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研究生： 曾世凱
Tzeng, Shi-Kai
論文名稱： 氧化鋅一維結構成長、元件組裝及紫外光偵測器製作之研究
Growth, Assembly, Ultraviolet Photodetector Fabrication of One-dimensional ZnO
指導教授： 洪敏雄
Hon, Min-Hsiung
學位類別： 博士
Doctor
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： 2012
畢業學年度： 100
語文別： 中文
論文頁數： 115
中文關鍵詞： 水熱法 、水溶液法 、氧化鋅 、紫外光檢測器 、表面改質 、奈米結構
外文關鍵詞： hydrothermal, aqueous-solution process, zinc oxide, ultraviolet photodetector, surface modification, nanostructure
相關次數： 點閱：94  下載：1 
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    • 本篇論文主要目標是以低溫的溼式化學法製程，製作出高效能的紫外光偵測器。從材料合成、組裝與元件的製作及測量，製程的最高溫度小於200oC。採用的方法是先利用水熱法合成單晶的氧化鋅奈米線，並藉由調控界面活性劑以改變氧化鋅奈米結構的尺寸。之後利用介電泳動的製程將單晶氧化鋅奈米線在電場的輔助下組裝成紫外光偵測器。接著，表面改質氧化鋅奈米線以提高光偵測器對光的靈敏度與響應時間。最後為了簡化製程與縮短時間，直接將成長氧化鋅的晶種以電化學沉積於電極上，隨後於溶液中成長氧化鋅時，使之自組裝成光偵測器。
    為搭配後端的光偵測器應用，氧化鋅奈米線的尺寸需要在合成的過程中獲得良好的控制，在此使用聚乙烯醇作為奈米線成長的導向劑，並藉由調控聚乙烯醇的添加量以達到控制奈米線的目的。在室溫時，聚乙烯醇的氫氧基能與溶液中二價鋅離子配位，在反應溫度為150 oC的鹼性溶液中，聚乙烯醇的氫氧基斷鍵導致鋅離子能在反應過程中持續的被釋放。此過程中聚乙烯醇相當於儲存鋅離子的裝置，在反應前因為鋅離子的含量較少所以有較少的成核點，隨著延長持溫時間，鋅離子能緩慢的被釋放以提供氧化鋅成長所使用。當聚乙烯醇的添加量由0增加至0.92 wt%時，氧化鋅奈米線的平均長度由1.3 m增加至126 m。在本研究中藉由介電泳動排列氧化鋅奈米線並跨接於電極之間，用以製作成光導體式的紫外光偵測器，並藉著聚甲基丙烯酸甲酯作為鈍化層被覆於氧化鋅表面，進而達到降低暗電流的效果。同時，為了增加光偵測器對光的靈敏度，藉由溶劑輔助式壓印製程在光偵測器上製作具微透鏡陣列的結構的聚甲基丙烯酸甲酯，用以增加入射光的穿透度與降低反射率，進而加強了光偵測器的訊雜比。為降低響應時間，在本研究中將銀奈米顆粒光還原沉積於氧化鋅表面，並發現銀/氧化鋅的界面存在著非劑量比的氧化銀，推測這非計量比的氧化銀導致銀奈米顆粒與氧化鋅表面產生蕭基式接觸，為改善元件性能的重要關鍵。接著，直接利用濕式化學法合成氧化銀奈米顆粒，並使之附著於氧化鋅表面，更降低光偵測器的響應時間，氧化銀奈米顆粒作為p型半導體將附著於n型的氧化鋅上，使其間產生p-n接面。在光偵測器未照光時，此p-n接面可增加氧化鋅表面之空乏層厚度，降低暗電流。偵測器在照射與關閉光的情況下，可藉內建電場的輔助同時增加光靈敏度與加速光響應速度。將氧化鋅表面沉積氧化銀後可獲得大於105的訊雜比，響應時間小於1 sec的高效能紫外光偵測器。
    為了簡化製作光偵測器的製程與縮短元件製作時間，利用電鍍鋅於電極上作為晶種，再藉由水溶液法合成氧化鋅，在電極間相向成長的氧化鋅奈米線晶體會同時自組裝成光偵測器的結構。經由光致發光光譜儀與X光電子能譜儀分析得知，水溶液法合成的氧化鋅表面佔約44.6%的 導致其響應時間極長，達7×104 sec以上。為改善此複雜的奈米結構的表面特性，則利用在純水中進行水熱反應的方式將表面鈍化，並有效的降低響應時間致220 sec。

    Fabrication of high-performance ZnO nanowire-based photodetectors through low temperature processes is the main purpose of this dissertation. For this purpose, a wet chemical process was employed as the main technique for synthesizing ZnO nanowires. Besides, the morphology and size of ZnO nanowires were tuned by the addition of PVA with varied amount. PVA acts as a structure-directing agent for growing the ultra-long ZnO nanowires. Then, the ZnO UV photdetectors were fabricated by aligning ZnO nanowires between the interdigitated electrodes via a dielectrophoresis process. Based on decreasing the reflection of UV light on ZnO surface, the signal to noise ratio can be improved via capping PMMA micro-lens arrays. Then Ag nanoparticles were loaded onto the surface of ZnO nanowires by a photoreduction process, for the purpose of decreasing the response time. By investigating the Ag/ZnO interface, a non-stoichiometric AgOx phase is observed by HRTEM images and SAED patterns. Ag2O nanoparticles were also decorated onto the surface of ZnO nanowires. Photogenerated electrons and holes can be separated by the built-in potential induced by Ag2O/ZnO p-n junction. After decorating Ag2O nanoparticles onto ZnO surface, the maximum signal to noise ratio is larger than 105, accomplishing both a short rise time and a decay time of less than 1 s. After turning off UV irradiation, the current of Ag2O/ZnO heterostructured UV detector is recovered to the initial value within around 10~13s.
