以鋅(II)與鉻(III)離子定量及轉化氧化鐵電極之表面態

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研究生：	林晟 Lin, Cheng
論文名稱：	以鋅(II)與鉻(III)離子定量及轉化氧化鐵電極之表面態 Quantification and Conversion of Surface States of Hematite Electrodes Using Zn(II) and Cr(III)
指導教授：	王竹方 Wang, Chu-Fang
口試委員:	談駿嵩 Tan, Chung-Sung 黃志彬 Huang, Chih-Pin 蔣本基 Chiang, Pen-Chi
學位類別：	碩士 Master
系所名稱：	原子科學院 - 生醫工程與環境科學系 Department of Biomedical Engineering and Environmental Sciences
論文出版年：	2017
畢業學年度：	105
語文別：	英文
論文頁數：	80
中文關鍵詞：	赤鐵礦、光化學反應、表面態、定量、鈍化
外文關鍵詞：	hematite, PEC, surface state, quantification, passivation
相關次數：	點閱：4 下載：0
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隨著人類社會對能源的需求增加，永續性能源的發展極為迫切。使用光化學反應產生氫油是其中一個具有前景的方法，而氧化鐵正是作為光化學反應電池中光陽極的合適材料。不過，由於氧化鐵上的表面態所導致的低效率，造成普及應用發展上的瓶頸。更進一步，由於缺乏表面態與光化學表現的量化關係，更成為近一步發展的阻礙。在這項研究中，我們將痕量的鋅(II)和鉻(III)分別加入溶液中進行電化學實驗的測量，並同時利用感應耦合電漿質譜儀測量金屬離子在氧化鐵電極表面覆蓋率。結果顯示無論是鉻(III)或是鋅(II)都在0.1 %覆蓋率時擁有最小的起始電壓0.88 VRHE。我們也將鋅(II)覆蓋之氧化鐵電極藉由120 oC燒結兩小時，轉化為催化劑，並且觀察到了顯著提升的光電流與下降的起始電壓。Fe(III)和Ni(II)也經過同樣的處理，並且也觀察到較好的光化學反應效果。對於氧化鐵表面態的定量之研究將會是我們將來發展選擇性結合單分子催化劑在氧化鐵電極上的墊腳石。

As the demand for energy rises, the need for sustainable green energy is in urgent. Utilizing photoelectrochemical reaction (PEC) to produce hydrogen fuel is a promising way to the future, and α-Fe2O3 is a suitable candidate for the photoanode of PEC cells. However, the low efficiency due to surface states of hematite electrode has long been a bottleneck in development. Furthermore, the lack of quantified relation between surface states and its photochemical behavior set a barrier for improvement. In this study, trace amount of Zn(II) and Cr(III) ions were added respectively in the solution then several electrochemical measurements as well as the coverage on hematite surface by ICP-MS were conducted. The results suggested a minimal onset potential 0.88 VRHE when coverage was about 0.1 % regardless of whether Cr(III) or Zn(II) was used as ion probes. We also transformed Zn(II) ion probes to catalysis after annealed at 120 oC for 2h. It is observed that the photocurrent and onset potential improved significantly. Fe(III) and Ni(II) also undergo the same procedure, it is noted that the Fe(III) and Ni(II) also behave well after annealing. The quantification of surface states sets a stepping stone for selectively associating molecular catalysts, which is the target in our ongoing study.

Index
Chapter 1    Introduction    1
Chapter 2    Literature Review    4
2.1    Photoelectrochemical Cells    5
2.1.1    Brief Introduction of Photoelectrochemical Cells    5
2.1.2     Water Splitting Reaction    7
2.2    Hematite as Photoanodes    12
2.2.1    Properties of Hematite    12
2.2.2    The Development of Hematite as Photocatalysts    14
2.3    The Barriers of Hematite Electrodes in PEC Reaction    17
2.3.1    The Water Splitting Process of Hematite    17
2.3.2    Charge Separation and Hole Collection    19
2.3.3    Water Oxidation Kinetics    20
Chapter 3    Experimental Section    23
3.1    Chemical Reagents    23
3.2    Experimental Instruments    24
3.2.1    Inductively Coupled Plasma-Mass Spectroscopy (ICP-MS)    24
3.2.2    Electrochemical Workstation    26
3.2.3    X-ray Photoelectron Spectroscopy (XPS)    27
3.3    Details of Preparations and Experimental Methods    29
3.3.1    Preparation of α-Fe2O3 photoelectrodes    29
3.3.2    Electrochemical Measurements    29
3.3.3    Characterization of Electrodes    31
Chapter 4    Results and Discussion    32
4.1    Quantification of Surface States    32
4.2    Electrochemical Behaviors of Ion-Probed Hematite    44
4.3    Conversion of Surface States of Hematite to Highly Catalytic Sites    54
Chapter 5    Conclusions and Future Works    69
5.1    Conclusions    69
5.2    Future Works    70
Reference    71
Appendix    78

