貴重電極之製備及其應用於電化學製備之金屬奈米粒子之研究

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研究生：	林葆喜 Pau Yee Lim
論文名稱：	貴重電極之製備及其應用於電化學製備之金屬奈米粒子之研究 Noble Electrode Fabrication and Its Application to the Electrochemical Deposition of Metal Nanoparticles
指導教授：	施漢章 Han-Chan Shih
口試委員:
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2006
畢業學年度：	94
語文別：	英文
論文頁數：	197
中文關鍵詞：	化學氣相沉積、薄膜電極、滲硼鑽石薄膜、背景電流、電位範圍、電化學動能、氧化銥、鈦基材、熱處理、酸蝕、氫化鈦、表面粗度、銀奈米粒子、電化學合成、分散性
外文關鍵詞：	chemical vapor deposition, thin film electrode, boron doped diamond film, background current, potential window, electrochemical kinetics, iridium oxide, titanium substrate, heat treatmrent, acid etch, titanium hydrides, surface roughness, silver nanoparticles, electrochemical synthesis, dispersion
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奈米技術在許多不同產業領域埋藏巨大的商機。其中，金屬奈米粒子在實用上頗受各產業的殷切期待，包括資訊電子產業、構造材料、觸媒塗料、抗菌等應用；同時亦積極尋求可量產製備奈米金屬粉體之技術。本研究中探討以電化學法製備高度分散在溶液中之奈米金屬粉體之前瞻技術，以及應用在金屬離子還原反應形成粒子之貴重電化學電極材料技術。
研究証實於室溫條件下在電化學電極表面即可快速並有效還原金屬金及銀離子，並同時分散奈米金及銀金屬粒子於溶液中。奈米金屬粉體以電化學法製備的液相環境分別包括乙二醇及水溶液；添加其中之分散劑聚乙烯呲咯酮(Poly(N-vinylpyrrolidone))亦經檢驗其電化學穩定性。電化學法所製備奈米金屬粉體之特性如粒徑分布、粒子形狀及大小、微結構及成長方向等則利用物理分析技術如,HRTEM及NBED進行觀察。為未來可量產及提高效率，實驗並進一步針對製程條件探討其對於奈米銀粒子形成之影響。透過利用紫外光-可見光頻譜，分析溶液中之奈米銀粒子形成量因著條件改變之變化；包括電化學條件及電解液條件如分散劑之分子量、KNO3濃度，以及電化學電位之影響。另外，在電極材料方面，實驗比較使用鉑、鈦、IrO2-Ti2O5 及BDD(含硼鑽石)做為陰極材料對於奈米銀粉體製備效率的差異。
本研究中並分別探討鈦覆BDD膜及IrO2-Ta2O5層之電化學電極特性。實驗分析鈦基材表面條件對於所鍍BDD鑽石膜之電化學特性的影響。經過處理之鈦材基板表面所沉積之BDD膜以拉曼頻譜、SEM、壓痕測試等分析其鑽石膜品質，並進一步分析其電化學特性及耐久性。顯然，利用粗化表面可降低CVD鑽石膜高温製程所產生殘留內應力，有改善鑽石膜和鈦基材之間的附著性。另外，鈦基材採用化學酸蝕，不但得使表面獲得粗化，亦因表面附有TiH可加速CVD鑽石膜成核而獲得致密鑽石膜，進而使鈦覆BDD電極的背景電流極低，且電化學耐久性增加。
鈦基材表面粗化以及氧化層表面保護膜對於表面覆IrO2-Ta2O5層之電化學觸媒電極之耐久性亦有提升之效果。鈦基板處理過程包括熱處理、噴砂、酸蝕可獲得粗度極高的表面，經過熱氧化產生保護膜後再利用熱分解法覆上IrO2-Ta2O5電化學觸媒層。在嚴苛的硫酸液環境下長期以外加電流加速進行陽極氧化反應之加速壽命試驗並顯示，鈦基材表粗度及保護膜氧化層厚度對IrO2-Ta2O5/鈦之電化學電極壽命有直接之關係，並且有加成之作用。
Grade 1 鈍鈦與鈦合金例如Ti–6Al–4V和Ti–3Al–2.5V經由相同表面處理(過程：□及□相熱處理、噴砂、鹽酸蝕刻)後，相比較其微結構差異。實驗並探討微結構變化對於其曝露在酸液中的金屬析出行為及蝕刻後表面粗度。熱處理使Ti–6Al–4V和Ti–3Al–2.5V之晶粒合金元素重新分佈，因而易發生晶粒蝕刻而增加粗糙度，同時因鈍化之晶界逐漸露出表面而獲得較高化學穩定性。