    The aqueous solution processes were also used to self-assemble ZnO nanobridge photodetcors. By investigation with XPS and PL, singly ionized oxygen vacancies induce the persistence photoconductivity of ZnO-nanowire-based UV photdetectors. A hydrothermal process was used to passivate the surface states and singly ionized oxygen vacancies on the ZnO nanowires. The photoresponse time decreases significantly after extending the hydrothermal duration.

    總目錄 摘要 I Abstract III 致謝 V 總目錄 VI 圖目錄 VIII 表目錄 XII 中英名詞與符號對照表 XIII 第一章、緒論 1 1-1引言 1 1-2研究動機與目的 3 第二章、理論基礎 5 2-1半導體光偵測器原理 5 2-1-1 光的吸收 5 2-1-2 光偵測器元件結構 5 2-1-3 光偵測器特性參數 8 2-2 ZnO的性質 9 2-2-1 ZnO的晶體結構 9 2-2-2 ZnO的本質缺陷 11 2-3 ZnO一維奈米結構的合成技術 11 2-4 濕式化學法合成ZnO一維奈米結構 12 2-5 一維奈米結構元件組裝 13 2-6 ZnO紫外光偵測器 16 2-7 氧氣於ZnO表面的吸附與脫附 18 2-8 電化學沉積ZnO一維奈米結構之晶種 19 2-8-1 鋅晶種層 19 2-8-2 電化學沉積 20 第三章 實驗步驟與方法 23 3-1 實驗藥品 24 3-2 水熱法合成ZnO一維結構 25 3-2-1 水熱法設備 25 3-2-2 合成方法 25 3-2-3 鋅離子濃度量測 27 3-3 介電泳動製程組裝ZnO一維結構 27 3-3-1 實驗流程 27 3-4聚甲基丙烯酸甲酯微透鏡陣列(MLA)製作 28 3-5 光還原沉積Ag奈米顆粒於ZnO一維結構表面 30 3-6 Ag2O奈米顆粒合成 30 3-7 電化學沉積晶種鋅 31 3-7-1 電化學沉積設備 31 3-7-2 實驗流程 31 3-8 水溶液法製程自組裝ZnO一維結構光偵測器 33 3-8-1水溶液法製程 33 3-8-2 水熱法改質ZnO表面 33 3-9 材料分析與元件特性分析 34 3-9-1 X光繞射分析(XRD) 34 3-9-2 掃瞄式電子顯微鏡分析(SEM) 34 3-9-3 X光電子能譜儀(XPS) 34 3-9-4 穿透式電子顯微鏡(TEM) 35 3-9-5 傅利葉轉換紅外線光譜儀(FT-IR) 35 3-9-6 光致發光光譜儀(PL) 35 3-9-7 光偵測器特性分析 35 第四章 實驗結果與討論 37 4-1 水熱法合成ZnO一維結構 37 4-1-1 水熱法合成ZnO之晶體結構 37 4-1-2 鋅離子濃度對ZnO一維結構成長的影響 39 4-1-3 聚乙烯醇添加對ZnO一維結構成長之影響 41 4-2 介電泳動製程組裝ZnO一維結構 47 4-3 ZnO一維結構紫外光偵測器特性 49 4-4 聚甲基丙烯酸甲酯(PMMA)微透鏡陣列改善ZnO紫外光偵測器特性 53 4-4-1 ZnO/聚甲基丙烯酸甲酯複合材料光學特性 54 4-4-2 聚甲基丙烯酸甲酯微透鏡陣列的光學特性 62 4-4-3 聚甲基丙烯酸甲酯微透鏡陣列對ZnO紫外光感測器特性的影響 65 4-5 Ag奈米顆粒改善ZnO紫外光偵測器特性 67 4-6 Ag2O奈米顆粒改質ZnO紫外光偵測器特性 77 4-6-1 Ag2O奈米顆粒合成 77 4-6-2 Ag2O/ZnO異質結構紫外光偵測器特性分析 81 4-7 電鍍Zn晶種參數對ZnO橋接式紫外光偵測器特性的影響 85 4-7-1 電鍍Zn晶種尺寸對ZnO型貌之影響 85 4-7-2 橋接式ZnO光偵測器特性 89 第五章 結論 102 第六章 參考文獻 104 圖目錄 Fig. 2- 1 Optical generated electron-hole pair formation in semiconductor, when (a) h =Eg, (b) h >Eg and (c) h <Eg[1,22]. 6 Fig. 2- 2 Schematic structure of different semiconductor photodetectors: (a)photoconductor, (b)Schottky photodiode, (c)p-n photodiode and (d) p-i-n photodiode[2]. 6 Fig. 2- 3 Stick and ball representation of ZnO crystal structure: (a) cubic rocksalt, (b) cubic zinc blende, and (c) hexagonal wurtzite. The shaded gray and black spheres denote Zn and O atoms, respectively[24]. 10 Fig. 2- 4 Energy levels of native defects in ZnO. The donor defects are Zni●●, Zni●, ZniX ,Vo●●,Vo●,VoX and the acceptor defects are Vzn' ,Vzn' [30]. 