矽烷接枝二氧化矽奈米顆粒及蒙特納石黏土對不飽和聚酯、乙烯基酯、及環氧樹脂之体積收縮、內部可染色性、機械性質及微觀型態結構之影響研究

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研究生：	許麗琪 Yuliana - Tassia
論文名稱：	矽烷接枝二氧化矽奈米顆粒及蒙特納石黏土對不飽和聚酯、乙烯基酯、及環氧樹脂之体積收縮、內部可染色性、機械性質及微觀型態結構之影響研究 Effects of silane-grafted silica nanoparticles and montmorillonite clay on the volume shrinkage, internal pigmentability, mechanical properties and cured sample morphology for unsaturated polyester, vinyl ester, and epoxy resins
指導教授：	黃延吉 Yan-Jyi Huang
口試委員:	陳崇賢 Chorng-Shyan Chern 邱文英 Wen-Yen Chiu
學位類別：	碩士 Master
系所名稱：	工程學院 - 化學工程系 Department of Chemical Engineering
論文出版年：	2013
畢業學年度：	101
語文別：	英文
論文頁數：	286
中文關鍵詞：	silane 、silica nanoparticle 、montmorillonite (MMT) 、unsatured polyester (UP) 、vinyl ester resin (VER) 、interfacial adhesion 、volume shrinkage
外文關鍵詞：	silane, silica nanoparticle, montmorillonite (MMT), unsatured polyester (UP), vinyl ester resin (VER), interfacial adhesion, volume shrinkage
相關次數：	點閱：312 下載：6
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The synthesis of silane-grafted silica nanoparticles with different size (d = 15 and 30 nm) and montmorillonite clay (MMT) with the subsequent characterization of the grafting efficiency, grafting density, as well as the surface silanol groups conversion have been carried out. The silane coupling agents used for the treatment are γ-methacryloxy propyl trimethoxy silane (MPS) and γ-glycidyloxy propyl trimethoxy silane (GPS). The effects of those silane-modified silica nanoparticles and MMT on the volume shrinkage characteristics, internal pigmentability, mechanical properties, and cured sample morphology for styrene (St)/unsaturated polyester (or vinyl ester)/additive ternary systems have been carried out.
The number of silane coupling agents grafted on the MMT or silica surface and their silanol groups conversion were characterized by Fourier Transform Infrared Spectroscopy (FTIR). The cured sample morphology was observed by Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM). The volume shrinkage of the cured sample was measured by density method. Mechanical properties of the St/VER(n=2)/MPS-grafted silica (d = 30 nm) was investigated by using the universal testing machine and impact tester.
The addition of silane-grafted MMT or silica nanoparticles reveals different results in the reduction of volume shrinkage for different UP or VER, each with different molecular weight, which is due to the incompatibility of the ternary system. Higher viscosity of the resin matrix, the characteristics of the silane-grafted MMT or silica nanoparticles, and the interfacial adhesion determine the sufficient incompatibility between the additive and the resin matrices. Therefore, an acceptable volume shrinkage and even a volume expansion could be achieved.

ACKNOWLEDGMENTS								          i
TABLE OF CONTENTS								         ii
LIST OF TABLES									      viii
LIST OF FIGURES									        xi
ABSTRACT										    xxiv
CHAPTER I INTRODUCTION							          1
I. 1. Inorganic/Organic Core-Shell Structure Using SiO2 as the Core		          1
I. 2. Preparation of SiO2 Particles							          2
I. 3. Montmorillonite (MMT) and MMT/Polymer Nanocomposites			          2
I. 4. Unsaturated Polyester, Vinyl Ester, and Epoxy Resins			          	          5
I. 5. Volume Shrinkage, Pigmentability, and Mechanical Properties for St/UP or VER/Additive Ternary Systems						         	          6
I. 6. Objectives									          8
CHAPTER II LITERATURE OVERVIEW						          9
II. 1. Unsaturated Polyester (UP) Resin						          9
II. 2. Vinyl Ester Resins (VER)							        14
II. 3. Epoxy Resin									        18
II. 4. Inorganic Nanofillers                                       					        22
II. 4. 1. Montmorillonite (MMT) nanoclay						        23
II. 4. 2. Silica nanoparticle								        26
