本文關(guān)鍵詞： 納米氧化銦 薄膜 八面體結(jié)構(gòu) 氣敏性 光解水　出處：《濟(jì)南大學(xué)》2015年碩士論文　論文類型：學(xué)位論文

【摘要】：氧化銦作為一種重要的n型半導(dǎo)體材料,具有2.8-3.6電子伏特的帶隙,被廣泛應(yīng)用在氣體傳感器,光電器件,太陽(yáng)能轉(zhuǎn)換等領(lǐng)域。近年來(lái),低維氧化銦納米結(jié)構(gòu),如納米線、納米棒、納米帶等,多有報(bào)道,而作為一種有望在氣敏、場(chǎng)發(fā)射等領(lǐng)域有重要應(yīng)用的八面體結(jié)構(gòu)的氧化銦,其報(bào)道的較少,且僅有的報(bào)道其合成方法主要為化學(xué)氣相沉積法。本文著重研究如何通過(guò)溫和的液相化學(xué)路線來(lái)制備八面體結(jié)構(gòu)的氧化銦,并通過(guò)調(diào)控其微觀結(jié)構(gòu),進(jìn)一步研究材料結(jié)構(gòu)和性質(zhì)之間的關(guān)系。主要的研究?jī)?nèi)容如下:1.基于普通玻璃基片的氧化銦八面體薄膜的制備及其氣敏性質(zhì)研究通過(guò)溶膠凝膠法在普通的載玻片上制備納米氧化銦薄膜。實(shí)驗(yàn)探討了原材料氯化銦(InCl3·4H2O)、溶劑冰醋酸(C2H5COOH)以及添加劑乙二醇(HOC2H4OH)和檸檬酸(C6H8O7·H2O)用量對(duì)溶膠質(zhì)量的影響,得到優(yōu)化條件,即當(dāng)In Cl3·4H2O為8.0 g,乙酸為10 mL,乙二醇為2 mL,乙醇為5 mL,水為3 mL,檸檬酸為1.2 g,低溫回流時(shí)間為2.5 h時(shí),所得溶膠其粘度適合制膜。之后分別采用提拉法和旋涂法制膜。對(duì)溶膠以90 mm·min-1的提拉速度得到凝膠膜,然后在500?C下退火4小時(shí)得到微觀結(jié)構(gòu)為納米片的氧化銦薄膜;調(diào)節(jié)旋涂參數(shù),使低轉(zhuǎn)速為5000 rpm,時(shí)間為50 s,高轉(zhuǎn)速為6500 rpm,時(shí)間為20 s進(jìn)行旋涂,再在500?C下退火4 h得到微觀結(jié)構(gòu)為八面體的氧化銦薄膜。把兩種氧化銦薄膜制成氣敏傳感器,在室溫下分別測(cè)試了其對(duì)二氧化氮?dú)怏w的響應(yīng)。實(shí)驗(yàn)發(fā)現(xiàn),相較于片狀結(jié)構(gòu)的氧化銦薄膜,八面體結(jié)構(gòu)的氧化銦薄膜對(duì)二氧化氮?dú)怏w有更高的靈敏度和分辨率,檢測(cè)限達(dá)到了100 ppb;此外,氣敏選擇性實(shí)驗(yàn)表明,相較于其它常見的毒性氣體,如CO、NH3和H2等,器件對(duì)二氧化氮具有良好的氣敏選擇性。2.基于FTO基片的摻氮氧化銦八面體結(jié)構(gòu)薄膜的制備及其光解水性能研究薄膜采用上述的旋涂工藝進(jìn)行制備。所用溶膠與上述溶膠基本相同,只是在其中添加了0.08 g的尿素。采用轉(zhuǎn)速4500 rpm下旋涂50 s和隨后高轉(zhuǎn)速5000 rpm下旋涂20 s的工藝制得凝膠薄膜,然后經(jīng)過(guò)500退火處理4小時(shí),在FTO基片上得到氧化銦八面體納米晶薄膜。作為對(duì)比,在FTO上用同樣工藝制備了不摻氮的薄膜,即所用溶膠未添加尿素。以所制得的摻氮氧化銦八面體納米晶薄膜為工作電極進(jìn)行了光電化學(xué)分解水的實(shí)驗(yàn)。實(shí)驗(yàn)發(fā)現(xiàn),在光強(qiáng)為一個(gè)太陽(yáng)的模擬太陽(yáng)光的照射下,摻氮改性后的八面體光解水的光電流可達(dá)到0.17 mA·cm-2,在實(shí)驗(yàn)的30 min內(nèi)穩(wěn)定,沒有明顯的衰減;而未摻氮的光電流只有0.03 mA·cm-2。
[Abstract]:As an important n-type semiconductor material, indium oxide has a band gap of 2.8-3.6 electron volts. It has been widely used in gas sensors, photovoltaic devices, solar energy conversion and other fields. In recent years, low-dimensional indium oxide nanostructures, such as nanowires, have been widely used. Nanorods, nanobelts, etc., are mostly reported. However, as a kind of indium oxide, which is expected to have important applications in gas sensing, field emission and other fields, there are few reports of indium oxide. The only reported method of synthesis is chemical vapor deposition. This paper focuses on the preparation of indium oxide with octahedron structure through a mild liquid chemical route, and regulates its microstructure. The main research contents are as follows: 1. Preparation and gas sensing properties of indium oxide octahedron thin films based on ordinary glass substrates. The effects