十八世紀工業革命以來，人類文明的發展相當倚重煤、石油、天然氣等化石能源。然而因其存量有限，在不久的將來化石能源或將耗盡。台灣本身化石能源主要仰賴進口，發展替代能源與降低化石燃料依賴，實是刻不容緩的課題。氫能源乃是取代化石能源的方案之一。氫能經濟以氫氣為能源載體，利用可重複性能源，如太陽能、風力、地熱等，將其轉化的電能具有零碳排放特性。因為質子交換膜燃料電池(PEMFC)具有高效率、低汙染等優異性能，未來有可能取代內燃機，做為車用動力的主要來源。然而因鉑(Pt)觸媒的成本居高不下與產量有限，如何降低用量、提高陰極活性、增加持久性，實為質子交換膜燃料電池商業化的課題與挑戰。
本論文研究亦以上述目標為前提，以原子層沉積(atomic layer deposition, ALD)技術製備高活性鉑觸媒與新穎奈米結構支撐材，取代傳統之溼式化學還原鉑觸媒與碳黑載體。本論文分為三部分，針對原子層沉積鉑觸媒製程、新穎支撐材合成、鉑沉積於不同材料表面的現象，進行研究。第一部分中，比較水平流場(horizontal-flow)與垂直強制流場(vertical force-flow)反應腔體，研究對鍍層基材與鍍覆量的影響。並利用垂直強制流場，提高鉑前驅物的使用效率、降低腐蝕性副產物對支撐材的氧化，並沉積3奈米鉑觸媒於導電氮氧化鈦(TiOxN1-x)奈米顆粒支撐材，其氧氣還原活性(ORR)優於濕式化學還原之鉑觸媒，且氧還原活性與持久性均優於商用材(E-tek)。第二部分利用水平流原子層沉積技術製備二氧化鈦(TiO2)鍍層於聚碸高分子中空多孔纖維，之後進行不同階段熱處理，移除聚碸高分子中空多孔纖維，並予以氮化處理，製備導電多孔氮氧化鈦及氮化鈦(TiN)奈米結構，研究結果顯示二氧化鈦金紅石相(rutile)含量越少及氮化溫度愈高，愈容易形成氮化鈦。並進一步以垂直強制流場鍍覆鉑奈米顆粒於多孔氮氧化鈦與氮化鈦奈米結構，其氧還原活性均高於商用材，尤其是以三十次循環製備出的3奈米鉑鍍覆在多孔氮氧化鈦上，其氧活化半電位(E1/2)達0.874 V。此外若對鍍覆二氧化鈦的聚碸中空多孔奈米纖維直接進行氮化處理，因沉積之二氧化鈦鍍層具有高緻密性，可抵擋高溫氮化時的型變，聚碸之中空多孔奈米纖維之形貌與交連結構(interconnected nanostructure)在氮化後均被保留，且隨不同氮化溫度而轉變成氮氧化鈦或氮化鈦，而聚碸則被碳化，而得到氮氧化鈦與碳、氮化鈦與碳之奈米分層結構，並仍維持中空多孔纖維形貌。若以氮氧化鈦與碳或氮化鈦與碳之複合材做為奈米鉑載體，其氧還原活性均優於以碳黑為載體之鉑觸媒與商用材。第三部分則先製備鎳奈米蜂巢結構(Ni nanohoneycomb structure)，在予以進行氬氣處理(400 oC)，以及利用水平流場比較在不同基材原子層沉積鉑的成長行為，研究基材表面特性對原子層沉積鉑鍍覆量的影響，發現熱處理後的鎳奈米蜂巢結構有較高的鉑鍍覆量與均一性。

Since the industrial revolution in the eighteenth century, the development of new technologies has relied heavily on fossil energies such as coal, petroleum, and natural gas. However, due to the limited reserves, fossil fuels may be exhausted in the near future. Hydrogen energy is one of the solutions to replace fossil energy. The hydrogen energy economy utilizes hydrogen as the energy carrier. By using renewable energy sources, e.g., solar energy, wind power, and geothermal energy, the conversion to electricity is a zero-carbon emission process. Because proton exchange membrane fuel cell (PEMFC) bears with high efficiency and low pollution, it is highly anticipated to replace the internal combustion engine as a power source for vehicles in the future. However, due to high cost and limited reserves of platinum (Pt), reducing the loading, improving the cathode activity, and increasing the durability are the challenges for the commercialization of PEMFC.
