표제지
목차
I. 서론 10
II. SiCl₄ 증류 정제 15
1. 이론적 고찰 16
1) 금속염화물의 증기압 데이터 16
2. 실험 21
1) 실험 장치 21
2) 시료 주입 방법 24
3) 실험 방법 26
4) 분석 방법 28
3. 결과 및 고찰 29
1) 시운전 29
2) 1 단계 증류 31
3) 2 단계 증류 33
III. SiC derived Carbon의 기공크기 조절 35
1. 이론적 고찰 36
1) 열역학적 고찰 36
2. 실험 38
1) SiC derived carbon (SiC-CDC)의 제조 38
2) 실험 장치 39
3) 실험 방법 42
4) 분석 방법 43
3. 결과 및 고찰 44
1) SiC derived carbon (SiC-CDC)의 특성분석 44
(1) SEM-ED× 분석 44
(2) TG 분석 46
(3) 비표면적 분석 46
(4) TEM 분석 48
2) 온도에 따른 전환율 변화 49
3) 전환율에 따른 비표면적 변화 51
4) 반응 시간에 따른 기공 크기 변화 53
IV. SiC derived carbon의 활용 56
1. 촉매의 지지체 57
1) CVI에 의한 Fe/C 촉매 제조 58
(1) 실험 장치 및 방법 58
(2) 분석 방법 61
(3) 촉매의 특성 평가 62
2) Incipient Wetness 법에 의한 Fe/C 제조 70
(1) Incipient Wetness (IW) 법 이용한 촉매 제조 70
(2) 촉매의 특성분석 및 비교 71
2. 수소 흡착 77
1) 실험 장치 및 방법 78
2) 실험 결과 80
V. 결론 82
VI. Reference 84
ABSTRACT 88
Appendix 90
Table 1. Chemical analysis of Si-SiC sludge 14
Table 2. Chemical analysis of crude SiCl₄ 17
Table 3. Relationship between metal chloride vapor pressure and temperature 18
Table 4. Chemical analysis of impurity content in SiCl₄ before and after 1st distillation 32
Table 5. Chemical analysis of impurity content in SiCl₄ before and after 2nd distillation 34
Table 6. SEM EDX analysis of SiC derived carbon 45
Table 7. Specific surface area of before and after Iron loading 63
Table 8. Iron content of Fe/C catalyst 67
Figure 1. Schematic of drawing of Si-SiC chlorination. 14
Figure 2. Relationship between metal chloride vapor pressure and temperature. 19
Figure 3. Flowsheet for SiCl₄ purification by distillation. 20
Figure 4. Schematic drawing of distillation of SiCl₄. 22
Figure 5. Photograph of SiCl₄ distillation apparatus. 23
Figure 6. Photograph of packing (borosilicate 3×3 ㎜ glass raschig ring) used for SiCl₄ distillation. 23
Figure 7. Schematic drawing of SiCl₄ feeding to the flask at the bottom of the distillation column. 25
Figure 8. Detailed drawing of the cap of the SiCl₄ bottle in Figure 7. 25
Figure 9. Computer simulated effect of reflux ratio on concentration of Ti in the distillate. (ppm=㎎-Ti/㎏-distillate) 30
Figure 10. Experimental effect of reflux ratio on concentration of Ti in the distillate. (ppm=㎎-Ti/㎏-distillate) 30
Figure 11. Relationship between temperature and equilibrium constant for varying reaction. 37
Figure 12. Schematic drawing of gasification of SiC-CDC with H₂O. 40
Figure 13. Photograph of gasification of SiC-CDC with H₂O. 41
Figure 14. (a) SEM image, EDX spectrum (b) before and (c) after H₂ annealing (4 h) of SiC derived carbon. 45
Figure 15. TG analysis of SiC derived carbon. 47
Figure 16. Pore size distribution of SiC derived carbon using NLDFT method. 47
Figure 17. TEM image of SiC derived carbon. 48
Figure 18. Variation of conversion with reaction time for activation of SiC derived carbon with H₂O vapor. 50
Figure 19. Variation of specific surface area with conversion for activation of SiC derived carbon with H₂O vapor. 52
Figure 20. Temporal evolution of pore volume with varying gasification temperature 54
Figure 21. Variation pore size distribution with gasification at 900 ℃. 55
Figure 22. Schematic drawing of the batch reactor for loading with iron. 59
Figure 23. Photograph of the batch reactor for loading with iron. 60
Figure 24. TEM image (a)SiC derived carbon and (b) SiC derived carbon loading with iron. 65
Figure 25. Comparison of H₂-TPR profile between raw carbon and activated carbon as support for iron loading. 69
Figure 26. TEM image of (a)raw carbon, (b) and (d)Fe/C catalyst via CVI method, and (c) and (e)Fe/C catalyst via IW method. 72
Figure 27. XRD patterns of raw carbon and Fe/C catalysts via CVI and IW method. 74
Figure 28. Comparison of H₂-TPR profiles between CVI and IW method for two carbon source 76
Figure 29. Photograph of MSB (Magnetic Suspension Balance) device for measuring H₂ uptake. 79
Figure 30. Hydrogen adsorption and desorption of (a) SiC-CDC and (b) Fe/C catalysts. 81