10 Fig. 2- 5 Bridge-type GaAs nanowhisker arrays grown on the side wall of a ditch formed on the substrate. (a) SEM image of the fabricated bridge-type nanowhisker arrays. (b) Schematic illustration of (a). Nanowhiskers grew on side wall in the <111> As direction , and their tops reached the other side[49]。 15 Fig. 2- 6 Schematic energy band diagrams of ZnO-nanowire surface illustrate the states (a) in dark and (b) under UV light illumination[51]. 17 Fig. 2- 7 Typical adsorption isobars: the solid lines are equilibrium physisorption and a chemisorption isobar, the dashed line represents irreversible chemisorption. A maximum coverage of chemisorbed molecules is obtained at a temperature Tmax. Below Tmax the chemisorption is irreversible because the rate of desorption becomes negligible[56]. 17 Fig. 3- 1 The flow chart of experiment for growth, assembly and fabrication of ZnO nanowires-based UV photodetectors via wet chemical processes. 23 Fig. 3- 2 Photograph of autoclaves used in the study. 26 Fig. 3- 3 (a) Schematic diagram of dielectrophoresis equipment. (b) ZnO nanowires aligned on interdigitated electrode by dielectrophoresis process. 29 Fig. 3- 4 (a) Shematic structure of ZnO photodetector with MLA-patterned capping PMMA layer. (b) SEM image of the MLA structure patterned on the device. 29 Fig. 3- 5 The schematic diagram of equipments for electrodeposition 32 Fig. 3- 6 Schematic diagram of ZnO nanobridge in the gap of interdigitated electrode 32 Fig. 3- 7 Shematic diagram of equipments used for characterizing photodetectors. 36 Fig. 4- 1 The TEM images of (a)birght-field, (b) high-resolution and (c) SAED-pattern revealing ZnO nanostructure synthesized by mixing with 2.5 M 10 ml TMAH and 0.16 M Zn(Ac)2 methanol solution 5 ml at 150oC for 24 h. (d) and (e) show the d-spacing measurement marked in (b). 38 Fig. 4- 2 The SEM images of ZnO nanostructures synthesized in reaction solution having different [Zn2+]. The concentration of TMAH, reaction temperature and reaction time are 2.5 M, 150oC and 24 h, respectively. 40 Fig. 4- 3 The variation of length and diameter of ZnO nanowires synthesized by different Zn2+ concentrations. 40 Fig. 4- 4 SEM images of as-prepared ZnO at 150oC for a reaction time of 24 h with PVA addition of (a) 0 wt%, (b) 0.23 wt%, (c) 0.46 wt%, and (d) 0.92 wt%. 42 Fig. 4- 5 (a) XRD patterns of as-prepared ZnO at 150oC for a reaction time of 24 h with PVA addition of 0.92 wt%. Average length of 1-D structures plotted as a function of (b) PVA addition and (c) growth time. 43 Fig. 4- 6 The relationship between PVA content and Zn2+ ion concentration in methyl solution at room temperature. 45 Fig. 4- 7 FT-IR spectra for (a) PVA and (b) the residual solutions of PVA+TMAH aqueous solution after reaction at 150oC for 12 h. 45 Fig. 4- 8 The channel cross-section area between electrode gap is plotted as a function of (a) applied electrical field, and (b) frequency. 48 Fig. 4- 9 (a), (b) I-V characteristics and (c) time-dependent photocurrent characterized at UV light 365 nm with a power density of 1.46 mW/cm2. 