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title page
Abstract
Contents
1. Introduction 15
2. Literature survey 17
2.1. Ni(OH)₂ 17
2.1.1. Crystal structure of Ni(OH)₂ 17
2.1.2. Ni-MH batteries 19
2.1.2.1. Improvement of Ni-MH cell energy density 19
2.2. Hydrothermal process for fabrication of nanocrystals 24
2.2.1. Hydrothermal process[34-38] 24
2.2.2. Method of hydrothermal process 25
2.2.2.1. Temperature-difference method 25
2.2.2.2. Temperature-reduction technique 25
2.2.2.3. Metastable-phase technique 25
2.2.3. Fabrication of Ni(OH)₂by using hydrothermal process 26
2.3. Mechanism for crystal structure, size and shape of nanocrystals 28
2.3.1. Crystal structure control 28
2.3.2. Shape control of nanocrystals[46] 31
2.3.2.1. Thermodynamic theory 31
2.3.2.2. Selective-adsorption model 31
2.3.2.3. Effective-monomer model 32
2.3.2.4. Hofmeister series[47] 33
2.3.3. Size control of nanocrystals[75] 36
3. Experimental procedures 39
3.1. Fabrication process of Ni(OH)₂nanocrystals 39
3.1.1. Chemicals 39
3.1.2. Reaction apparatus 39
3.1.3. Heating and cooling profile 42
3.2. Characterization of Ni(OH)₂nanocrystals 44
3.2.1. Microstructure of Ni(OH)₂nanocrystals 44
3.2.2. X-ray diffraction 44
3.2.3. Fourier transformation infrared spectroscopy 44
3.2.4. BET analysis 44
3.2.5. TGA/DSC analysis 45
4. Results and discussions 46
4.1. Fabrication of Ni(OH)₂nanocrystals 46
4.1.1. Microstructures of mixture of crystal and amorphous Ni(OH)₂ 46
4.1.2. Fabrication of Ni(OH)₂nanocrystals by HTHP reaction 46
4.2. Effect of process parameters on size of Ni(OH)₂nanocrystals 55
4.2.1. Effect of reaction temperature on Ni(OH)₂nanocrystals 55
4.2.2. Effect of reaction time on Ni(OH)₂nanocrystals 55
4.3. Effect of process parameters on shape of Ni(OH)₂nanocrystals 61
4.3.1. Effect of reaction temperature and time on Ni(OH)₂nanocrystals 61
4.3.2. Effect of pH control on Ni(OH)₂nanocrystals 64
4.3.3. Effect of anion on Ni(OH)₂nanocrystals 67
4.3.4. Effect of surfactant on Ni(OH)₂nanocrystals 71
4.4. Effect of anion on crystal structure of Ni(OH)₂nanocrystals 73
5. Conclusions 86
Future plans 88
국문요약 89
References 91
감사의 글(Acknowledgement) 96
Table 2.1. List of various precursors, precipitators, condition and results in the hydrothermal process. 27
Fig. 2.1. Crystal structure of Ni(OH)₂ 18
Fig. 2.2. Comparison of energy density of the secondary batteries. 21
Fig. 2.3. Scheme of charging reaction of Ni-HM battery. 22
Fig. 2.4. Weight percentage distribution of battery components. 23
Fig. 2.5. Relation between hexagonal and monoclinic structure of CuFeO₂ 29
Fig. 2.6. Schematic representation of intercalation of DIK via anionic exchange. 30
Fig. 2.7. TEM micrograph of Nanocrystals obtained by adding 10³M of various anions. The chemical reaction is ended after 3h. 35
Fig. 2.8. (a) Reverse micelles, (b) control of nanocrystal size with w, that is, control of the size of water-in-oil droplets. 38
Fig. 2.9. Silver nanocrystals made in reverse micellar solution. (a) Decahedron. (b) Icosahedron. (c) Cubo-octahedron. 38
Fig. 3.1. Fabrication process of Ni(OH)₂ Nanocrystals. 40
Fig. 3.2. Apparatus for fabrication of Ni(OH)₂Nanocrystals by hydrothermal process (HTHP reactor), 1.Reaction Vessel, 2.Thermocouple, 3.Bent, 4.Gas controller, 5.Outlet for gas, 6. Stirring controller. 41
