工業廢料級AZ61鎂合金的儲氫性能：製造和表徵｜國立臺灣科技大學博碩士論文系統

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研究生：	Matoke Peter Mose Matoke Peter Mose
論文名稱：	工業廢料級AZ61鎂合金的儲氫性能：製造和表徵 Hydrogen storage properties of industrial waste grade AZ61 Magnesium alloy: Fabrication and Characterization
指導教授：	黃崧任 Song-Jeng Huang
口試委員:	黃崧任 Song-Jeng Huang 丘群 Chun Chiu 王丞浩 Chen-Hao Wang 曾有志 Yu-Chih Tzeng 林景崎 Jing-Chie Lin 汪俊延 Jun-Yen Uan 李天錫 Tien-Hsi Lee
學位類別：	博士 Doctor
系所名稱：	工程學院 - 機械工程系 Department of Mechanical Engineering
論文出版年：	2023
畢業學年度：	111
語文別：	英文
論文頁數：	118
外文關鍵詞：	Magnesium, Hydrogen storage, High-energy ball milling, Catalyst
相關次數：	點閱：287 下載：0
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ABSTRACT    I
概要    III
ACKNOWLEDGEMENT    IV
TABLE OF CONTENTS    V
LIST OF FIGURES    VII
LIST OF TABLES    IX
1    Introduction    1
1.1    Background    1
1.2    Green Energy Production Worldwide: Trends and Forecast    3
1.3    Current Status and Future Trends in Solid-State Hydrogen Storage    8
1.4    Evolution of hydrogen storage    10
1.5    Market outlook for solid-state hydrogen    12
1.6    Research targets    15
1.7    Outline and Scope of the research    16
1.7.1    The scope of this research    16
1.7.2    Thesis outline    16
2    Literature Review    18
2.1    Introduction    18
2.2    Overview of Mg-based solid-state hydrogen storage    20
2.3    Tailoring Mg-based hydrogen storage performance    23
2.3.1    Compositional design    24
2.3.2    Nanoconfinement    26
2.3.3    Amorphization    26
2.3.4    Additive with catalytic effect    26
2.3.5    Advanced synthesis methods    27
2.4    Conclusion    30
3    Methodology    31
3.1    Material selection    31
3.2    Design of Experiment (DOE) with Taguchi method-Ball milling optimization    33
3.3    Composite synthesis    34
3.4    Casting and ECAP process    35
3.5    Characterization    38
3.5.1    Microstructure characterization.    38
3.5.2    Powder morphology    38
3.5.3    Phase composition and crystal structure    39
3.5.4    Particle size analysis    40
3.5.5    Chemical state of elements    40
3.5.6    Hydrogen storage properties.    40
3.5.7    Differential Scanning Calorimetry (DSC) and thermogravimetric analysis (TGA)    41
4    Results    43
4.1    Particle size analysis    43
4.2    Powder morphology    47
4.3    Energy dispersive spectroscopy (EDS) analysis    49
4.4    Phase and crystal structure analysis    52
4.5    Chemical bonding analysis    59
4.6    Specific surface area analysis    62
4.7    Hydrogen storage properties    65
4.7.1    Absorption-desorption kinetics    65
4.7.2    Reaction Kinetics    69
4.7.3    Desorption activation energy    72
4.7.4    Cycle stability    74
4.8    Effect of ECAP on Hydrogen properties    74
4.8.1    Microstructure analysis    74
4.8.2    Hydrogen absorption    79
4.8.3    Thermogravimetric analysis    80
5    Discussion of results    82
5.1    Particle size analysis    82
5.2    Specific surface area    82
5.3    Powder morphology and the effect of HEBM    82
5.4    Hydrogen properties    83
5.5    Reaction mechanism    84
5.6    Reaction kinetics    86
5.6.1    Reaction kinetics of AZ61 alloy    86
5.6.2    Reaction kinetics after use of catalyst    87
5.7    Kinetics of hydrogen desorption    88
5.8    Effect of Co, Ni and Ni-Co additives on hydrogen storage properties    89
5.9    Effect of ECAP+HEBM on hydrogen storage    91
6    Technology Comparisons with related literatures    93
7    Conclusion and future work    94
7.1    Conclusions    94
7.2    Future work    96
List of Publications    96
References    98
APPENDIX    109

