超音波輔助化學水浴法製備 AgInS2 薄膜之電化學阻抗頻譜分析

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李芳紜(Fang-Yun Li) 查詢紙本館藏

畢業系所

化學工程與材料工程學系

論文名稱

超音波輔助化學水浴法製備 AgInS2 薄膜之電化學阻抗頻譜分析
(Electrochemical Impedance Spectroscopic Analysis of AgInS2 Thin Films Prepared by Using Ultrasonic Assisted Chemical Bath Deposition)

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摘要(中)

本研究利用超音波輔助化學水浴法製備不同厚度之AgInS2半導體薄膜，並分析此材料之物性與光電性質，探討載子傳輸機制。從實驗結果可發現AgInS2薄膜為Orthorhombic phase，使用吸收光譜推測直接能隙值約為1.93~1.98 eV。光電性質量測的結果顯示，薄膜隨著鍍膜次數增加，可有效降低基材裸露與暗電流上升問題，其中鍍膜兩次之AgInS2光電極具有較佳的光電流值，在偏壓 1 V vs. SCE 下為 1.8 mA/cm2。由開環電位法量測薄膜於犧牲試劑( Na2S+K2SO3 )之費米能階(平帶電位)為 -0.845 V~ -1.020 V v.s. SCE，而Electrochemistry Impedance Spectroscopy（EIS）分析得知薄膜於相同犧牲試劑之費米能階為 -0.8　V~ -1.2 V vs. SCE，兩者數值相近。暗反應中，於犧牲試劑量測之EIS，可發現隨著鍍膜次數增加，R1(溶液電阻及薄膜電阻)也隨著增加；隨著偏壓較負，由於空乏區厚度變薄，會使得半導體電容越來越大；於照光情況下使用犧牲試劑為電解質所量測出來之EIS，可推測照光下，光激發生成之載子在不同偏壓下的傳輸機制，隨著光強增加，R2(電荷傳輸阻抗)會變小，使得載子傳輸較為容易。而不同光強下，皆於 -1.0 V ( vs. S.C.E.) 電容有最大值且載子存活時間最長。
未來的研究可調整不同銀銦比所製備之薄膜，由 EIS 分析技術得知薄膜於照光下之表面態電容、表面態時間，以了解此三成分硫化物光電極薄膜的光電化學行為。

摘要(英)

In our previous studies, we have prepared photocatalyst thin films using Ultrasonic Chemical Bath Deposition (UCBD). By controlling [Ag]/[In] molar ratios in the precursors, we can obtain a single phase AgIn5S8, mixtures of AgIn5S8 and AgInS2 and a single phase AgInS2 thin films. Our studies focused on preparing AgInS2 films with different thickness and studying their electrochemical properties.
All the AgInS2 films after 400 °C thermal treatment have the orthorhombic structure and the direct energy band gap in the range of 1.93 to 1.98 eV. In order to understand the photoelectrochemical properties, AgInS2 films with different coatings were prepared. Xe lamp with an intensity of 100 mW/cm2 was then used to illuminate our samples. The photocurrent densities as a function of applied potential were measured. It was found that homogeneous AgInS2 films were obtained with increasing coatings. In addition, these dense films can effectively suppress the the dark current. In particular, the AgInS2 thin film of deposition two times (485.2 ± 28.2 nm) has the highest photocurrent density of 1.8 mA/cm2 under a bias of 1 V vs. SCE.
The fermi level (flat band potential) of films can be estimated from open circuit potential (OCP) measurements, as well as electrochemical impedance spectroscopic (EIS) analysis. The fermi levels of films in the sacrificial reagent consisted of Na2S and K2SO3 measured using OCP and EIS were varied from -0.845 V~ -1.020 V and -0.8 V~ -1.2 V, respectively. More information, such as charge transfer resistance and capacitance, can be retrieved from EIS analysis by fitting the experimental data to the model. In fact, Randle’ s model fitted the data better than other complicated models, which suggested that carriers transfer to the electrolyte directly from valence band under illumination. When depositing times increase, the resistance R1 (solution resistance and film resistance) will increase. When the applied potential decreases, the capacitance of the semiconductor will increase due to the thinner depletion layer. R2 (charge transfer resistance) will decrease dramatically under illumination, perhaps due to much higher carrier density. At -1.0 V vs. SCE, the AgInS2 film (D3) has the highest capacitance and the logest lifetime.
In the future, the EIS analysis can be used to investigate Ag-In-S thin film photoelectrode with different [Ag]/[In] molar ratios, to realize the physical original of charge transfer process of such materials.

