Nanoparticulate Materials Synthesis, Characterization, and Processing

KATHY LU, PhD, is a Professor of Materials Science and Engineering at Virginia Tech who teaches both undergraduate and graduate courses. She has authored three book chapters and some 100 papers as well as edited four books. Dr. Lu has been honored with several awards, including the Friedrich Wilhelm Bessel Research Award, Karl Schwartzwalder-PACE Award, and Ralph E. Powe Junior Faculty Enhancement Award.

Preface

About the Author

List of Symbols

List of Abbreviations

Chapter 1 Introduction

1.1. Overview       2

1.2. Nanoparticle-based Materials    3

1.3. Unique Characteristics     4

1.4. Properties      7

1.5. Key Scientific and Technical Challenges       13

1.6. Applications 15

1.7. Processing Overview        17

1.8. Summary      19

Questions   19

References  20

Chapter 2 Nanoparticle Synthesis

2.1. Introduction  3

2.2. Theory 4

2.2.1. Nucleation  4

2.2.1.1. Homogeneous nucleation     4

2.2.1.2. Heterogeneous nucleation    6

2.2.2. Growth       7

2.3. Gas Phase Nanoparticle Synthesis      10

2.3.1. Gas-gas reaction  10

2.3.1.1. Physical vapor synthesis     10

2.3.1.2. Chemical vapor synthesis    18

2.3.1.3. Laser ablation   21

2.3.2. Gas-liquid reaction        27

2.3.3. Gas-solid reaction         30

2.4. Liquid Nanoparticle Synthesis   30

2.4.1. Fundamental method     30

2.4.1.1. Precipitation     30

2.4.1.2. Metal salt reduction    35

2.4.1.3. Hydrolysis        37

2.4.1.4. Solvothermal synthesis        41

2.4.1.5. Cryochemical synthesis       46

2.4.2. Confinement method     48

2.4.2.1. Spray pyrolysis          48

2.4.2.2. Solventless synthesis  53

2.4.3. Composite nanoparticle synthesis    54

2.4.3.1. Core/shell structure    54

2.4.3.2. Electroless deposition 59

2.4.3.3. Templating       60

2.4.3.4. Bio-based synthesis    62

2.4.4. Field-assisted nanoparticle synthesis         65

2.4.4.1. Micelle synthesis        65

2.4.4.2. Laser-assisted synthesis       68

2.4.4.3. Plasma-assisted synthesis    71

2.4.4.4. Microwave-assisted synthesis       73

2.4.4.5. Sonication-assisted synthesis        74

2.4.4.6. Radiation-assisted synthesis          77

2.4.4.7. Electric field assisted synthesis      77

2.5. Solid Nanoparticle Synthesis     78

2.5.1. Milling        78

2.5.2. Reaction between solids          83

2.6. Summary      85

Questions   91

References  93

Chapter 3 Nanoparticle Characterization

3.1. Introduction  2

3.2. Size, Shape, and Morphology    3

3.2.1. Microscopy          4

3.2.1.1. Scanning electron microscopy       4

3.2.1.2. Transmission electron microscopy          5

3.2.1.3. Scanning probe microscopy 7

3.2.2. Dynamic light scattering         9

3.2.3. X-Ray diffraction line broadening    10

3.2.4. Small angle scattering    12

3.2.5. Optical spectroscopy    17

3.3. Energetics and Global Thermodynamics       17

3.4. Surface Area 19

3.5. Porosity and Pore Size     20

3.5.1. Electron imaging  21

3.5.2. Gas adsorption    21

3.6. Structure       23

3.6.1. Surface structure  23

3.6.1.1. Low energy electron diffraction     23

3.6.1.2. Atomic force microscopy     25

3.6.1.3. Scanning tunneling microscopy     25

3.6.2. Bulk structure      27

3.6.2.1. X-ray diffraction        27

3.6.2.2. Electron diffraction    28

3.6.2.3. Neutron diffraction     32

3.7. Composition 32

3.7.1. Surface composition      33

3.7.1.1. Auger electron spectroscopy         33

3.7.1.2. X-ray photoelectron spectroscopy          36

3.7.1.3. Secondary ion mass spectroscopy 38

3.7.2. Bulk composition          40

3.7.2.1. Optical atomic spectroscopy         40

3.7.2.2. X-ray fluorescence spectroscopy   41

3.7.2.3. Energy dispersive X-ray analysis  42