50 Fig. 4- 10 Photocurrent of ZnO nanowires-based UV photodetector plotted as a function of irradiative wavelength. 51 Fig. 4- 11 (a) Photoluminescence spectra of ZnO/PMMA hybrid film with different blending amounts of ZnO nanowires into PMMA. (b) Integral area ratio of UV/visible and (c) near-band-edge emission plotted as a function of blending amount of ZnO nanowires. (d) The corresponding SEM image of ZnO nanowires which blended into PMMA. 55 Fig. 4- 12 The FT-IR spectra of PMMA and ZnO/PMMA hybrid films. 57 Fig. 4- 13 Schematic diagram of (a) ZnO nanostructures blended into PMMA matrix with varied vol%, and (b) the effect of PMMA passivation layer on the rigid band diagram of ZnO. 57 Fig. 4- 14 (a) SEM image of ZnO nanoparticles, and (b) corresponding PL spectra of ZnO/PMMA with varied volume ratio. (c) the enlarged view of (b) in the range of 360-400 nm. 59 Fig. 4- 15 (a) The transmittance of ZnO/PMMA hybrid film with different blending amounts of ZnO nanoparticles in PMMA. (b) the optical bandgap of ZnO and ZnO/PMMA composite (0.5×10-3 vol%). 61 Fig. 4- 16 (a) transmittance (without substrate) of flat and MLA-patterned PMMA films, and (b) reflection (made with SiO2/Si substrate) of flat and MLA-patterned PMMA films. 63 Fig. 4- 17 Optical microscopic image of aligned ZnO nanowires between electrodes (a) without and (b) with PMMA capping layer. 66 Fig. 4- 18 (a) I-V curves taken in dark and under illumination for samples with different surface treatments, and corresponding SEM images of (b) as-fabricated and (c) MLA-patterned ZnO-nanowires photodetectors. 66 Fig. 4- 19 (a) XRD pattern, (b) bright field and (c) dark field image of Ag-decorated ZnO NWs after being irradiated in AgNO3 solution at =365 nm for 30 mins. 69 Fig. 4- 20 (a) HRTEM image shows the interface between Ag nanoparticle and ZnO nanowire. The corresponding nano-beam SAED of ZnO nanowire, Ag nanoparticle and ZnO/Ag interface (circle (b), (c) and (d)) are shown in (b), (c) and (d), respectively. (e) HRTEM image reveals the Ag/ZnO interface. 70 Fig. 4- 21 (a) I-V characteristics, (b) photoresponsivity and (c) time-dependent photocurrent of ZnO nanowires-based UV detector decorated with and without Ag nanoparticles, received under UV light ( l=365 nm) with power density of 964 W/cm2. 73 Fig. 4- 22 Schematic energy band diagrams for blank and Ag-decorated ZnO nanowires-based photodetectors illustrating the states in dark and under UV light illumination. 75 Fig. 4- 23 XRD patterns of Ag2O /ZnO heterostructure synthesized with various pH value. (a) and (b) show the results of ZnO nanowires immersed in blank NaOH and AgNO3 solution, respectively. (c), (d) and (e) show the results of ZnO/Ag2O heterostructure synthesized under identical AgNO3 concentration with various pH values: (c) 12,(d) 13 and (e) 13.9. 78 Fig. 4- 24 SEM images of ZnO NWs immersed in blank (a) NaOH and (b) AgNO3 solution, respectively. (c), (d) and (e) show the images of ZnO/Ag2O heterostructure synthesized under identical AgNO3 concentration with various pH values of 13.9, 13 and 12, respectively. 