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研究生： 陳佑瑜
Chen, Yow-Yu
論文名稱： 針尖誘導局部陽極氧化與蜇合劑非導電溶液的協同作用製備摻雜氮(N) TiO2/Ti 薄膜
Synergistic effect of chelating agents and tip-induced anodization through non-conducting solutions for Local deposition of N-doped TiO2 films on Ti substrates
指導教授： 張高碩
Chang, Kao-Shuo
學位類別： 碩士
Master
系所名稱： 工學院 - 材料科學及工程學系
Department of Materials Science and Engineering
論文出版年： 2023
畢業學年度： 111
語文別： 英文
論文頁數： 142
中文關鍵詞： 溶液製程法 、選區局部陽極氧化法 、化學蜇合劑 、氮摻雜二氧化鈦薄膜
外文關鍵詞： tip-induced anodization process, non-conducting solution, local anodization, chelating agent, nitrogen-doped TiO2 film
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    • 本研究為新穎的薄膜製程方法，針尖誘導局部陽極氧化，可在常溫常壓的一般環境下進行，透過針尖電極在鈦基板上局部陽極氧化，直接製備氮摻雜的二氧化鈦（TiO2）薄膜。相較於傳統使用導電性電解液的陽極氧化技術，本研究使用了乙二醇為溶劑分別和尿素或鈦異丙醇酸酯形成錯合物的非導電性溶液。透過施加直流高電壓到銳利的陰極鎢針上，使基板上的局部區域能夠進行陽極氧化。該方法實現了陽極氧化薄膜的形成，並將摻雜物(氮或是鈦)引入氧化膜中。此外，通過電腦控制的三軸移動載臺，能夠在無需物理遮罩的情況下對薄膜進行定制圖案化。因此，這是一種單步驟、成本效益高且低能耗的方法。

    本研究闡述了在鈦基板上直接沉積氮摻雜的TiO2薄膜以及在矽基板上沉積鈦摻雜的二氧化矽（SiO2）薄膜的方法。透過控制不同螯合劑（如乙二醇和檸檬酸）的添加和尿素的用量，成功製備了具有不同特性和形貌的氧化膜。對於氮摻雜的二氧化鈦薄膜的形成機制，我們提出了一種假設：當高電壓作用下，尿素在電化學過程中被斷鍵破壞，釋放出帶負電的氮離子，接著氮離子被吸引到正偏壓鈦基板上所生成的二氧化鈦薄膜中達到氮摻雜效果。我們的結果表明，螯合劑與針尖誘導的非導電性溶液陽極氧化具有協同效應。

    This study reports a novel method of localized anodic oxidation through a needle-tip electrode to fabricate nitrogen-doped titanium dioxide (TiO2) thin films directly on titanium substrates at room temperature. Compared with traditional anodic oxidation techniques that employ conductive electrolyte solutions, non-conductive solutions composed of urea or titanium isopropoxide complexes were used. By applying a high DC voltage to a sharp cathodic tungsten needle, local regions on a substrate were enabled for anodic oxidation.
    This approach enabled the formation of anodic oxide films and the incorporation of dopants into oxide films as well. Additionally, a computer-controlled three-axis moving stage allows customizable patterning of films without the need of physical masks. Thus, this approach indicates a single-step, cost-effective, and low-energy consumption method that operates under ambient conditions. In this study, direct deposition of nitrogen-doped TiO2 films on titanium substrates and titanium-doped silicon dioxide (SiO2) films on silicon substrates were elucidated. By controlling the addition of different chelating agents (such as ethylene glycol and citric acid) and amounts of urea, the oxide films with diverse characteristics and morphologies were fabricated. The formation mechanism of the nitrogen -doped TiO2 film was proposed that when the urea and ethylene glycol solution was applied by high voltages, urea was electrochemically damaged and released negatively charged nitrogen ions, which were then incorporated in the resulting TiO2 film on a positively biased Ti substrate. Our results suggest the synergistic effect of chelating agents and tip-induced anodization in non-conductive solutions.

