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研究生:曾泓傑
研究生(外文):Hong-Jie Tseng
論文名稱:鋯鈦酸鉛薄膜沉基在不同基板上之研究
論文名稱(外文):Microfabrication of Thin-Film PZT on Ti/Pt and SiNx Layers
指導教授:吳嘉哲
學位類別:碩士
校院名稱:國立中興大學
系所名稱:機械工程學系所
學門:工程學門
學類:機械工程學類
論文種類:學術論文
畢業學年度:96
語文別:中文
論文頁數:69
中文關鍵詞:鋯鈦酸鉛薄膜溶膠凝膠製程退火白金基板未退火白金基板氮化矽基板焦化處理微制動器微感測器
外文關鍵詞:PZT thin filmsol-gel processannealed Pt substratenonannealed Pt substrateSiNx subatratepyrolysis processmicro-actuatormicro-sensor
相關次數:
  • 被引用被引用:5
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  • 收藏至我的研究室書目清單書目收藏:1
近幾年來,利用鋯鈦酸鉛(PZT)薄膜所發展的微制動器與微感測器受到極大重視。鋯鈦酸鉛薄膜微制動器與微感測器具有廣大的頻寬,大的驅動力、快的反應時間,微小的體積和極高的靈敏度。文獻上常見的PZT薄膜常沉積於單一基板上。如果能將PZT薄膜沉積在不同基板上將可增加薄膜之應用性。另外將PZT薄膜應用於微制動器與微感測器上將需要大面積、無缺陷、品質良好的PZT薄膜。本論文利用不同的前處理和燒結方法將PZT薄膜沉積於退火、未退火白金基板及氮化矽基板上,之後並對沉積的PZT薄膜作表面觀察及特性量測。表面觀察分別利用光學顯微鏡對薄膜表面做巨觀觀測,利用場發射電子顯微鏡對薄膜表面微觀觀測。特性量測分別利用XRD來檢測薄膜之結晶性,和電滯曲線來檢測薄膜之鐵電特性。
本論文將鋯鈦酸鉛薄膜沉積在退火白金基板上,其中最重要的製程參數為如何控制白金退火後之表面孔洞。將薄膜沉積於基板上之後,使用XRD檢測結晶性。第一層燒結後的薄膜已經有很好的鈣鈦礦結晶。電滯曲線量測方面其電極為2mm×2mm,施加最大電場70kV/cm,殘留極化量約7.81μC/cm2,矯頑電場約194kV/cm。而LCR量測中薄膜電容值為29.4nF漏電流僅0.025,介電常數為553,由以上量測可得沉積的PZT薄膜具良好的特性。
本論文也將沉積鋯鈦酸鉛薄膜沉積到未退火白金基板上,其中有兩個重要的製程參數;分別為白金表面改質和薄膜表面焦化處理。有效的控制這兩個參數可以沉積表面品質良好的PZT薄膜。電滯曲線量測方面其電極為2mm×2mm,其在施加最大電場70 kV/cm時殘留極化量約34.9μC/cm2,矯頑電場約221 kV/cm。而LCR量測中薄膜電容值為41.65nF而漏電流僅0.05。
本論文最後也將鋯鈦酸鉛薄膜沉積在氮化矽基板上,其中有四個重要的製程參數;分別為控制溶膠成份、焦化溫度、焦化時間及燒結流程。選用的溶膠成份中採原溶膠增加甘油量至20ml、乙二醇量至10ml。焦化溫度採用540度,在有機物揮發及分解溫度。焦化時間選用5分鐘以上,使有機物能徹底揮發及分解。燒結流程採用三個燒結溫度為620度、640度及650度燒結時間為5分鍾。使用XRD檢測薄膜之結晶性,發現PZT薄膜具有很好的鈣鈦礦結晶。
Recently, Lead Zirconate Titanate Oxide (PZT) thin film actuators and sensors have received increasing attention because of their high frequency bandwidth, large actuation strength, fast response, small size and high sensitivity. To fabricate PZT thin film, one of the most promising techniques is sol-gel process. Although recipes to fabricate sol-gel derived PZT film have long been available in the literature, critical parameters to fabricate high yield, good quality and large crack-free-area PZT film have not been identified and reported. Also, how to fabricate sol-gel derived PZT film on different substrates for various application have not been studied. In this these, we present a systematic approach to identify those critical parameters which affects film’s quality on different substrates. The film’s quality is characterized by optical microscope, field emission scanning electron microscope (FESEM), X-ray diffraction (XRD), precision materials analyzer for P-E hysteresis loop, LCR meter.
