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Enhancement of Photocatalytic Activity by Site Poisoning

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Enhancement of Photocatalytic Activity by Site Poisoning ENHANCEMENT OF PHOTOCATALYTIC ACTIVITY BY SITE POISONING PLATINUM DOPED TITANIUM DIOXIDE A Thesis Presented to The Graduate Faculty of The University of Akron In Partial Fulfillment of the Requirements for the Degree Master of Science Yang Chu December, 2014 ENHANCEMENT OF PHOTOCATALYTIC ACTIVITY BY SITE POISONING PLATINUM DOPED TITANIUM DIOXIDE Yang Chu Thesis Approved: Accepted: _________________________________ _________________________________ Advisor Dean of the College Dr. Steven S.C. Chuang Dr. Eric J. Amis _________________________________ _________________________________ Faculty Reader Interim Dean of the Graduate School Dr. Xiong Gong Dr. Rex Ramsier _________________________________ _________________________________ Department Chair Date Dr. Coleen Pugh ii ABSTRACT Photoelectrochemical cell (PEC) is a device that could interconvert chemicals and electricity with the energy of light by the photovoltaic effect1. PEC is widely studied recently for hydrogen production and waste organics degradation2. The main structure is composed of photocatalyst, electrolyte, counter electrode and power supply. Water and organics are converted to hydrogen and carbon dioxide gases by irradiating the photocatalyst with ultraviolet radiation. The challenge for commercialization is mainly because of the low efficiency. Extensive research has been directed toward developing highly active photocatalysts by the doping of platinum. Platinum doped titanium dioxide 3, 4 (Pt-TiO2) has shown the ability to faster degrade organics than TiO2 . The mechanism is that the low potential of platinum that functions as a trap for the electrons and thus reduces the electron-hole recombination. However, there has not been a significant breakthrough that can lead PEC to commercialization. Recently, we hypothesize that selectively poisoning the electron generating site could significantly reduce the electron- hole recombination. Pt-TiO2 was treated with hydrogen sulfur (Pt-TiO2/H2S) at high temperature and H2S were converted to sulfur and completely covered the platinum. Characterization of TiO2, Pt-TiO2 and Pt-TiO2/H2S both in powder and thin film format was done by infrared spectroscopy (IR), ultraviolet-visible spectroscopy (UV-vis), x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy-dispersive X-ray spectroscopy (EDS). Ethanol and some other organics are added in electrolyte to increase the current density of the PEC and iii produce more hydrogen due to the lower oxidation potential than water5. Comparing the working electrode of TiO2, Pt-TiO2 and Pt-TiO2/H2S in PEC, we analyzed the different amount of gaseous products, the current density and the degradation of methylene blue. The results showed that Pt-TiO2/H2S has the best oxidative activity per unit thickness of catalyst. This research will lead us to find the applications of PEC in utilization of the shale gas that can provide the energy with high efficiency and environmental friendly in the future. iv ACKNOWLEDGEMENTS Firstly, I will thank my advisor, Dr. Steven Chuang for giving me this opportunity to do research in his group. He provided me this project and taught me how to think for the science and technology. I really appreciate Dr. Xiong Gong to be the reader for my master thesis. He is so busy but he still squeezes his time to help me improve my writing skill. I would like to thank the group members of the photocatalyst, who are Mehdi Lohrasbi, Piyapong Pattanapanishsawat, Dan Huang, Jie Yu. They taught me how to set up the experiment and the way to analyze the data. They are friends more than the colleagues. Secondly, I am very grateful for my parents. They give me all their love and understand to support me to finish my Master degree. They are always the strongest backup whatever I meet all the problems. I also need to thank all my friends. They helped me overcome the hardest time in USA and always encourage me to do my favorite things. Last, I am thankful to my wise, Yu Zhang. She did everything she could to help me finish my Master degree. She is the most important people to me and she will always be. v TABLE OF CONTENTS Page LIST OF FIGURES ......................................................................................................... viii LIST OF TALBES ........................................................................................................... xiii CHAPTER I. INTRODUCTION ........................................................................................................... 1 II. LITERATURE REVIEW ............................................................................................... 4 2.1. Photocatalysts .......................................................................................................... 4 2.2. Titanium dioxide ...................................................................................................... 4 2.3. Photoelectrochemical cell ........................................................................................ 7 III. EXPERIMENTAL ...................................................................................................... 12 3.1. Preparation and characterization of platinum doped titanium dioxide and platinum ....................................................................................................................................... 12 3.1.1. Preparation of platinum doped titanium dioxide ............................................ 12 3.1.2. Preparation of platinum doped titanium dioxide treated by hydrogen sulfide 13 3.1.3. Preparation of TiO2 thin film, Pt-TiO2 thin film and Pt-TiO2/H2S thin film ... 14 3.1.4 Characterization of catalysts in forms of powder and thin film ....................... 16 3.2. Setup of photoelectrochemical cell ........................................................................ 17 3.3. Characterization of gas products and solution in photoelectrochemical cell ......... 19 3.4. Experimental procedure of photoelectrochemical cell .......................................... 19 IV. RESULTS AND DISCUSSION .................................................................................. 22 4.1. Characterization of TiO2-based catalysts ............................................................... 22 4.1.1 TiO2-based catalysts in powder and thin film form ......................................... 22 vi 4.1.2 TEM analysis of TiO2-based catalyst in powder form ..................................... 23 4.1.3 SEM analysis of TiO2-based catalysts in thin film form.................................. 25 4.1.4 FTIR spectroscopy characterization of TiO2-based catalysts .......................... 25 4.1.5 UV-Vis spectroscopy characterization of TiO2-based catalysts ....................... 30 4.1.6 Two-dimensional wide angle X-ray diffraction spectroscopy of TiO2-based catalysts. .................................................................................................................... 32 4.1.7 Energy-dispersive X-ray spectroscopy of TiO2-based catalysts ...................... 33 4.2. Results of photoelectrochemical cell ..................................................................... 33 4.2.1 Photoelectrochemical reactions ....................................................................... 33 4.2.2 Electrical experimental results of photoelectrochemical cell .......................... 34 4.2.3 Gas production results of photoelectrochemical cell experiment. ................... 37 4.2.4 Photo oxidation of methylene blue in the photoelectrochemical cell experiment ................................................................................................................................... 39 4.2.5 pH change ........................................................................................................ 42 4.3. Conclusions ............................................................................................................ 45 REFERENCES ................................................................................................................. 46 APPENDICES .................................................................................................................. 51 APPENDIX A DYE-SENSITIZED SOLAR CELLS (DSSC) ..................................... 52 APPENDIX B INTENSITY OF UV LIGHT................................................................ 72 APPENDIX C PHOTO DEGRDATION OF PVC THIN FILMS ................................ 80 APPENDIX D NFPA AND HMIS RATING OF CHEMICALS ................................ 104 vii LIST OF FIGURES Figure Page 1. Organization of master project and thesis ....................................................................... 3 2. Band positions of several semiconductors in contact with aqueous electrolyte at pH 1. 5 3. Ball and stick model for three different forms of titanium dioxide. ............................... 6 4. (a) Chemical structure of methylene blue and the IR band assignment. (b) Variations of the IR intensity of MB bands at 1488 cm-1 during 240 min of the MB photocatalytic degradation. ................................................................................................................... 7 5. Current-voltage profile of the photoelectrochemical cell.. ............................................. 8 6. Experimental procedure of Pt-TiO2 preparation ........................................................... 13 7. Experimental procedure of Pt-TiO2/H2S preparation ...................................................
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