II. 5. Silane Coupling Agents and Silane Modification				        28
II. 6. Polymer Nanocomposites							        31
II. 6. 1. Polymer/MMT nanocomposites						        34
II. 6. 2. Polymer/silica nanocomposites 						        35
II. 7. Segregating Effect Mechanism 							        36
CHAPTER III EXPERIMENTAL 							        39
III. 1. Materials 									        39
III. 1. 1. Unsaturated Polyester (UP) Resin 						        39
III. 1. 2. Epoxy Resin (EPR)								        39
III. 1. 3. Vinyl Ester Resin (VER) 							        39
III. 1. 4. Styrene, ACROS								        43
III. 1. 5. 4,4’-diaminodiphenyl methane (DDM), ACROS				        43
III. 1. 6. 4,4’-diaminodiphenylsulfone (DDS), ACROS				        43
III. 1. 7. Tert-butyl peroxybenzoate (TBPB), ACROS				        44
III. 1. 8. 1,4-Benzoquinone (BQ), ACROS						        44
III. 1. 9. Montmorillonite Clay (MMT) PK-805, Pai Kong Tech Nanotechnology Co     44
III. 1. 10. Sodium Chloride (NaCl), ACROS						        45
III. 1. 11. Silver nitrate (AgNO3), ACROS						        45
III. 1. 12. Activated silica nanoparticles, self synthesized				        45
III. 1. 13. γ-methacryloxy propyl trimethoxy silane (MPS), A-174, OSI Specialties       45
III. 1. 14. γ-glycidyloxy propyl trimethoxy silane (GPS), Sigma-Aldrich		        46
III. 1. 15. Methanol (CH3OH), ACROS						        46
III. 1. 16. Potassium Bromide (KBr, IR Grade), International Crystal Labs		        46
III. 1. 17. Bordeaux R, ACROS							        46
III. 1. 18. Dichloromethane (CH2Cl2), ACROS					        47
III. 1. 19. 12-aminolauric acid (12-ALA), Sigma-Aldrich				        47
III. 1. 20. Hydrochloric acid (HCl), ACROS						        47
III. 1. 21. Deionized water								        47
III. 1. 22. Acetone									        47
III. 2. Instrumentation									        48
III. 2. 1. Round bottom reaction vessels (1 L and 5 L), IWAKI, Asahi Techno Glass      48
III. 2. 2. High performance centrifuge system, Avanti J-25				        48
III. 2. 3. Vacuum oven								        48
III. 2. 4. Metal mortar and pestle							        48
III. 2. 5. 200-mesh sieve, Bunsekifurui					                    48
III. 2. 6. Thermostated silicon oil bath and water bath				        48
III. 2. 7. Digital hot plate stirrer, Cimarec, Barnstead/Thermolyne 			        48
III. 2. 8. Fourier Transform Infrared Spectroscopy (FTIR), Nicolet iS10, Thermo Scientific										        49
III. 2. 9. Differential Scanning Calorimeter (DSC), Q20, TA Instruments		        49
III. 2. 10. Pycnometer									        49
III. 2. 11. Aluminum plate (50 × 50 × 2 mm)						        49
III. 2. 12. Electronic densimeter, MD-200S, MIRAGE			    	        49
III. 2. 13. Digital balance								        49
III. 2. 14. Vacuum pump, G-50DA, ULVAC Company 			 	        49
III. 2. 15. Aluminum mold							                    50
III. 2. 16. Dumbbell type of mold							        50
III. 2. 17. Universal testing machine, Testometric M500-25AT			        50
III. 2. 18. Impact tester, BPI Basic Pendulum Impact Tester, Dynisco		        50
III. 2. 19. Grinding machine								        50
III. 2. 20. Field Emission Scanning Electron Microscope (FE-SEM), Hitachi S-800       50
III. 2. 21. Transmission Electron Microscope, TEM, Hitachi H-7100		        50
III. 2. 22. Chromameter, CR-300, MINOLTA					        51
III. 2. 23. Small-Angle X-ray Scattering (SAXS) system, Rigaku Innovative Technology, Inc., USA									  	        51
III. 2. 24. Digital pH/MVmeter, TS-1, SUNTEX				                    51
III. 2. 25. Mechanical stirrer, Eurostar digital (EURO-ST D S1), IKA-WERKE	        51
III. 2. 26. Microviscometer, Lovis 2000M, Anton Paar				        51
III. 3. Procedure of Experiment							        52
III. 3. 1. Sodium Activation of Neat MMT PK-805 (Na-MMT)26,57			        52
III. 3. 2. Silane Treatment of MMT26,57 or Silica (Silane-grafted MMT or Silica) 	        52