    Chapter 1 Introduction 1 1.1 Background 1 1.1.1 Film deposition techniques 1 1.1.2 Solution processing 1 1.1.2.1 Conventional approach: electrodeposition through electrolyte solution 3 1.1.2.1.1 Electroplating 4 1.1.2.1.2 Anodization 8 1.1.2.1.2.1 Working Principles 8 1.1.2.1.2.2 Two types of anodic layers: barrier type & porous type 10 1.1.2.1.2.2.1 Barrier-type anodic layers 10 1.1.2.1.2.2.2 Porous/tubular-type anodic layers 12 1.1.2.1.2.3 Field assisted dissolution of films 13 1.1.2.1.2.4 Field assisted oxidation of films 16 1.1.2.1.2.5 Effect of Applied Voltage or Current 19 1.1.2.1.2.6 Application 21 1.1.2.2 Novel approach: electrochemical deposition in non-conducting solutions 22 1.1.2.2.1 Localized Anodization in Non-conductive Solutions 26 Non-conductive solutions 27 High voltage & low current 27 Tip – substrate distance 29 Radius of sharp tip 30 Tip scanning rate 31 1.1.2.2.1.1 Tip–substrate interface interaction 33 1.1.2.2.1.1.1 Bias-induced oxidation 33 1.1.2.2.1.1.2 Space charge effect 35 1.1.2.2.2 Doping by Polymerized complex method 37 1.1.2.2.2.1 Chelation reaction 39 1.1.2.2.2.2 Why is chelating agent needed? 40 1.1.2.2.2.3 Polymerization reaction 41 Addition polymerization 42 Condensation polymerization 42 1.2 Fabrication process of a sharp tip 43 1.2.1 Background of electrochemical etching 43 1.2.2 Mechanism of tip etching 45 1.2.3 Experimental parameters for the fabrication process of tip-etching 47 Chapter 2 Experimental method 48 2.1 Materials 48 2.1.1 Chemicals for solution precursors 48 2.1.2 Chemicals for substrate cleaning 48 2.1.3 Substrate 49 2.1.4 Substrate cleaning process 49 2.2 Fabrication process of a tungsten tip 51 2.2.1 Materials and equipment 51 2.2.2 Experimental procedure for the fabrication of a tungsten tip 53 2.2.3 Tungsten tip cleaning 57 2.3 Preparation of precursor solutions 59 2.3.1 Preparation of titanium polymerized complex precursors (with citric acid) 59 2.3.2 Preparation of titanium complex precursors (without citric acid) 60 2.3.3 Preparation of nitrogen-contained precursors 61 2.4 Experiment setup 62 2.5 Plasma test experiment 68 2.6 Non-conductive solutions test 70 2.7 Fabrication of titanium-doped SiO2 films on silicon substrates 70 2.8 Fabrication of TiO2 films on titanium substrates 71 2.9 Fabrication of nitrogen-doped TiO2 films on titanium substrates through chelating agent 71 2.10 Characterization 73 2.10.1 X-ray diffraction (XRD) analysis 73 2.10.2 Optical microscopy (OM) 74 2.10.3 High Resolution Scanning Electron Microscope (SEM) 74 2.10.4 X-ray Photoelectron Spectroscopy (XPS) 75 2.10.5 Alpha-step analysis 76 2.10.6 Optical emission spectrum test (OES) 77 2.10.7 Conductivity- TDS-Salinity meter 78 Chapter 3 Results and discussion 79 3.1 Electrochemical reaction in conductive solutions 79 3.2 Electrochemical reaction in non-conductive solutions 80 3.3 Tip induced local anodic oxidation in non-conductive solutions 81 3.4 Various non-conductive solutions 82 3.5 Tip induced oxidation on silicon substrates 84 3.5.1 Experimental parameters 85 3.5.1.1 Distance between a tip and a substrate 85 3.5.1.2 Voltage / current for oxide surface morphology 86 3.5.1.3 Time effect on the size of films 89 3.5.1.4 Time effect on thickness of films 90 3.5.1.5 Stability study of a cathodic tungsten tip 91 3.5.2 Characterization of the film on Si substrates 98 3.5.2.1 XRD 98 3.5.2.2 Raman spectroscopy 99 3.5.2.3 SEM EDS mapping 101 3.5.2.4 XPS 104 3.5.2.5 XPS depth profile 106 3.6 Tip induced oxidation on a Ti substrate 109 3.6.1 Experimental parameters 109 3.6.1.1 Voltage / current to tune the morphology of resulting oxide films 109 3.6.1.2 Time effect on the size of the films 112 3.6.1.3 Scanning rate effect on film thickness 113 3.6.2 Characterization of the TiO2 film 115 3.6.2.1 XRD 115 3.6.2.2 XPS 117 3.6.2.3 SEM 119 3.6.2.4 SEM EDS mapping 120 3.6.3 Nitrogen-doped TiO2 films 121 3.6.3.1 Tuning of nitrogen concentrations 121 3.6.3.1.1 Heating temperature of precursors & anodization time 121 3.6.3.1.2 Amounts of urea 122 3.6.3.2 Characterization of N-TiO2 124 3.6.3.2.1 XPS 124 3.6.3.2.2 SEM EDS mapping 126 Chapter 4 Conclusions and future work 128 4.1 Conclusions 128 4.2 Future work 130 Chapter 5 References 131

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