關鍵字(中)

★ 光觸媒
★ 半導體薄膜
★ 電化學阻抗頻譜分析
★ 載子傳輸

關鍵字(英)

★ photocatalyst
★ semiconductor thin films
★ EIS
★ carrier transfer

論文目次

中文摘要 i
Abstract ii
誌謝 iii
目錄 iv
圖目錄 vi
表目錄 ix
第一章緒論 1
1-1 前言 1
1-2 EIS（Electrochemical Impedance Spectroscopy）簡介 3
1-3 研究動機 4
第二章文獻回顧 5
2-1 能帶理論 5
2-2 光觸媒 6
2-3 Ag-In-S半導體薄膜簡介 6
2-4 Ag-In-S薄膜製備技術 7
2-4-1 噴霧熱裂解法 (Spray Pyrolysis, SP) 8
2-4-2 硫化法 (Sulphurization) 9
2-4-3 連續式離子層吸收和反應 (Successive Ionic Layer Adsorption and Reaction) 9
2-4-4 熱蒸鍍法(Thermal Evaporation) 10
2-4-5 電沉積法 (Electrodeposition) 11
2-4-6 化學水浴沉積法 (Chemical Bath Deposition, CBD) 12
2-5 電化學交流阻抗頻譜（Electrochemistry Impedance Spectroscopy，EIS） 13
2-5-1 EIS基礎理論與分析 13
2-5-2 等效電路模型(Equivalent Circuit Models) 16
2-5-3 EIS 之數據分析 19
第三章研究方法 31
3-1 實驗藥品 31
3-2 實驗儀器 32
3-3 實驗流程圖 33
3-4 實驗步驟 33
3-4-1 基材清洗 33
3-4-2 超音波輔助化學水浴法製備 Ag-In-S 光觸媒薄膜 34
3-5 薄膜基本性質檢測 36
3-5-1 二次離子質譜儀(Secondary ion mass spectrometry，SIMS)分析 36
3-5-2 拉曼光譜學(Raman spectroscopy)分析 37
3-5-3 UV-vis分析 38
3-6 光電化學量測 39
3-6-1 光電極薄膜製備 39
3-6-2 光電流量測 39
3-6-3 霍爾量測 (Hall Effect Measurement) 40
3-6-4 開環電位法(Open Circuit Potential，OCP) 40
3-6-5 電化學阻抗頻譜（Electrochemistry Impedance Spectroscopy，EIS） 41
第四章結果與討論 43
4-1 超音波輔助化學水浴法製備AgInS2 43
4-2 晶型結構與表面型態分析 45
4-2-1 X光繞射(X-ray Diffraction，XRD)分析 45
4-2-2 掃描式電子顯微鏡(Scanning Electron Microscope，SEM)分析 46
4-3 元素分析 55
4-3-1 SIMS分析 55
4-3-2 拉曼光譜學(Raman spectroscopy)分析 58
4-4 光電化學測量與分析 59
4-5 UV-vis分析及霍爾量測分析 62
4-6 開環電位分析及電化學阻抗分析 65
4-6-1 開環電位分析 65
4-6-2 電化學阻抗分析 66
第五章結論與未來展望 85
參考文獻 86
附錄 90

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指導教授

李岱洲(Tai-Chou Lee)

審核日期

2013-7-29

推文