Specifically, three goals have been achieved. The first goal is to fabricate PZT thin film on annealed Pt/Ti/SiNx/SiO2/Si substrate. Experimental results show that suitable and uniform microstructures on the Pt layers after annealing can significantly affect the quality of PZT films. In XRD measurement, the intensity of PZT<101><110> could reach 450 for one-layer PZT film, and 880 for three-layer PZT film. In the P-E hysteresis measurement, the saturation poling field is 700kV/cm. Remnant polarization is 7.8μc/cm2 and coercive field is 194kV/cm. In the LCR measurement, the capacitance of PZT film is 29.4nF. Dielectric loss is just 0.025.
The second goal is to fabricate PZT thin film on nonannealed Pt/Ti/SiNx/SiO2/Si substrate. Experimental results show that surface energy on Pt layer and contraction strain of PZT film can significantly affect the quality of PZT films. In XRD measurement, the intensity of PZT<101><110> could reach 590 for one-layer PZT film, and 990 for three-layer PZT film. In the P-E hysteresis measurement, the saturation poling field is 700kV/cm. Remnant polarization is 34.9μc/cm2 and coercive field is 22kV/cm. In the LCR measurement, the capacitance of PZT film is 41.7nF. Dielectric loss is just 0.05.
The third goal is to fabricate PZT thin film on SiNx/SiO2/Si subatrate. Experimental results show components of sol, temperature and time of pyrolysis process, and procedure of sintering process can significantly affect the quality of PZT films. The PZT sol for SiNx/SiO2/Si subatrate is adopted from original sol added 20ml glycerol and 10ml ethylene glycol. The temperature of pyrolysis is chosen 540℃. The time of pryolysis lasts more than 5 minutes to evaporate and decompose organic solvent. Sinetring process is rapid thermal sintering at 620℃ 5 minutes, cool down, rapid thermal sintering at 640℃ 5 minutes, cool down and 650℃ 5 minutes. In XRD measurement, the intensity of PZT<101><110> could reach 750 for three-layer PZT film.
致謝 I
摘要 II
Abstract IV
目錄 VI
圖目錄 VIII
表目錄 X
第一章 前言 1
1-1研究動機與文獻回顧 1
第二章 簡介溶膠凝膠技術 8
2-1 溶膠-凝膠技術 8
2-2 鋯鈦酸鉛薄膜製程 11
2-2-1 溶膠調配 12
2-2-2 基板製備 13
2-2-3 薄膜旋度 14
2-2-4 燒結製程 15
2-3 薄膜性質量測 15
2-3-1 薄膜巨觀表面觀察 15
2-3-3 薄膜結晶性檢測 15
2-3-4 鐵電滯曲線量測 16
2-3-5 電容、阻抗量測 16
第三章 沉積鋯鈦酸鉛薄膜於白金基板 17
3-1 退火白金基板 17
3-1-1 白金退火 17
3-1-2 薄膜表面型態 20
3-1-3 鋯鈦酸鉛薄膜結晶性檢測 21
3-1-4 鋯鈦酸鉛薄膜表、側面觀測 23
3-1-5 鋯鈦酸鉛薄膜特性量測 24
3-2 未退火白金基板 26
3-2-1 白金基板親、疏水性檢測 26
3-2-2 薄膜焦化、燒結製程 28
3-2-3 鋯鈦酸鉛薄膜結晶性檢測 33
3-2-4 鋯鈦酸鉛薄膜表、側面觀測 35
3-2-5 鋯鈦酸鉛薄膜特性量測 37
第四章 沉積鋯鈦酸鉛薄膜於氮化矽基板 39
4-1 溼度影響 40
4-2 溶液成份分析 45
4-3 薄膜焦化、燒結製程 50
4-4 鋯鈦酸鉛薄膜結晶性檢測 59
4-5 鋯鈦酸鉛薄膜表、側面觀測 62
第五章 結論與未來展望 64
5-1 結論 64
5-2 未來展望 65
參考文獻 66
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