This thesis reports a novel method of using electrochemical process in the synthesis of monodispersed metal nanoparticles. The fabrication of the noble electrodes devised for the electrochemical system was also studied. The synthesis of monodispersed Ag and Au nanosphere particles in ethylene glycol and aqueous solution at room temperature by electrochemical method was demonstrated. Poly(N-vinylpyrrolidone) (PVP) was chosen as the stabilizer and tested for electrochemically stablility. Further characterization by high-resolution transmission electron microscopy (HRTEM) and nano-beam electron diffraction (NBED) pattern was carried out to investigate the particles size and growth direction of the nanosphere particles. For the large scale production of Ag nanoparticles for industrial uses, investigation has been focused on the effect of the electrochemical parameters on the formation of monodisperse Ag nanoparticles. The time evolution of absorption spectra by UV-Visible spectroscopy was employed to illustrate that silver nanoparticles in the electrolyte increase upon electrochemical process under the effect of different electrolyte compositions, applied potential and electrode materials. Suitability of the BDD (boron-doped diamond) electrode and IrO2 coated Ti electrode for the electrochemical synthesis of the Ag nanoparticles was demonstrated.
The electrode properties of BDD thin films grown by a hot-filament chemical vapor deposition technique on the surface modified Ti substrates were evaluated. The BDD films deposited thereon were characterized with various methods, including Raman spectroscopy, scanning electron microscopy (SEM), film adhesion using Vicker’s indentation method, and e.t.c.. Influence of the BDD film quality on the electrochemical performance and electrode stability has also been evaluated. The substrate roughened surface obviously reduces the film inner stress thus improved the film adhesion. In addition, the preetching of the Ti substrate produces the titanium hydride layer that can affect the BDD film growth significantly. The electrodes reveal minimal background current and better stability.
The Ti substrate surface, associated with an intense micro-roughness and a layer of protective Ti oxide, exhibits a significant contribution to the durability of the IrO2-Ta2O5 coated Ti electrode. The IrO2-Ta2O5 coated Ti-supported anodes were examined using c.p. grade 1 Ti plates as the starting substrate material which were given various treatment processes including annealing, chemical etching and thermal oxidation prior to the coating of IrO2-Ta2O5 active layer by the conventional thermo-decomposition method. The attempts analyzed the result of a modified approach to form a significant intense roughness to provide additional bonding and anchoring for the catalyst oxide coating. The roughened Ti substrate was further given protection by a thin thermal oxide layer on the surface. The service life of the IrO2-Ta2O5 coated Ti base electrode was assessed in aqueous solution of H2SO4 in order to clarify the effect of improved bonding durability between IrO2-Ta2O5 coating layer and Ti base metal. The surface morphology and phase structure properties of the Ti substrates and as well as the IrO2-Ta2O5 coating layer were investigated by scanning electron microscope (SEM), X-ray energy dispersive spectroscopy (EDS), X-ray diffraction technique (XRD) and Auger electron spectroscopy (AES) analyses.
Microstructure effect on chemical etching behavior of the annealed Ti–6Al–4Vand Ti–3Al–2.5V titanium (Ti) alloys was compared with that of unalloyed c.p titanium. The microstructural evolution of structure phases after annealing the titanium and its alloys at temperature near and above β transus and followed by furnace cooling to room temperature was studied using optical microscope, SEM and XRD. The microstructure study illustrates that the heat treatment enhanced partitioning effect allows extensive formation of hemispherical and near spherical pits roughened surface to be readily acquired by chemically etching the annealed α+β titanium alloys. The increasing networks of grain boundary β phase near surface act as a barrier over the underneath α grain. The kinetics of the chemical etching reaction process shows that the annealed α+β titanium alloys exhibit relatively lower weight loss and thickness reduction rate, thus illustrate less chemical activity than the annealed unalloyed c.p. titanium.