 
Figure Index

Figure 1 1    Flow chart of experimental scheme    3
Figure 2 1 The basic schemes of the photoelectrochemical cells. a, Regenerative-type cell which produce electricity; b, a cell that generates a chemical fuel and hydrogen.    5
Figure 2 2 At pH 0, the energy states and band gaps of several popular metal oxide semiconductor used in Photocatalytic cells.    7
Figure 2 3 Solar energy spectrum (AM of 1.5) from earth’s surface.    7
Figure 2 4 The overall energy diagrams of photocatalytic water splitting (a) one-step excitation and (b) two-step excitation ; and the photoelectrochemical reaction using (c) a photoanode, (d) photocathode, and (e) photoanode and photocathode in tandem configuration.    10
Figure 2 5 The crystal structure of hematite. (a) The rhombohedral primitive cell. (b) The hexagonal cell, the oxygen atom is indicated as red; the gray one is iron.    13
Figure 2 6 SEM images of different morphology of the nanostructured hematite using in water splitting reaction.    16
Figure 2 7 The process of charge and energy transfer if hematite. The recombination pathways are represented in dotted red arrow.    17
Figure 2 8 The scheme of charge transfer process by hematite/reduced-graphene oxide composite.    19
Figure 3 1    An image of Agilent 7500a ICP-MS.    26
Figure 3 2 The instrument diagram of ICP-MS    26
Figure 3 3 Block diagram of the electrochemical analyzer    27
Figure 3 4 Simplified mechanism of XPS    28
Figure 4 1 Representative linear sweep voltammetry of hematite electrodes with different amount of surface coverage by either (a) Cr(III) or (b) Zn(II) measuring at the chopping mode.    32
Figure 4 2 Determined (a) photocurrent onset potential (VRHE) and (b) photocurrent density of hematite electrodes in 10 mM NaHCO3 (pH 8.2) solutions as a function of surface coverage.    36
Figure 4 3 The mechanism of the metal ions binding on the active sites of hematite surface, a)Lewis and b)Bronstedt acid coordination[60].    41
Figure 4 4 Representative cyclic voltammetry of hematite electrodes with different amount of surface coverage by Zn(II) at scan rate 600 mV/s.    44
Figure 4 5 Representative cyclic voltammetry of hematite electrodes with different amount of surface coverage at 100 mV/s by either (a) Cr(III) or (b) Zn(II).    46
Figure 4 6 The chop mode experiment which applied constant potential VRHE=1.3 on different coverage of Zn2+ and Cr3+ ions on hematite electrodes.    48
Figure 4 7 Tafel plots which are selected from representative measurements of hematite electrodes with different amount of surface coverage by either (a) Cr(III) or (b) Zn(II)    50
Figure 4 8 The photocurrent at VRHE=1.1 V and the changing of the onset potential. Control is pure hematite; the red bar is hematite electrode with Zn2+ coverage about 0.09% and the green bar is hematite electrode with Zn2+ coverage about 0.09% after annealing.    54
Figure 4 9 The XPS analysis of the Zn(II) passivated hematite(red) and annealed hematite(blue).    57
Figure 4 10 Tafel plots which are selected from representative measurements of pure hematite, Zn(II) covered 0.09 % hematite and Zn(II) covered hematite after annealing.    59
Figure 4 11 Representative linear sweep voltammetry of hematite electrodes with pure hematite (black), Zn2+ with coverage 0.09 % (red) and Zn2+ with coverage 0.09 % after annealing (blue) measuring at the chopping mode respectively.    61
Figure 4 12 Representative cyclic voltammetry of hematite electrodes with Zn(II) before and after annealing at scan rate 100 mV/s.    63
Figure 4 13 The photocurrent at VRHE=1.1 V and the changing of the onset potential. Control is pure hematite; the red bar is hematite electrode with 10 µM Ni2+ and the green bar is hematite electrode with 10 µM Ni2+ after annealing.    64
Figure 4 14 The photocurrent at VRHE=1.1 V and the changing of the onset potential. Control is pure hematite; the red bar is hematite electrode with 10 µM Fe3+ and the green bar is hematite electrode with 10 µM Fe3+ after annealing.    67
Figure A 0 1 Titration of Surface Active Sites    78
Figure A 0 2 Open circuit plot of Zn(II) ion probed hematite    78
Figure A 0 3 Open circuit plot of Cr(III) ion probed hematite    79
Figure A 0 4 Open circuit plot of pure and annealed hematite    79
Figure A 5 Full tafel plot of Zn(II) ion probed hematite    80
Figure A 6 Full tafel plot of Cr(III) ion probed hematite    80


                                

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