LIST OF FIGURES
Figure 1. Feedstocks, routes and primary sources of hydrogen production [23]    7
Figure 2. The evolution of hydrogen storage    11
Figure 3. Methods available for storing hydrogen [43]    19
Figure 4. hydrogen-metal interactions during absorption-desorption process [47].    21
Figure 5. Diagram illustrating the impact of Mg particle size on the absorption kinetics of Mg-based materials for hydrogen storage [40].    23
Figure 6. Techniques used to enhance hydrogen storage properties.    23
Figure 7. Schematics of the casting equipment    36
Figure 8. Processing ECAP billet to ball milling    38
Figure 9: Brucker D2 Phaser instrument    39
Figure 10. X-ray Photoelectron Spectroscopy (XPS): ULVAC-PHI. Inc. / PHI 5000 VersaProbe Ⅲ    40
Figure 11. Sievert-type hydrogen measurement system.    41
Figure 12. Mettler Toledo-DSC calorimeter    42
Figure 13. Experimental Flowchart    42
Figure 14. Particle size statistics    43
Figure 15. Sample 3; Particle size and crystallite size analyses.    44
Figure 16. Powder Morphology for various samples: (a) as-received, (b) Sample 1, (c) Sample 2, and (d) Sample 3.    47
Figure 17. Powder Morphology for various samples: (a) Sample 5, (b) Sample 6, (c) Sample 7, and (d) Sample 8.    48
Figure 18. SEM images of as-received powders of: (a) AZ61 alloy, (b) Ni powder, and (c) Co powder (d) AZ61+2wt.%Ni, (e) AZ61+2wt.%Co, and (f) AZ61+2wt.%Co-Ni    49
Figure 19. Figure 18. EDS for Co-Ni mixture (point spectrum)    49
Figure 20. EDS for Co-Ni mixture (sum spectrum)    50
Figure 21. EDS Scan for Pure AZ61 powder    50
Figure 22. EDS Scan of AZ61+2wt.% Co    50
Figure 23. EDS elemental mapping of Mg, Al, Zn and Co in AZ61+2wt.%Co sample    51
Figure 24. EDS Scan for AZ61+2wt.%Ni    51
Figure 25. EDS elemental mapping of Mg, Al, Zn and Ni in AZ61+2wt.%Ni sample    51
Figure 26. EDS Scan for AZ61+2wt.%Co-Ni    52
Figure 27. EDS elemental mapping of Mg, Al, Zn, Co, and Ni in AZ61+2wt.%C0-Ni sample    52
Figure 28. XRD patterns peak broadening for as-received and samples no. 1-9.    53
Figure 29. XRD patterns for samples 1-9.    55
Figure 30. XRD patterns for sample 2 before and after hydrogenation    56
Figure 31. XRD pattern for sample 3 before and after hydrogenation    57
Figure 32. XRD patterns for sample 6 before and after hydrogenation    57
Figure 33. XRD patterns for (a) Ball-milled Ni-Co mixture, (b) Ni and (c) AZ61 alloy, (d) Co powder    58
Figure 34. XRD patterns (a) before and (b) after absorption    59
Figure 35. XPS analysis of Co 2p and Ni 2p before milling (a, c) and after milling (b, d)    60
Figure 36. C 1s high resolution spectra    60
Figure 37. XPS analysis of Mg 2p and O 1s before milling (a, b) and after milling (c, d)    61
Figure 38. Adsorption-desorption curves and BET-plot for Sample 1    63
Figure 39. Adsorption-desorption curves and BET-plot for sample 2    63
Figure 40. Adsorption-desorption curves and BET-plot for sample 3    64
Figure 41. Adsorption-desorption curves and BET-plot for sample 4    64
Figure 42. Adsorption-desorption curves and BET-plot for sample 6    65
Figure 43. Average absorption kinetic curves for samples 2, 3, 6 & 8    66
Figure 44. Desorption kinetic curves for samples 2, 3, 6 & 8.    67
Figure 45. Absorption-desorption kinetic curves for AZ61+2wt%Ni sample.    68
Figure 46. Absorption-desorption kinetic curves for AZ61+2wt%Co sample    68
Figure 47. Absorption-desorption kinetic curves for AZ61+2wt%. Co-Ni sample    69
Figure 48. Combined Ab/desorption kinetic curves for different catalysts    69
Figure 49. Avrami plots for sample 2, 3, 6 and 8    70
Figure 50. JMAK linear plots (a) Sample 2, (b) sample 3, (c) sample 6, and (d) sample 8    71
Figure 51. JMAK plots for sample with (a) Co, (b) Ni, (c) Ni-Co mixture and (d) Combined Avrami plots.    71
Figure 52. a) DSC scan and (b) Kissinger Plot for pure AZ61 alloy after absorption (Sample 6)    72
Figure 53. (a) DSC Scan and (b) Kissinger plot for AZ61+2wt.% Co    73
Figure 54. DSC curve before (black) and after (blue) absorption for Sample 6: heating rate-5 C°/min    73
Figure 55. Cycle Stability plots    74
Figure 56. Optical image of AZ61 as-cast condition (Magnification, 20X)    75
Figure 57. Optical image of AZ61 as-cast condition (Magnification, 50X)    75
Figure 58. Optical image of ECAP sample-2passes (Magnification, 20X)    76
Figure 59. Optical image of ECAP sample-2passes (Magnification, 50X)    76
Figure 60. Optical image of ECAP sample-3passes (Magnification, 20X)    77
Figure 61. Optical image of ECAP sample-3passes (Magnification, 50X)    77
Figure 62. Grain Size Distribution – As-cast condition    78
Figure 63. Grain Size Distribution - Homogenized condition    79
Figure 64. Grain Size Distribution-ECAP 2 passes    79
Figure 65. Comparison of the H2 absorption after HEBM, ECAP+HEBM and As-cast    80
Figure 66. DSC and TGA graphs for AZ61+2wt.%Ni HEBM    80
Figure 67. DSC/TGA curves for AZ61+2wt.%Ni-HEBM+ECAP (4pass)    81


LIST OF TABLES
Table 1. Chemical composition of AZ61 magnesium    32
Table 2. Experimental Parameters    34
Table 3. Crystallite Size (Å) at different conditions    46
Table 4. ANOVA Table of results    46
Table 5. Crystallite Size Variation, micro-strain and crystallinity    53
Table 6. Comparison of observed and theoretical values of 2θ (°) for AZ61-Mg (as received) and Pure Mg respectively.    54
Table 7. Crystal structure data for the identified phases after milling    55
Table 8. Specific surface area    62
Table 9. Comparison table for the ab/desorption kinetics    66
Table 10. Comparison of hydrogen storage performance of Mg-Al alloys    93
                                

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