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ОбложкаNoriega N.M. New method for the synthesis of BaTiO3 nanoparticles / nanostructures and the production of nanocomposites with mechanically tunable refractive index: Diss. … Dr. rer. nat. - Dresden: TU Dresden, 2015. - vii, 383 p.: ill., tab. - Bibliogr.: p.320-340.
Шифр: (И/Л2-N78) 02
 

Место хранения: 02 | Отделение ГПНТБ СО РАН | Новосибирск

Оглавление / Contents
 
ACKNOWLEDGEMENTS

TABLE OF CONTENT ................................................ i

ABBREVIATIONS ................................................. vii

1   OBJECTIVES, MOTIVATION AND JUSTIFICATION .................... 1

2    BACKGROUND AND STATE OF THE ART ............................ 7
2.1  NANOMATERIALS .............................................. 7
     2.1.1  General Properties and Characteristics .............. 8
       Mechanical Properties .................................... 9
       Thermal Properties ....................................... 9
       Magnetic Properties ..................................... 10
       Electrical and Optical Properties ....................... 10
     2.1.2  Nanoparticles Synthesis ............................ 11
       Sol-Gel (Aqueous and Non-Aqueous) ....................... 12
       Solvothermal / Hydrothermal ............................. 14
       Seed-Mediated Growth  ................................... 16
     2.1.3  Special Nanostructures ............................. 17
     2.1.4  Nanocomposites Preparation ......................... 20
2.2  PIEZOELECTRICS ............................................ 22
     2.2.1  General Concept and Properties ..................... 22
     2.2.2  Barium Titanate - BaTiO3 ........................... 26
     2.2.3  Size Effect in Piezoelectrics/Ferroelectrics ....... 30
2.3  OPTICAL POLYMERS .......................................... 36
     PMMA - Properties and Preparation ......................... 38
     PDMS - Properties and Preparation ......................... 40
2.4  LIGHT - MATTER INTERACTION ................................ 44
     2.4.1  Light - General Properties ......................... 44
     2.4.2  Interaction with Matter ............................ 46
     2.4.3  Propagation and Transmission ....................... 48
       Refraction .............................................. 49
       Scattering .............................................. 50
       Materials Classification According its Transmittance .... 51
     2.4.4  Polarization and Refractive Index .................. 51
2.5  REFRACTIVE INDEX MODIFICATION - STATE OF THE ART .......... 59
     Composition Change ........................................ 60
     Chemical Stimulus ......................................... 64
     Thermal Stimulus .......................................... 64
     Photonic Stimulus ......................................... 64
     Electrical Stimulus ....................................... 65
     Mechanical Stimulus ....................................... 69

3    EXPERIMENTAL SECTION ...................................... 70
3.1  CHEMICALS AND REAGENTS .................................... 70
3.2  EXPERIMENTAL PROCEDURE .................................... 71
     3.2.1  Synthesis of Nanoparticles ......................... 71
       3.2.1.1  ВаТiO3 from Ba(OH)2-8H20 and TiO2 Nanoparticles
         (Nanoparticle Conversion) ............................. 71
       3.2.1.2  ВаТiO3 from Ba(OH)2-8H2O and Titanium (IV)
         Isopropoxide (Alkoxide-Hydroxide) ..................... 74
       3.2.1.3  ВаТiO3 from Barium Oleate and Titanium (IV)
         Isopropoxide (Alkoxide-Oleate) ........................ 77
       3.2.1.4  ВаТiO3 from Ва(ОН)2-8H2O and Ti(OH)62-
         Titanium (IV) Isopropoxide (Modified
         Alkoxide-Hydroxide) ................................... 80
       3.2.1.5  ВаТЮз from Ba(OHfc Anhydrous and Titanium
         (IV) Isopropoxide (Alkoxide- Anhydrous Hydroxide)
         (Urchin Like) ......................................... 83
       3.2.1.6  ВаТiO3 by Seed - Growth ........................ 90
         3.2.1.6.1  Growth by Alkoxide - Hydroxide Approach .... 91
         3.2.1.6.2  Growth by Modified Alkoxide - Hydroxide
           Approach ............................................ 92
         3.2.1.6.3  Growth by Alkoxide - Anhydrous Hydroxide
           Approach ............................................ 93
     3.2.2  Surface Modification of Nanoparticles (Ex-Situ) .... 95
     3.2.3  Preparation of Nanocomposites ...................... 97
       3.2.3.1  PMMA-BaTiO3_OA ................................. 97
       3.2.3.2  PMMA-BaTiO3_R-PO(OH)2 .......................... 99
       3.2.3.3  PMMA_R-PO(OH)2- ВаТiO3 ........................ 101
       3.2.3.4  PDMS-ВаTiO3_ОА ................................ 103
3.3    CHARACTERIZATION TECHNIQUES ............................ 105
     3.3.1  Dynamic Light Scattering (DLS) .................... 105
     3.3.2  Fourier Transform Infrared Spectroscopy (FTIR) .... 106
     3.3.3  Nuclear Magnetic Resonance Spectroscopy
            (Solution NMR) .................................... 106
     3.3.4  Powder X-Ray Diffraction (XRD) .................... 106
     3.3.5  Raman Spectroscopy ................................ 107
     3.3.6  Scanning Electron Microscopy (SEM) ................ 107
     3.3.7  Spectroscopic Ellipsometry ........................ 108
     3.3.8  Thermogravimetric-Differential Thermal Analysis
            (TGA - DTA) ....................................... 111
     3.3.9  Transmission Electron Microscopy (ТЕМ) ............ 111
     3.3.10 UV-Vis Spectroscopy ............................... 111
     3.3.11 Zeta-Potential .................................... 112