80 Fig. 4- 25 (a) I-V characteristics of blank ZnO nanowire photodetectors measured both in dark and under 365 nm UV light illumination with a power density of 1.46 mW/cm2. (b) Photoresponse behavior of blank ZnO nanowire photdetectors measured under 365 nm UV light with different irradiation powers (operation bias -4 V). 82 Fig. 4- 26 Photocurrent of ZnO NWs plotted as a function of excitation intensity ( =365 nm) with -4 V applied bias. 83 Fig. 4- 27 The energy band diagram near the surface of Ag2O/ZnO in dark and and after turning on the UV light. 83 Fig. 4- 28 SEM images of electrodeposited Zn films with varied current density at an identical deposition time of 450 s. 86 Fig. 4- 29 The (a) grain size and (b) thickness of Zn films plotted as a function of deposition time. 88 Fig. 4- 30 X-ray diffraction patterns of as-synthesized ZnO-NWs films grown on the seed layers with different grain sizes. 88 Fig. 4- 31 Texture coefficient (TC) of the low index planes of ZnO NWs obtained on various seed-layer grain sizes. 90 Fig. 4- 32 The diameters of ZnO NWs are plotted as a function of Zn grain size. 90 Fig. 4- 33 The SEM images of ZnO nanobridge UV detector with varied ZnO diameter (a) 530 nm and (b) 190 nm. The corresponding I-V curves of ZnO nanowires photodetectors. 92 Fig. 4- 34 Time-dependent photoresponse of ZnO nanowires photodetectors characterized in air under 0.1 V bias ( =365 nm, intensity=72 W/cm2). The green lines indicate that the decay process can be fitted well by a biexponential relaxation equation. 92 Fig. 4- 35 Photoluminescence spectra of ZnO NWs of different diameters measured at room temperature with an excitation wavelength of 325 nm. 94 Fig. 4- 36 Schematic energy band illustration for ZnO NWs in recovery process: ① band-to-band recombination mechanism, ② photogenerated electrons trapped by , ③ is formed due to trapping of electron by and acts as shallow donor before recombination. 94 Fig. 4- 37 (a) photoluminescence spectrum of ZnO NWs treated with different hydrothermal duration at 200oC. (b) the ratio of UV/green plotted as a function of hydrothermal duration in pure water. 96 Fig. 4- 38 The O1s XPS spectra of ZnO NWs treated with varied hydrothermal time. 97 Fig. 4- 39 (a) The I-V characteristics and (b) the time-dependent photocurrents of ZnO NW-based photodetectors with different hydrothermal durations. ( =365 nm, power density=1.46 mW/cm2). 99 Fig. 4- 40 (a) time-dependent photoresponse of post-hydrothermal ZnO NWs with an applied bias of 0.5 V under different power density of light ( =365 nm). (b) photocurrent of ZnO NWs measured as a function of excitation intensity with 0.5 V applied bias. 101 表目錄 Tab. 3- 1 The chemicals used in this study 24 Tab. 4- 1 Results for O1s XPS spectra of ZnO NWs with different hydrothermal time. 97

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