of raw material indium chloride (InCl _ 3 路4H _ 2O), solvent glacial acetic acid (C _ 2H _ 5COOH), as well as additives ethylene glycol (HEC _ 2H _ 4OH) and citrate (C _ 6H _ 8O _ 7 路H _ 2O) on the sol quality were investigated. When in Cl3 路4H 2O was 8.0g, acetic acid was 10 mL, ethylene glycol was 2 mL, ethanol was 5 mL, water was 3 mL, citric acid was 1.2g, reflux time at low temperature was 2.5h. The viscosity of the obtained sol is suitable for film preparation. Then the film is prepared by Czochralski method and spin-coating method respectively. The gel film is obtained at the Czochralski rate of 90 mm 路min-1 for the sol, and then the gel film is obtained at 500 mm 路min-1. After annealing for 4 hours under C, indium oxide thin films with nano-structure were obtained by adjusting the spin-coating parameters to make low rotation speed 5000 rpm, time 50 s, high rotation speed 6500 rpm, time 20 s, and then spin coating at 500s? Indium oxide thin films with octahedron structure were obtained by annealing at C for 4 h. Two indium oxide thin films were made into gas sensors and their responses to nitrogen dioxide gas were measured at room temperature. Compared with indium oxide thin films with sheet structure, indium oxide thin films with octahedron structure have higher sensitivity and resolution to nitrogen dioxide gas, and the detection limit reaches 100 ppb. Compared with other common toxic gases, such as COG NH 3 and H 2, The device has good gas sensitivity selectivity to nitrogen dioxide. 2. Preparation and photolysis properties of indium oxide octahedron structure films based on FTO substrates; thin films prepared by the above spin-coating process. The sol is basically the same, Only 0.08 g urea was added to the gel film. The gel film was prepared by spinning 50 s under rotating speed of 4 500 rpm and 20 s at high speed of 5 000 rpm. The film was then annealed for 4 hours. Indium oxide octahedral nanocrystalline thin films were prepared on FTO substrates. Using the prepared indium oxide octahedron nanocrystalline film as the working electrode, the photochemical decomposition of water was carried out. It was found that the photochemical decomposition of water was carried out when the light intensity was simulated by the sun. The photocurrent of nitrogen-doped octahedron photodissociated water can reach 0.17 Ma 路cm ~ (-2), which is stable and has no obvious attenuation within 30 min of experiment, but the photocurrent without nitrogen doping is only 0.03 Ma 路cm ~ (-2).
【學(xué)位授予單位】：濟(jì)南大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TQ133.53;TB383.2

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本文編號(hào)：1504124