Atomic layer deposition (ALD) technique was employed to fabricate Pt catalyst and alternative support materials in this study. It is also attempted to replace the Pt prepared by chemical wet reduction. This dissertation is divided into three parts: (1) Employing the horizontal-flow and vertical forced-flow configurations of ALD to investigate the different behaviors of Pt loading on powder substrates. Using vertical forced-flow ALD could enhance the Pt precursor utilization efficiency and protect the support material from forming oxidative byproducts. Moreover, the Pt in a particle size of 3 nm deposited on TiOxN1-x nanoparticles exhibited better oxygen reduction reaction (ORR) activity than those of Pt formed by chemical reduction and commercial E-tek. Its durability was also much better than that of E-tek. (2) The horizontal-flow ALD was used to coat TiO2 on porous polysulfone (PSF) hollow fibers with good uniformity and conformality. Removal of the PSF fibers by thermal treatment and followed by nitridation led to formation of conductive TiOxN1-x and TiN hollow fibers as the support material for Pt. Less rutile phase in the starting material of TiO2 and higher nitridation temperature benefited the formation of TiN. The Pt nanoparticles in a size of 3 nm deposited by vertical forced-flow mode exhibited a high half-wave potential (E1/2) of 0.874 V. Direct nitridation of ALD TiO2-coated PSF hollow fibers at 800 oC and 1000 oC led to the formation of TiOxN1-x@C and TiN@C nanostructures, respectively. Since the ALD of TiO2 bears with high compactness, which can withstand the strain of ripening during nitridation, the hierarchical structures of TiOxN1-x@C and TiN@C were obtained. Moreover, the shape of mesoporous hollow fiber and its interconnected nanostructure were preserved. The ORR activities of Pt deposited by chemical reduction on TiOxN1-x@C and TiN@C were higher than those of Pt on carbon black and commercial JM catalyst. (3) The comparison of ALD of Pt on various Ni nanohoneycomb substrates was made to investigate how the surface species affected the loading and chemical components of Pt. The annealed Ni nanohoneycomb structure showed better affinity for deposition of Pt. The loading and uniformity of Pt on annealed Ni nanohoneycombs were significantly higher than those of Pt on pristine nanohoneycombs.

