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喷雾热解技术合成的TiO₂薄膜的结构与形态表征

Structural and morphological characterization of TiO2 thin films synthesized by spray pyrolysis technique.

作者信息

Raut N C, Mathews Tom, Sundari S Tripura, Sairam T N, Dash S, Tyagi A K

机构信息

Materials Science Division, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102, TN, India.

出版信息

J Nanosci Nanotechnol. 2009 Sep;9(9):5298-302. doi: 10.1166/jnn.2009.1121.

Abstract

Thin films of nanocrystalline TiO2 were synthesized by spray pyrolysis technique in the temperature range 300 degrees C to 550 degrees C in steps of 50 degrees C. The films were coated on glass and quartz substrates by ultrasonic nebulization of titanium-oxy-acetyl acetonate followed by pyrolysis. The structure and morphology of the thin films were characterized by X-ray Diffraction (XRD), Raman Spectroscopy (RS) and Scanning Electron Microscopy (SEM), while the optical band gaps were measured by Spectroscopic Ellipsometry (SE) and UV-Visible spectroscopy. XRD investigations revealed distinct crystal structures of the films synthesized above and below 300 degrees C. While films grown at substrate temperature 300 degrees C were amorphous, those grown at 350 dgrees C and above showed tetragonal anatase crystal structure. The morphological investigations from SEM showed that the films deposited at 350 degrees C were porous and exhibited flower like morphology. The microstructures of the films grown on quartz at 450 degrees C were found to be uniform and dense. The nominal grain sizes evaluated from High Resolution SEM (HRSEM) studies were approximately 20 nm and compared well with the grain sizes calculated from XRD. The band gap values calculated from ellipsometry studies were approximately 3.7 eV and 3.95 eV for the films grown at 450 degrees C and 350 degrees C, respectively. This is in good agreement with those obtained from UV-Visible spectroscopy.

摘要

采用喷雾热解技术,在300℃至550℃的温度范围内,以50℃为步长合成了纳米晶TiO₂薄膜。通过对乙酰丙酮氧钛进行超声雾化,然后热解,将薄膜涂覆在玻璃和石英衬底上。利用X射线衍射(XRD)、拉曼光谱(RS)和扫描电子显微镜(SEM)对薄膜的结构和形貌进行了表征,同时通过光谱椭偏仪(SE)和紫外-可见光谱测量了光学带隙。XRD研究揭示了在300℃以上和以下合成的薄膜具有不同的晶体结构。在衬底温度300℃下生长的薄膜是非晶态的,而在350℃及以上生长的薄膜呈现四方锐钛矿晶体结构。SEM的形貌研究表明,在350℃沉积的薄膜是多孔的,呈现出花状形貌。发现在450℃在石英上生长的薄膜的微观结构均匀且致密。通过高分辨率SEM(HRSEM)研究评估的标称晶粒尺寸约为20nm,与由XRD计算的晶粒尺寸相当。对于在450℃和350℃生长的薄膜,由椭偏仪研究计算得到的带隙值分别约为3.7eV和3.95eV。这与从紫外-可见光谱获得的结果非常吻合。

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