표제지
목차
국문 요약 9
제1장 서론 15
제2장 이론적 배경 22
2.1. 타이타늄 Titanium 22
2.1.1. Titanium 22
2.1.2. 타이타늄 산업 및 응용 합금 26
2.2. 금속열환원에 의한 타이타늄 산화/환원 열역학 28
2.2.1. Ellingham Diagram 28
2.2.2. Ti의 산소 친화력 31
2.3. Electrochemistry of Metal 34
2.3.1. 용융염 전해정련 34
2.3.2. 전기화학 반응 35
2.3.3. 물질 전달 프로세스 39
2.3.4. Faraday's Law 43
2.3.5. Cyclic Voltammetry (CV) 45
2.3.6. 분극 거동 48
2.3.7. 정전류법 Chronopotentiometry (CP) 48
2.4. Titan ium Manufacturing Process 49
2.4.1. Hunter Process 50
2.4.2. Kroll Process 51
2.4.3. TiO₂ 활용 타이타늄 신 제련 공정 현황 53
제3장 연구 방법 61
3.1. 금속 열환원 기반 Ti-Cu 조금속 제조 방법 61
3.1.1. 원료 61
3.1.2. Ti -Cu 제조를 위한 도가니 선정 및 조건 62
3.2. Ti-Cu 조금속으로부터 Ti 전해 추출 방법 65
3.2.1. 원료 65
3.2.2. CV, CP 분석 위한 전해 추출 셀 구성 67
제4장 연구 결과 및 고찰 70
4.1. 도가니 소재에 따른 Ti-Cu 조금속 제조 분석 결과 70
4.1.1. 도가니 선택을 위한 열역학 계산 70
4.1.2. Ti 도가니 금속 열환원 결과 및 분석 72
4.1.3. Mo, W 도가니 금속 열환원 결과 및 분석 77
4.1.4. 공정 시간에 따른 Ti-Cu 추출 결과 및 분석 87
4.2. Ti-Cu 조금속에서 Ti 용융염 전해 추출 분석 결과 92
4.2.1. 전해질 선정 위한 TG-DTA, CV 결과 92
4.2.2. 분극 거동 및 전해추출 위한 정전류법(CP) 분석 96
4.2.3. 전해추출 후 회수된 타이타늄 및 Ti-Cu 조금속 분석 98
제5장 결론 101
Reference 104
Abstract 111
Table 2.1. Components of commercial pure titanium (CP-Ti) and Ti metal grades 1 to 5. 27
Table 3.1. Fluoride-based molten salt CV, CP cell structure conditions 69
Fig 1.1. Oxidation potential diagram of TiO₂, TiO, MgO and CaO. 17
Fig 1.2. Cu, Ti redox potential section using standard reduction potential 20
Fig 1.3. Process flow chart of this study 21
Fig 2.1. The crystal structure of (a) α titanium of HCP and (b) β titanium of BCC. 24
Fig 2.2. Biocompatibility comparison graph based on polarization resistance by metal type. 25
Fig 2.3. Ellingham diagram. 30
Fig 2.4. Ellingham diagrams of some selected oxides and the solid solution of Ti-O. 33
Fig 2.5. Schematic of electrochemical cell. 37
Fig 2.6. General pathway of mass and charge transfer in electrode surface reaction. (1) Mass transfer, (2) Chemical reactions, (3) Electron transfer. 38
Fig 2.7. Cyclic voltammetry (CV) (a) triangular waveform, (b) typical cyclic voltammogram. 47
Fig 2.8. Flow chart of titanium manufacturing process (a) Hunter process, and (b) Kroll process. 52
Fig 2.9. Flow chart of the HAMR process for Ti or Ti hydride production. 55
Fig 2.10. Schematic diagram of the FFC-Cambridge process for the electrochemical reduction of Titanium oxide to Ti metal in... 56
Fig 2.11. Schematic diagram of the MER Corporation. 57
Fig 2.12. Schematic diagram of OS process. 60
Fig 3.1. Phase diagram of Cu-Ti 63
Fig 3.2. Schematic diagram of Ti - Cu metal production in CaCl₂ molten salt using TiO₂ 64
Fig 3.3. Schematic diagram of initator (BaTiF6) production[이미지참조] 66
Fig 3.4. Actual experimental equipment and configuration diagram for molten salt electrolytic refining: (a) Glove box equipment and... 68
Fig 4.1. Reaction result of raw materials and crucible materials according to temperature TiO₂ + 2Ca + Cu + 10 CaCl₂ + X... 71
Fig 4.2. Internal shape of Ti crucible after metallothermic reduction - Temperature: 1100 ℃, holding: 60 min 73
Fig 4.3. OM image of inside the Ti crucible after metallothermic reduction (a) Top view, (b) bottom view 73
Fig 4.4. XRD analysis result of reduced (upper part) material in Ti crucible after metallothermic reduction 75
Fig 4.5. SEM-EDS analysis of reduced (upper part) material in the Ti crucible with washing and drying after metallothermic reduction... 76
Fig 4.6. Internal shape of Mo, W crucible after metallothermic reduction - Temperature: 1100 ℃, holding: 90 min 78
Fig 4.7. OM image of inside the Mo, W crucible after metallothermic reduction 79
Fig 4.8. XRD analysis result of reduced material in Mo, W crucible after metallothermic reduction 82
Fig 4.9. SEM-EDS analysis of reduced material surface in the Mo crucible with washing and drying after metallothermic... 83
Fig 4.10. SEM -EDS image of reducing material in Mo crucible after metallothermic reduction of metal (a)... 84
Fig 4.11. SEM-EDS analysis of reduced material surface in the W crucible with washing and drying after metallothermic reduction... 85
Fig 4.12. SEM -EDS image of reducing material in W crucible after metallothermic reduction of metal (a) Cross-sectional... 86
Fig 4.13. XRD results of Ti-Cu Crude alloy extraction with a syringe in W Crucible according to metallothermic reduction time 88
Fig 4.14. SEM image of Ti-Cu metal extraction with a syringe in W Crucible according to metallothermic reduction time (a) 2 hour,... 89
Fig 4.15. (a) N/O and (b) ICP-OES component analysis result of Ti-Cu metal in W crucible according to metallothermic reduction time 91
Fig 4.16. TG-DTA analysis result of 61 LiF-39 NaF 94
Fig 4.17. LiF-NaF-a BaTiF6 CV analysis result for titanium electrorefining[이미지참조] 95
Fig 4.18. Results of (a), (b) polarization behavior of two electrodes and (c), (d) electrorefining by CP 97
Fig 4.19. SEM-EDS results of electrodeposited titanium on cathode after electrorefining 99
Fig 4.20. SEM-EDS result of Ti-Cu metal (anode material) after electrorefining 100