Fig. 3.3. Typical time-temperate profile for fabrication of Ni(OH)₂nanocrystals by hydrothermal process. 43
Fig. 4.1. Mixture of Amorphous and crystal Ni(OH)₂. 48
Fig. 4.2. (a) Ni(OH)₂Nanocrystals (b) Amorphous Ni(OH)₂. 49
Fig. 4.3. XRD pattern of previous fabricated Ni(OH)₂. 50
Fig. 4.4. (a) DSC curve of Ni(OH)₂. 51
Fig. 4.4. (b) TGA curve of Ni(OH)₂ (c) DTG curve of Ni(OH)₂. 52
Fig. 4.5. Ni(OH)₂ with perfect crystallization. 53
Fig. 4.6. XRD pattern of Ni(OH)₂ with perfect crystallization. 54
Fig. 4.7. TEM micrographs of Ni(OH)₂ nanocrystals fabricate by hydrothermal process. (a) 150°C and 0 min (b) 200°C and 0 min. 56
Fig. 4.8. TEM micrographs of Ni(OH)₂ nanocrystals fabricate by hydrothermal process. (a) 150°C and 0 min (b) 200°C and 0 min. 57
Fig. 4.9. TEM micrographs of Ni(OH)₂ nanocrystals fabricate by hydrothermal process at 200°C (a) not HTHP reaction (b)for 1 h (c )for 10 h (d)for 24 h. 58
Fig. 4.10. Graph showing relationship between reaction time and diameter of Ni(OH)₂ nanodisks. The bar is standard deviation. 59
Fig. 4.11. TEM micrographs of Ni(OH)₂ nanocrystals fabricated by hydrothermal process at 150°C (a) not HTHP reaction (b) for 0 min (c) for 60 min (d) for 600 min. 60
Fig. 4.12. TEM micrographs of Ni(OH)₂ nanocrystals fabricated by hydrothermal process at 150°C (a) for 0 min (b) for 60 min (c) for 600 min. 62
Fig. 4.13. TEM micrographs of Ni(OH)₂ nanocrystals fabricated by hydrothermal process at 200°C (a) for 60 min (b) for 600 min. 63
Fig. 4.14. TEM micrographs of Ni(OH)₂ nanocrystals fabricated by hydrothermal process at 200°C for 600 min. (a) pH 12 (b) pH 10 (c) pH 8. 65
Fig. 4.15. Relative percentage of Ni(OH)₂ nanocrystals differing by their shapes. 66
Fig. 4.16. TEM micrograph of Ni(OH)₂ nanocrystals fabricated by hydrothermal process at 200°C for 60 min and pH 8. (a) 0.1M HCI solution (b) 0.1M HNO₃solution. 68
Fig. 4.17. TEM micrograph of growth direction of Ni(OH)₂ nanocrystals. (b) HRTEM of dotted line in (a) : radial direction. 69
Fig. 4.18. TEM micrograph of growth direction of Ni(OH)₂ nanocrystals.(b) HRTEM of doted line in (a) : Axis direction. 70
Fig. 4.19. TEM micrograph of Ni(OH)₂ nanocrystals fabricated by hydrothermal process at 200°C for 60 min using different surfactant (a) SDS (b) AOT. 72
Fig. 4.20. TEM micrograph of Ni(OH)₂ nanocrystals fabricated by hydrothermal process at 200°C for 60 min and pH 8 (1M H₂SO₄solution). 74
Fig. 4.21. XRD pattern comparison of Ni(OH)₂ fabricated by hydrothermal process at 200°C for 60 min and pH 8, (HCI and H₂S0₄used pH control acid type). 75
Fig. 4.22. Scheme of changing from hexagonal structure to monoclinic structure (a) hexagonal structure (b) monoclinic structure. 76
Fig. 4.23. FT-IR spectra of Ni(OH)₂and Ni(SO₄)o.₃(OH)₁.₄ . 78
Fig. 4.24. HR-TEM micrograph of growth direction of Ni(SO₄)o.₃(OH)₁.₄. 79
Fig. 4.25. (a) DSC curve of Ni(SO₄)o.₃(OH)₁.₄after heat treatment. 81
Fig. 4.25. (b) TGA curve of Ni(SO₄)o.₃(OH)₁.₄after heat treatment. (c) DTG curve of Ni(SO₄)o.₃(OH)₁.₄after heat treatment. 82
Fig. 4.26. FT-IR spectra of Ni(SO₄)o.₃(OH)₁.₄after heat treatment. 83
Fig. 4.27. XRD pattern comparison of Ni(SO₄)o.₃(OH)₁.₄after heat treatment. 84
Fig. 4.28. TEM microgaph of Ni(SO₄)o.₃(OH)₁.₄after heat treatment (a) after heat treatment at 250°C for 2h. (b) after heat treatment at 500°C for 2h. 85
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