Abstract
Dedication
Acknowledgements

Chapter 1  Introduction...................................1
1 Motivation............................................1
2 Background............................................2
2.1 Metal powder synthesis..............................3
2.2 Electrodeposition of Metal.........................10
2.3 Conductive diamond electrode.......................14
2.4 Electrocatalytic noble metal electrode.............29
3 Research topics and objectives.......................35
4 Contents and structure of the thesis.................35

Chapter 2  Synthesis of monodispersed metallic nanoparticles by electrochemical method .................38
1  Introduction    .......................................38
2  Experimental........................................40
2.1  Electrolyte preparation...........................40
2.2  Electrochemical measurement.......................41
2.3  Electrochemical synthesis.........................42
2.4  Nanoparticles characterization....................43
3  Results and discussion..............................44
3.1  Electrochemical measurement.......................44
3.2  Particles characterization........................48
4  Conclusion..........................................55

Chapter 3  Influence of electrochemical parameters on electrochemical synthesis of monodispersed metal nanoparticles............................................57
1  Introduction........................................57
2  Experimental........................................58
2.1  Electrolyte preparation...........................58
2.2  Electrochemical synthesis.........................58
2.3  Nanoparticles characterization....................59
3  Results and discussion..............................60
3.1  Electrochemical reaction time.....................60
3.2  Effect of electropolarized potential..............62
3.3  Effect of concentration of KNO3 supporting electrolyte..............................................65
3.4  Effect of concentration of metal precursor........68
3.5  Effect of PVP molecular weight....................71
3.6  Effect of PVP/Ag ratio............................74
3.7  Effect of electrode material......................76
4 Conclusions..........................................79

Chapter 4  Ti-based boron-doped CVD diamond thin-film electrodes: the effects of Ti substrate pretreatment on the electrode properties.....................................81
1 Introduction.........................................81
2 Experimental.........................................84
2.1 Substrate preparation and film deposition..........84
2.2 Film characterization..............................85
2.3 Electrochemical evaluation.........................86
3 Results and discussion...............................87
3.1 Material characterization..........................87
3.2 Electrochemical studies............................99
4 Conclusions.........................................110

Chapter 5  IrO2-Ta2O5 coated electrochemical catalyst Ti electrode：the effect of titanium substrate surface preparation on the electrode service life in aqueous solution of H2SO4.......................................113
1 Introduction........................................113
2 Experimental........................................116
2.1 Substrates preparation and film deposition........116
2.2 Physical characterization.........................119
2.3 Electrochemical measurements......................119
3 Results and discussion..............................121
3.1 Ti-substrates surface roughness...................121
3.2 Thermal oxide layer on Ti substrates..............122
3.3 Coating layer morphology and structure............126
3.4 Voltammetric measurements.........................130
3.5 Durability study..................................133
4 Conclusion..........................................140

Chapter 6  Pure Ti and α+β Ti alloys : microstructure effect on their chemical behavior and microtopography...142
2 Experimental........................................144
3 Results and Discussion..............................147
3.1 Surface morphology................................147
3.2 Chemical behaviour................................161
3.3 Surface roughening................................170
4 Conclusions.........................................174

Chapter 7  Summary......................................175

References..............................................180
Publications
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