3.7.2.4. Electron energy loss spectroscopy 45

3.7.2.5. Fourier transform infrared spectroscopy          47

3.7.2.6. Ultraviolet-visible absorption spectroscopy     49

3.7.2.7. Raman spectroscopy  52

3.8. Needs in Nanoscale Characterization  54

3.9. Summary      55

Questions   59

References  61

Chapter 4 Nanoparticle-Based Superstructures

4.1. Introduction  2

4.2. Top-down     2

4.2.1. Photolithography 3

4.2.2. Electron beam lithography      13

4.2.3. Ion beam lithography    19

4.2.4. Other top-down processes      21

4.3. Bottom-up    23

4.3.1. Non-directional interactions    26

4.3.1.1. van der Waals forces  26

4.3.1.2. Dipole moments         28

4.3.1.3. Electrostatic interactions      29

4.3.2. Directional interactions 30

4.3.2.1. Covalent bonding       31

4.3.2.2. Hydrogen bonding      33

4.3.4. Field-assisted assembly 35

4.3.5. Capillary forces   36

4.3.6. Other approaches          41

4.4. Hybrid 42

4.4.1. Functionalized interactions     43

4.4.2. Non-functionalized interactions        46

4.5. Templating    48

4.5.1. Natural template  48

4.5.2. Synthetic template         50

4.6. 3D Assembly 57

4.7. Summary      61

Questions   61

References  62

Chapter 5 Nanoparticle-Based Material Shaping

5.1. Introduction  2

5.2. Dry Forming Techniques  3

5.2.1. Uniaxial compaction     3

5.2.2. Cold isostatic pressing  5

5.2.3. Superhigh pressure compaction       6

5.2.4. Dynamic compaction    8

5.3. Semi-dry Forming Techniques   10

5.3.1. Molding      11

5.3.2. Extrusion   14

5.4. Wet Forming Techniques 19

5.4.1. Colloidal suspension     20

5.4.2. Pressure casting   24

5.4.3. Tape casting        28

5.4.4. Freeze casting      31

5.4.5. Gel casting 33

5.4.6. Electrophoretic deposition      36

5.5. Digital Processing Techniques   41

5.5.1. Direct writing       41

5.5.2. Stereolithography          45

5.5.3. Ink-jet printing     48

5.6. Bio-derived Processes      49

5.6.1. Bioactive materials        49

5.6.2. Biomimetic materials     50

5.7. Summary      51

Questions   55

References  55

Chapter 6 Sintering

6.1. Introduction  2

6.2. Theories        2

6.2.1. Sintering stages    2

6.2.2. Shrinkage   3

6.2.3. Grain growth       4

6.3. Characteristics of Nanoparticle Sintering      6

6.3.1. Designer systems 6

6.3.2. Particle size distribution and packing characteristics    7

6.3.3. Complex systems 8

6.3.4. Phase transformation    8

6.3.5. Lower sintering temperature   9

6.3.6. Larger sintering driving force  11

6.4. Porous Nanoparticle Material Sintering        12

6.4.1. Partial sintering   13

6.4.2. Pore forming sintering   16

6.4.3. Template-directed sintering     20

6.4.4. Special sintering processes     23

6.4.4.1. Microwave sintering   23

6.4.4.2. Electrical sintering      27

6.4.4.3. Laser sintering  29

6.5. Dense Nanoparticle-based Material Sintering         30

6.5.1. Free sintering       30

6.5.1.1. Customized nanoparticle systems 30

6.5.1.2. Customized sintering cycles 34

6.5.1.3. Remarks on free sintering    38

6.5.2. Pressure sintering 38

6.5.2.1. Hot pressing     39

6.5.2.2. Hot isostatic pressing 43

6.5.2.3. Sinter forging    45

6.5.2.4. Pressure spark plasma sintering    46

6.5.2.5. Other sintering techniques   52

6.6. Summary      53

Questions   54

References  57

Chapter 7 Manufacturing Issues and Emerging Areas

7.1. Introduction  2

7.2. Defects and Measurement 3

7.3. Process and Quality Control      8

7.4. Modeling and Simulation 9

7.5. Environmental and Health Concerns   13

7.5.1. Environmental concerns         14

7.5.2. Health concerns    16

7.6. Summary      18

Questions   19

References  19

Appendix 1 Nomenclatures

Appendix 2 Units

Index

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