1 INTRODUCTION ................................................. 1
2 NANOPARTICLE-POLYMER-COMPOSITES - A STATE OF THE ART ......... 4
2.1 Terminology ............................................. 5
2.1.1 Nanomaterials .................................... 5
2.1.2 Polymers ......................................... 7
2.1.3 State of Dispersion .............................. 8
2.2 Composite Synthesis/Preparation ......................... 9
2.2.1 Separate Synthesis of Particles and Polymers ..... 9
2.2.2 Synthesis of Nanoparticles within the Polymer ... 12
2.2.3 Synthesis of the Polymer with the Presence
of Nanoparticles ................................ 13
2.3 Industrial Products .................................... 14
3 THESIS MOTIVATION - DEVELOPMENT OF A MODULAR PROCESS CHAIN
FOR COMPOSITE PREPARATION ................................... 16
3.1 Process Steps .......................................... 16
3.1.1 Nanoparticle Synthesis .......................... 17
3.1.2 Liquid-Liquid Phase-Transfer .................... 17
3.1.3 Polymer Addition ................................ 18
3.1.4 Spray Drying .................................... 19
3.1.5 Powder Agglomeration ............................ 20
3.2 Composition ............................................ 21
3.2.1 Composite Composition ........................... 21
3.2.2 Colloid Composition ............................. 24
4 FOCUS ON THE PHASE TRANSFER OF NANOPARTICLES ................ 26
4.1 Theory ................................................. 26
4.1.1 Phase Transfer .................................. 26
4.1.2 Adsorption of Surfactants ....................... 27
4.1.3 Steric Stabilization ............................ 30
4.2 Physical Model of De agglomeration at the Interface .... 33
4.2.1 Gedankenexperiment .............................. 33
4.2.2 Geometrical Model ............................... 34
4.2.3 Numerical Results ............................... 36
4.3 Experimental Results ................................... 38
4.3.1 Visualization of the Phase Transfer ............. 38
4.3.2 Particle (Agglomerate) Size Distribution ........ 40
4.3.3 Primary Particle Concentration .................. 41
4.3.4 Inert Decomposition of Chemisorbed Ricinoleic
Acid on Magnetite Nanoparticles ................. 44
5 NANOPARTICLES AND POLYMERS IN AN ORGANIC SOLVENT ............ 51
5.1 Theory ................................................. 52
5.1.1 Polymers in Solution ............................ 52
5.1.2 Solubility ...................................... 57
5.1.3 Phenomena in Nanoparticle Polymer Mixtures ...... 59
5.2 Pair Interactions - DLVO-IIke Consideration ............ 60
5.3 Experimental Results ................................... 64
5.3.1 Influence of the Polymer ........................ 65
5.3.2 Influence of the Surfactant ..................... 73
5.3.3 Stabilization by Adsorption of PVB .............. 77
5.3.4 Influence of Mechanical Dispersing Methods on
the Stability ................................... 83
5.3.5 Kinetics of Flocculation at Low Nanoparticle
Concentration and high PMMA concentrations ...... 86
5.3.6 Influence of the Solvent ........................ 88
6 HIGHLY FILLED COMPOSITES .................................... 94
6.1 Theory ................................................. 94
6.1.1 Spray Drying .................................... 94
6.1.2 (Micro) Injection Molding ...................... 101
6.1.3 Image Processing and the Mathematical
Description of the State of Dispersion ......... 101
6.1.4 Filler Concentration - Agglomerate
Concentration - Stability Relation ............. 104
6.2 Experimental Results - Spray-Dried Microparticle
Composites ............................................ 107
6.2.1 Compositional Separation ....................... 107
6.2.2 Yield of Product ............................... 111
6.2.3 Influence of the Polymer ....................... 112
6.2.4 Influence of the Surfactant .................... 113
6.2.5 Increasing Filler Concentration F .............. 116
6.3 Experimental Results - Injection Molded Composites .... 119
6.3.1 PMMA vs. PC vs. PVB ............................ 120
6.3.2 Increasing Filler Concentration - PMMA
composite ...................................... 126
6.3.3 Identity of Agglomerates ....................... 128
6.3.4 Solution and Spray Drying Process vs. Melt
Mixing ......................................... 130
7 GENERAL CONCLUSIONS AND OUTLOOK ............................ 132
APPENDIX ...................................................... Al
REFERENCES ..................................................... Rl
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