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Title Page
Contents
ABSTRACT 12
CHAPTER 1 : Synthesis of Ni-Ag Core-Shell Nanoparticles by polyol process 13
1-1. Introduction 13
1-1-1. Core-shell nanoparticles 13
1-1-2. Methods for making core-shell nanoparticles 14
1-1-3. Ni-Ag core-shell nanoparticles and new method for making Ni-Ag core-shell nanoparticles 16
1-2. Experiment 17
1-2-1. Materials 17
1-2-2. Characterization 17
1-2-3. Synthesis of Ni-Ag core-shell nanoparticles 18
1-3. Result and discussion 19
1-3-1. Effect of capping agent 19
1-3-2. Effect of reaction time and reaction temperature to formation of Ni-Ag core-shell nanoparticles 21
1-3-3. The thermal oxidation resistance of Ni-Ag nanoparticles 24
1-4. Conclusions 26
CHAPTER 2 : Synthesis of hollow silica by St ber method with PSS and PAA as templates 27
2-1. Introduction 27
2-1-1. Hollow nanoparticles : properties, preparation and application 27
2-1-2. Hollow silica nanoparticles : properties, preparation and applications 28
2-1-3. The previous known process for making hollow silica 30
2-1-4. The new procedure for making hollow silica 31
2-2. Experiment 33
2-2-1. Material 33
2-2-2. Characterization 33
2-2-3. Synthesis of hollow silica spheres 34
2-3. Result and discussion 39
2-3-1. Synthesis of silica spheres with PAA as template 39
2-3-2. Synthesis of silica spheres with PSS as template 40
2-3-3. Synthesis of silica spheres with both of PAA and PSS as template 41
2-3-4. Making hollow silica in the presemce of aluminum alkoxide 53
2-4. Conclusions 58
REFERENCES 60
국문요약 66
Table 1 : Synthesis of hollow silica with various mole ratios between PSS and PAA. 35
Table 2 : Synthesis of hollow silica with various TEOS amounts 36
Table 3 : Synthesis of hollow silica with various concentrations of template solution 36
Table 4 : Synthesis of hollow silica with various solvent of template solution 37
Table 5 : Synthesis of hollow silica without MTMS 38
Table 6 : Synthesis of hollow silica with aluminum alkoxide 39
Table 7 : Properties of silica spheres with various mole ratios between PSS and PAA 41
Table 8 : BET data of samples which were synthesized in the presence of aluminum alkoxide 57
Figure 1-1 : Core-shell structure of nanoparticles 13
Figure 1-2 : Fabrication procedure of a Silver nanoshell on the Silica sphere by seed-mediated growth technique 14
Figure 1-3 : Schematics of pulsed sonoelectrochemical apparatus including the Sinaptec Linea S23-10-1/2 sonotrode 16
Figure 1-4-a : X-ray diffraction pattern of the Ni nanoparticles synthesized using polyol 20
Figure 1-4-b : X-ray diffraction pattern of the Ni nanoparticles synthesized using polyol process within PVP capping agent. 20
Figure 1-5 : TEM image of the Ni nanoparticles synthesized using polyol process at different magnifications 21
Figure 1-6 : TEM images of the Ni/Ag core/shell nanoparticles synthesized via polyol process at 120℃ for 1hr 22
Figure 1-7 : EDS of the Ni-Ag core-shell nanoparticles synthesized via polyol process at 120℃ for 1hr 22
Figure 1-8 : TEM images of the Ni/Ag core/shell nanoparticles synthesized via polyol process at 120℃ for 5 hours 22
Figure 1-9 : EDS the Ni/Ag core/shell nanoparticles synthesized via polyol process at 120℃ for 5 hours 23
Figure 1-10 : TEM images of the Ni/Ag core/shell nanoparticles synthesized at 60℃ for 7 days using polyol process, (a) scale bar 100nm and (b) 10nm 24
Figure 1-11-a : X-ray diffraction pattern of (a) Ni nanoparticles synthesized using polyol process dried at various temperatures. 25