4    RESULTS AND DISCUSSION ................................... 113
4.1  SYNTHESIS OF NANOPARTICLES ............................... 113
     4.1.1  BaTiO3 from Ba(OH)2-8H2O and TiO2 Nanoparticles
       (Nanoparticle Conversion) .............................. 114
       Educt Concentration .................................... 114
       Hydrothermal Temperature and Length .................... 118
     4.1.2  BaTiO3 from Ba(OH)2-8H2O and Titanium (IV)
       Isopropoxide (Alkoxide-Hydroxide) ...................... 126
       Oleic Acid Concentration ............................... 128
       Delaying on the Addition of Oleic Acid ................. 134
       Educt Concentration andSolvothermal Length ............. 137
       Solvothermal Temperature and Length .................... 141
     4.1.3  BaTiO3 from Barium Oleate and Titanium (IV)
       Isopropoxide (Alkoxide-Hydroxide/Oleate) ............... 145
       Solvent, Oleate and Precipitation ...................... 146
       Educt Concentration .................................... 157
       Solvothermal Temperature and Length .................... 163
     4.1.4  BaTiO3 from Ba(OH)2-8H2O and Ti(OH)62-
       (from Ti(O-iPr)4) (Modified Alkoxide-Hydroxide) ........ 168
       Proof of Concept (Temperature) ......................... 169
       Titanium to KOH Ratio .................................. 171
       Precipitation Temperature and Length ................... 175
       Solvothermal Temperature and Length .................... 179
     4.1.5  BaTiO3 from Ba(OH)2 Anhydrous and Titanium (IV)
       Isopropoxide (Alkoxide- Anhydrous Hydroxide) (Urchin
       Like) .................................................. 189
       Solvothermal Conditions (temperature and length) and
       Acetone Amount ......................................... 190
       Educt Concentration .................................... 208
       Short Solvothermal Treatments (200°C, <3 Hours) ........ 212
       Barium Hydroxide Alone ................................. 215
       Titanium (IV) Isopropoxide Alone ....................... 221
       No Solvothermai Treatment .............................. 223
     4.1.6  BaTiO3 by Seed - Growth ........................... 230
       4.1.6.1  Growth by Alkoxide - Hydroxide Approach ....... 232
         Reaction Time (Constant Seed Concentration) .......... 232
         Seed Concentration (Constant Educt Concentration) .... 235
         Multi-Step Growth - 80°C ............................. 238
         Multi-Step Growth - 150°C ............................ 241
       4.1.6.2  Growth by Modified Alkoxide - Hydroxide
         Approach ............................................. 244
         Seed Concentration ................................... 244
         Reaction Time (Constant Seed Concentration) .......... 247
       4.1.6.3  Growth by Alkoxide - Anhydrous Hydroxide
         Approach ............................................. 250
4.2  GRAPHICAL SUMMARY OF NANOPARTICLES ....................... 255
4.3  SURFACE MODIFICATION OF NANOPARTICLES .................... 259
4.4  PREPARATION OF NANOCOMPOSITES ............................ 264
     4.4.1  Poly(methyl methacrylate) (PMMA) Based
       Nanocomposites ......................................... 267
       Modification with Oleic Acid - PMMA Solution (Glass
       Substrates) ............................................ 268
       Modification with Phosphonic Acid - PMMA Solution
       (Brass Substrates) ..................................... 273
       Modification with Acrylic Acid - PMMA Solution &
       Phosphonate Terminated PMMA (Brass Substrates) ......... 278
       Modification with Acrylic Acid & Octylamine - PMMA
       Solution & Phosphonate Terminated PMMA (Stainless
       Steel Substrates) ...................................... 284
     4.4.2  Polydimethylsiloxane (PDMS) Based Nanocomposites .. 290
       Modification with Oleic Acid - PDMS In-situ
       Polymerization (Glass Substrates) ...................... 291
       Modification with Oleic Acid - PDMS In-situ
       Polymerization (Stainless Steel Substrates) ............ 294
     4.5  GLOBAL ANALYSIS ..................................... 299

5    CONCLUSIONS AND OUTLOOK .................................. 310

REFERENCES .................................................... 320

APPENDIX ...................................................... 341
     Nanoparticle Conversion .................................. 342
     Alkoxide-Hydroxide ....................................... 343
     Alkoxide-Hydroxide Oleate ................................ 350
     Modified Alkoxide-Hydroxide .............................. 354
     Alkoxide- Anhydrous Hydroxide (Urchin Like) .............. 358
     Seed-Growth (Alkoxide-Hydroxide) ......................... 369
     Seed-Growth (Modified Alkoxide-Hydroxide) ................ 373
     Seed-Growth (Alkoxide- Anhydrous Hydroxide - Urchin
     Like) .................................................... 376
     Preparation of Nanocomposites ............................ 378

Versicherung .................................................. 383

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