumar Mukhopadhyay

51.1 Introduction 381

51.2 Substrate Effect in Nanocomposite DLC Thin Films 382

51.3 Substrate Effect in Alumina Film 383

51.4 Conclusions 385

References 385

52. Future Scope of Novel Nanoindentation Technique 387

Arjun Dey and Anoop Kumar Mukhopadhyay

52.1 Introduction 387

52.2 Nanoindentation on Biological Materials and Nanostructures 387

52.3 In Situ Nanoindentation and Picoindentation 388

52.4 High Temperature Nanoindentation 388

52.5 Properties other than Hardness and Modulus: a Direct Measurement 388

      52.5.1 Fracture Toughness 389

      52.5.2 Residual Stress 389

      52.5.3 Adhesion Strength 390

      52.5.4 Nanofatigue 390

References 391

Conclusions 395

Common Abbreviations 403

Index 405

Dr. Anoop Kumar Mukhopadhyay is a chief scientist and head of the mechanical property evaluation section in the Materials Charac-terization Division of CSIR-CGCRI, Kolkata, India. He also heads the Program Management Division and Business Development Group of CSIR-CGCRI. He obtained his bachelor's degree with honours in physics from Kalyani University, Kalyani in 1978 followed by a master's degree in physics from Jadavpur University, Kolkata in 1982. In 1978, he initiated in India the research work on evaluation, anal-ysis and microstructure mechanical properties correlation of non oxide ceram-ics, for high temperature applications prior to joining CSIR-CGCRI, Kolkata, India in 1986, as a staff scientist Working on the critical parameters that control the high temperature fracture toughness of silicon nitride and its composites, he earned his Ph D. degree in science, in 1988 from the Jadavpur University, Kolkata. PA\During 1990-1992 he was awarded the prestigious Australian Common-wealth Post Graduate Research Fellowship and made pioneering contribu-tions about the role of grain size in wear of alumina ceramics during his post doctoral work on development of wear and fatigue resistant oxide ceramics with world renowned Prof. Yiu-Wing Mai and Prof. Michael V. Swain at the University of Sydney, Australia. PA\At CSIR-CGCRI, Kolkata, Dr. Mukhopadhyay established an enthusiastic research group on evaluation and analysis of mechanical and nanomechani-cal properties of glass, ceramics, bioceramic coatings and biomaterials, thin films and natural biomaterials. Dr. Mukhopadhyay wrote more than 200 pub-lications. Hewrote7 patents with 3 of them already granted, 2 book chapters already published and two books (in progress) to his credt. He has supervised seven doctoral students including one candidate who has already earned, a PhD at Bengal Engineering and Science University, Shibpur, Howrah in 2011. He contributed three chapters in "Handbook of Ceramics”edited by Dr. S. Kumar, internationally famous glass technologist and former director of CSIR-CGCRI, Kolkata, India and published by Kumar and Associates, Kolkata. He serves on the editorial board of Soft Nanoscience Letters. PA\In 2008, he won the Best Poster Paper Award at the 53rd DAE Solid State Physics Symposium. He also won in 2000 the Sir C V Raman Award of the Acoustical Society of India. In the same year, he also won the Best Poster Paper Award of the Materials Research Society of India. He was also awarded in 2000 the Visiting Scientist Fellowship to work on the fracture and nanoindentation behaviour of ceramic thermal barrier coatings with the world renowned scientist, Dr. R. W. Steinbrech at the Forschungszentrum, Juelich, Germany. He was awarded in 1997 the Outstanding Young Person Award for Science and Innovation by the Outstanding Young Achievers Association, Kolkata and won Lions Club of India award in 1996. His work was recognized in 1995 through the best Best Poster Paper Award of the Materials Research Society of India. PA\Recently in 2010, his paper won the Best Research Paper Award at the Diamond Jubilee Celebration Ceremony of CSIR-CGCRI, Kolkata. His cur-rent research interests cover a truly diverse span, e.g., physics of nanoscale deformation for brittle solids, very high strain rate shock physics of ceram-ics, tribology of ceramics, nanotribology of ceramic coatings and thin films, microstructure mechanical and/or functional property correlation as well as ultrasonic characterisation and fatigue of (a) structural and bio-ceramics, bio-ceramic coatings, bio-materials (b) multilayer composites (c) thick/thin hard ceramic coatings. He also has a very active interest in microwave processing of ceramics, ceramic composites and ceramic metal or ceramic/ceramic joining.

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