Figure 1-11-b : X-ray diffraction pattern of Ni/Ag core/shell nanoparticles synthesized using polyol process dried at various temperatures. 25
Figure 2-1 : General synthesis of hollow nanoparticles using templates 28
Figure 2-2 : Schematic diagram of the formation mechanism of hollow silica spheres 32
Figure 2-3 : X-ray diffraction pattern of silica spheres using PAA as templates 39
Figure 2-4 : TEM image of silica spheres obtained using PAA as templates, (a) scale bar 500nm and (b) 200nm. 40
Figure 2-5 : X-ray diffraction pattern of silica spheres using PSS as templates 40
Figure 2-6 : TEM image of calcined silica spheres obtained using PSS as templates, (a) and (b) scale bar 500nm and (c) 200nm. 41
Figure 2-7 : TEM image of calcined silica spheres obtained using both of PSS and PAA as templates with mole ratio PSS : PAA＝1 : 0.75, (a) scale bar 500nm and (b) 200nm (sample P1) 42
Figure 2-8 : TEM image of calcined silica spheres obtained using both of PSS and PAA as templates with mole ratio PSS : PAA＝1 : 1, (a) scale bar 500nm and (b) 50nm (sample P2). 42
Figure 2-9 : TEM image of calcined silica spheres obtained using both of PSS and PAA as templates with mole ratio PSS : PAA＝1 : 1.5, (a) scale bar 500nm and (b) 200nm (sample P3). 43
Figure 2-10 : TEM image of calcined silica spheres obtained using both of PAA and PSS as templates with mole ratio PSS : PAA＝1 : 2, (a) scale bar 200nm and (b) 100nm (sample P4). 43
Figure 2-11 : TEM image of calcined silica spheres obtained using both of PSS and PAA as templates with ratio PSS : PAA＝1:3 (a) scale bar 500nm and (b) 100nm (sample P5) 44
Figure 2-12 : TEM image of calcined silica spheres obtained using both of PSS and PAA as templates with mole ratio PSS : PAA =1 : 1.5 (0.042g : 0.22 g), (a) scale bar 200nm and (b) 100nm (sample P6) 45
Figure 2-13 : TEM image of silica spheres obtained using 0.375mL of TEOS 45
Figure 2-14 : (a) SEM and (b) TEM image of hollow silica spheres obtained using 0.50mL TEOS 45
Figure 2-15 : (a) SEM and (b) TEM image of hollow silica spheres obtained using 0.75mL TEOS 46
Figure 2-16 : (a) SEM and (b) TEM image of hollow silica spheres obtained using 1.00mL TEOS 46
Figure 2-17 : (a) SEM and (b) TEM image of the sample sample C1 (with template solution is diluted in 60mL C2H5OH)(이미지참조) 47
Figure 2-18 : (a) SEM and (b) TEM image of the sample sample C2 (with template solution is diluted in 90mL C2H5OH)(이미지참조) 48
Figure 2-19 : (a) SEM and (b) TEM image of the sample C3 (with template solution is diluted in 150mL C2H5OH)(이미지참조) 48
Figure 2-20 : The sample which used methanol as the solvent (a) before and (b) after washing 2 times by water 49
Figure 2-21 : TEM image of sample which used PGMEA as the solvent, scale bar (a) 200nm and (b) 100nm 50
Figure 2-22 : SEM images of the samples (a) without MTMS (C₂) and (b) within MTMS (Co) 51
Figure 2-23 : Thermogravimetric analysis of PSS and PAA 52
Figure 2-24 : Thermogravimetric analysis of hollow silica before calcination 53
Figure 2-25 : TEM image of sample C1 after calcination 54
Figure 2-26 : TEM image of hollow silica which was synthesized in present of aluminum alkoxide after washing by NaOH 54
Figure 2-27 : TGA of sample A1 which was washed by H₂O and NaOH 55
Figure 2-28-a : EDS of the sample which was washed by H₂O 56
Figure 2-28-b : EDS of the sample which was washed by NaOH 56
Figure 2-29 : N₂ adsorption isotherm of sample which was washed by (a) H₂O and (b) NaOH 57
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