Polymer Morphology - Qipeng Guo

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Résumé :

Preface xiii

List of Contributors xv

Part I Principles and Methods of Characterization 1

1 Overview and Prospects of Polymer Morphology 3
Jerold M. Schultz

1.1 Introductory Remarks 3

1.2 Experimental Avenues of Morphological Research 4

1.2.1 Morphological Characterization: The Enabling of in situ Measurements 4

1.2.2 Morphology-Property Investigation 5

1.2.3 Morphology Development 7

1.3 Modeling and Simulation 8

1.3.1 Self-Generated Fields 9

1.4 Wishful Thinking 11

1.5 Summary 11

References 12

2 X-ray Diffraction from Polymers 14
N. Sanjeeva Murthy

2.1 Introduction 14

2.2 Basic Principles 14

2.3 Instrumentation 16

2.4 Structure Determination 17

2.4.1 Lattice Dimensions 17

2.4.2 Molecular Modeling 18

2.4.3 Rietveld Method 18

2.4.4 Pair Distribution Functions 18

2.5 Phase Analysis 19

2.5.1 Crystallinity Determination 20

2.5.2 Composition Analysis 21

2.6 Crystallite Size and Disorder 21

2.7 Orientation Analysis 22

2.7.1 Crystalline Orientation 22

2.7.2 Uniaxial Orientation 22

2.7.3 Biaxial Orientation 24

2.7.4 Amorphous Orientation 25

2.8 Small-Angle Scattering 25

2.8.1 Central Diffuse Scattering 26

2.8.2 Discrete Reflections from Lamellar Structures 27

2.8.3 Small-Angle Neutron Scattering and Solvent Diffusion 29

2.9 Specialized Measurements 30

2.9.1 In situ Experiments 30

2.9.2 Microbeam Diffraction 31

2.9.3 Grazing Incidence Diffraction 32

2.10 Summary 33

References 33

3 Electron Microscopy of Polymers 37
Goerg H. Michler and Werner Lebek

3.1 Introduction 37

3.2 Microscopic Techniques 37

3.2.1 Scanning Electron Microscopy (SEM) 37

3.2.2 Transmission Electron Microscopy (TEM) 42

3.2.3 Comparison of Different Microscopic Techniques 45

3.2.4 Image Processing and Image Analysis 46

3.3 Sample Preparation 47

3.4 In situ Microscopy 50

References 52

4 Characterization of Polymer Morphology by Scattering Techniques 54
Jean-Michel Guenet

4.1 Introduction 54

4.2 A Short Theoretical Presentation 55

4.2.1 General Expressions 55

4.2.2 The Form Factor 56

4.3 Experimental Aspects 60

4.3.1 The Contrast Factor 60

4.3.2 Experimental Setup 61

4.4 Typical Results 62

4.4.1 Neutrons Experiments: A Contrast Variation Story 62

4.4.2 X-Ray Experiments: A Time-Resolved Story 67

4.5 Concluding Remarks 69

References 69

5 Differential Scanning Calorimetry of Polymers 72
Alejandro J. M?ller and Rose Mary Michell

5.1 Introduction to Differential Scanning Calorimetry. Basic Principles and Types of DSC Equipment 72

5.2 Detection of First-Order and Second-Order Transitions by DSC. Applications of Standard DSC Experiments to the Determination of the Glass Transition Temperature and the Melting Temperature of Polymeric Materials 74

5.3 Self-Nucleation 75

5.3.1 Quantification of the Nucleation Efficiency 77

5.4 Thermal Fractionation 78

5.5 Multiphasic Materials: Polymer Blends and Block Copolymers. Fractionated Crystallization and Confinement Effects 81

5.5.1 Blends and Fractionated Crystallization 81

5.5.2 Copolymers 85

5.5.3 Copolymers Versus Blends 87

5.5.4 The Crystallization of Polymers and Copolymers within Nanoporous Templates 88

5.6 Self-Nucleation and the Efficiency Scale to Evaluate Nucleation Power 91

5.6.1 Supernucleation 93