摘要
Abstract
致謝
Chapter 1 Introduction
1-1 Background of Research 1
1-1.1 Hydrogen energy 3
1-2 Fundamentals of Fuel Cell 5
1-2.1 The development and tendency of fuel cell 5
1-2.2 Advantages of fuel cell 10
1-2.3 Types of fuel cell 12
1-3 Atomic Layer Deposition (ALD) 15
1-3.1 The development of ALD 15
1-3.2 Advantages and limitations of ALD 16
1-4 Motivation and contact of the Research 20
References 22
Chapter 2 Literature Review
2-1 Fundamental of Proton Exchange Membrane Fuel Cell (PEMFC) 24
2-1.1 Thermodynamics of fuel cell 26
2-1.2 Kinetics of fuel cell 28
2-1.3 Mechanism of oxygen reduction reaction (ORR) 30
2-2 Components of PEMFC 33
2-2.1 Proton exchange membrane (PEM) 34
2-2.2 Catalyst layer 35
2-2.3 Gas diffusion layer 36
2-2.4 Bipolar plates 38
2-3 Catalysts 40
2-3.1 Material of catalyst 41
2-3.2 Fabrication of Pt catalyst 44
2-4 Support Material of Catalyst 45
2-4.1 Degradation of catalyst on support material 45
2-4.2 Carbon support 46
2-4.3 Non-carbonaceous support 48
2-4.4 Hybrid support 50
2-5 Atomic Layer Deposition (ALD) 50
2-5.1 Mechanism of ALD process 51
2-5.2 Instrumentation of ALD 56
2-5.3 ALD of Pt catalyst 56
2-5.4 ALD of TiO2 58
2-5.5 Configuration of vertical forced-flow 59
References 61
Chapter 3 Enabling Higher Electrochemical Activity of Pt Nanoparticles Uniformly Coated on Cubic Titanium Oxynitride by Vertical Forced-flow Atomic Layer Deposition
Abstract 66
3-1 Introduction 66
3-2 Experimental Procedures 69
3-2.1 Fabrication of Pt@TiOxN1-x 69
3-2.2 Characterization of Pt@ TiOxN1-x 70
3-2.3 Electrochemical measurement 72
3-3 Results and Discussion 73
3-3.1 Formation and characterization of conductive TiOxN1-x nanoparticles 73
3-3.2 Characterization of the Pt nanoparticles deposited on TiOxN1-x 77
3-3.3 Pt deposition with different cycles by vertical forced-flow mode 80
3-3.4 Electrochemical analysis of Pt@TiOxN1-x 83
3-4 Conclusion 88
References 89
Chapter 4 Fabrication of Porous TiOxN1-x and TiN Hollow Fibers and Deposition of Pt Nanoparticles by Atomic Layer Deposition and Their Enhanced Electrochemical Activities
Abstract 96
4-1 Introduction 96
4-2 Experimental Procedures 99
4-2.1 Fabrication of ALD-Pt@TiOxN1-x or TiN hollow fiber with interconnected nanotubes 99
4-2.2 Characterization of Pt@TiOxN1-x and TiN hollow fiber 102
4-2.3 Electrochemical measurement 102
4-3 Results and Discussion 103
4-3.1 ALD-TiO2 on PSF hollow fiber 103
4-3.2 Formation of TiOxN1-x and TiN hollow fibers 103
4-3.3 Characterization of Pt@TiOxN1-x and TiN hollow fibers 111
4-3.4 Electrochemical performances of Pt@TiOxN1-x and Pt@TiN hollow fiber catalysts 117
4-4 Conclusion 120
References 120
Chapter 5 Nitrogen-Doped Carbon Hollow Fiber Consisting of Internal Interconnected Nanofibers Fabricated by Confinement Effect of TiOxN1-x and TiN Coating
Abstract 126
5-1 Introduction 126
5-2 Experimental Procedures 129
5-2.1 Deposition of TiO2 on PSF by ALD and nitridation 129
5-2.2 Characterization of the nitridized samples 131
5-2.3 Electrochemical measurement 132
5-3 Results and Discussion 133
5-3.1 The TiO2 coating by ALD on PSF hollow fiber 133
5-3.2 Nitridation of TiO2-coated PSF hollow fibers 133
5-3.3 Electrochemical performance of the samples decorated with Pt catalyst 143
5-4 Conclusion 145
References 147
Chapter 6 Fabrication and Characterization of Pt Nanoparticles on Ni Nanohoneycomb Structure by Atomic Layer Deposition
Abstract 153
6-1 Introduction 153
6-2 Experimental 155
6-3 Results and Discussion 156
6-3.1 Formation of Ni nanohoneycomb structure 156
6-3.2 The effect of NiCl2 concentration 156
6-3.3 Deposition of Pt nanoparticles on Ni nanohoeycombs 159
6-4 Conclusion 164
References 165
Chapter 7 Conclusions 169
Chapter 8 Suggested Future Work 172

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Chapter 4
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Chapter 5
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Chapter 6
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