III. 3. 3. Characterization of Silane-grafted MMT or Silica by using FTIR  		        52
III. 3. 4. DSC Experiment for St/UP(MA-PA-PG)AN~20 system with MR=2/1 	        54
III. 3. 5. Cured Sample Preparation for Volume Shrinkage Study 			        55
III. 3. 6. Cured Sample Preparation for Mechanical Properties Study		        56
III. 3. 7. Cured Sample Preparation for Morphological Study by SEM		        59
III. 3. 8. Cured Sample Preparation for WAXS					        59
III. 3. 9. Cured Sample Preparation for Internal Pigmentability Study		        59
III. 3. 10. Alkyl-ammonium Treatment of MMT (AMMT)57,133			        60
III. 4. Experimental Calculation						 	        61
III. 4. 1. Characterization of Silane-grafted MMT or Silica by using FTIR		        61
III. 4. 2. Sample Composition								        62
III. 4. 3. Volume Shrinkage of Cured Sample					        63
CHAPTER IV RESULTS AND DISCUSSION					        65
IV. 1. Characterization of MPS-grafted MMT by using FTIR			        65
IV. 2. Characterization of MPS-grafted silica (d = 15 and 30 nm) by using FTIR	        87
IV. 2. 1. MPS-grafted silica (d = 15 nm)						        93
IV. 2. 2. MPS-grafted silica (d = 30 nm)					 	      103
IV. 3. Characterization of GPS-grafted silica (d = 15 nm) by using FTIR		      113
IV. 4. DSC Experiment for Neat St/UP(MA-PA-PG)AN~20 at MR = 2/1		      133
IV. 5. Static Phase Separation Characteristics for St/UP (or VER)/Additive Ternary Systems Prior to Cure									      136
IV. 6. Microstructure morphology of Cured Sample					      140
IV. 6. 1. SEM Micrographs								      140
IV. 6. 1. 1. Effects of Resin for St/VER and St/UP Binary System			      140
IV. 6. 1. 2. Effects of MPS-grafted MMT Concentrations for VER(n=2) Ternary Systems												      144
IV. 6. 1. 3. Effects of MPS-grafted silica (d = 15 nm) Concentrations for VER(n=2) Ternary Systems									      151
IV. 6. 1. 4. Effects of MPS-grafted silica (d = 30 nm) Concentrations for VER(n=2) Ternary Systems								 	      158
IV. 6. 1. 5. Effects of MPS-grafted MMT and MPS-grafted silica (d = 15 nm) for UP(MA-PG)AN~20 Ternary Systems							      164
IV. 6. 1. 6. Effects of MPS-grafted MMT and MPS-grafted silica (d = 15 nm) for UP(MA-PA-PG)AN~20 Ternary Systems						      172
IV. 6. 2. TEM Micrographs								      180
IV. 6. 2. 1. St/VER(n=2) Binary Systems						      180
IV. 6. 2. 2. Effects of MPS-grafted MMT Concentrations for VER(n=2) Ternary Systems												      181
IV. 6. 2. 3. Effects of MPS-grafted silica (d = 15 nm) Concentrations for VER(n=2) Ternary Systems									      187
IV. 6. 2. 4. Effects of MPS-grafted silica (d = 30 nm) Concentrations for VER(n=2) Ternary Systems									      193
IV. 7. The Takayanagi Models							      199
IV. 8. Volume Shrinkage of Cured Sample						      201
IV. 8. 1. Effects of Resin for St/VER and St/UP Binary Systems			      201
IV. 8. 2. Effects of MPS-grafted MMT Concentration and Resin Viscosity for VER Ternary Systems									      206
IV. 8. 3. Effects of MPS-grafted Silica Particle Size and Concentration for VER(n=2) Ternary Systems									      210
IV. 8. 4. Effects of MPS-grafted MMT Concentration and Resin Viscosity for UP(MA-PG) Ternary Systems									      213
IV. 8. 5. Effects of MPS-grafted MMT Concentration and Resin Viscosity for UP(MA-PA-PG) Ternary Systems								      217
IV. 9. Effects of MPS-grafted silica (d = 30 nm) Concentrations on Mechanical Properties of VER(n=2) Ternary Systems						      221
IV. 10. WAXS Measurements for Neat MMT Systems				      230
IV. 11. Radius of Gyration for UP and VER Resins by SAXS			      236
CHAPTER V CONCLUSIONS							      238
CHAPTER VI FUTURE WORK							      240
CHAPTER VII REFERENCES							      241
APPENDIX										     A-1

                                

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