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低温合成纯立方相 ZrO2 纳米粉体:结构与发光性能研究。

Low temperature synthesis of pure cubic ZrO2 nanopowder: structural and luminescence studies.

机构信息

Bharathiar University, Coimbatore 641 046, India; Department of Physics, Government Arts College, Udumalpet 642 126, India.

Department of Chemistry, M.S. Ramaiah Institute of Technology, Bangalore 560 054, India.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2014 Mar 25;122:216-22. doi: 10.1016/j.saa.2013.11.043. Epub 2013 Nov 16.

DOI:10.1016/j.saa.2013.11.043
PMID:24317256
Abstract

Pure cubic zirconia (ZrO2) nanopowder is prepared for the first time by simple low temperature solution combustion method without calcination. The product is characterized by Powder X-ray Diffraction (PXRD), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Fourier Transform Infra Red spectroscopy (FTIR) and Ultraviolet-Visible spectroscopy (UV-Vis). The PXRD showed the formation of pure stable cubic ZrO2 nanopowders with average crystallite size ranging from 6 to 12 nm. The lattice parameters were calculated from Rietveld refinement method. SEM micrograph shows fluffy, mesoporous, agglomerated particles with large number of voids. TEM micrograph shows honey comb like arrangement of particles with particle size ∼10 nm. The PL emission spectrum excited at 210 nm and 240 nm consists of intense bands centered at ∼365 and ∼390 nm. Both the samples show shoulder peak at ∼420 nm, along with four weak emission bands at ∼484, ∼528, ∼614 and ∼726 nm. TL studies were carried out pre-irradiating samples with γ-rays ranging from 1 to 5 KGy at room temperature. A well resolved glow peak at 377 °C is recorded which can be ascribed to deep traps. With increase in γ radiation there is linear increase in TL intensity which shows the possible use of ZrO2 as dosimetric material.

摘要

首次通过简单的低温溶液燃烧法制备了纯立方氧化锆(ZrO2)纳米粉末,无需煅烧。该产品采用粉末 X 射线衍射(PXRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、傅里叶变换红外光谱(FTIR)和紫外可见光谱(UV-Vis)进行了表征。PXRD 表明形成了纯稳定的立方 ZrO2 纳米粉末,平均晶粒尺寸在 6 至 12nm 之间。晶格参数通过 Rietveld 精修法计算得出。SEM 显微照片显示出蓬松、中孔、团聚的颗粒,具有大量的空隙。TEM 显微照片显示出颗粒呈蜂窝状排列,粒径约为 10nm。在 210nm 和 240nm 激发下的 PL 发射光谱由中心在约 365nm 和约 390nm 的强带组成。两个样品均在约 420nm 处出现肩峰,同时在约 484nm、528nm、614nm 和 726nm 处出现四个较弱的发射带。在室温下用 γ 射线对样品进行 1 至 5KGy 的预辐照后进行了 TL 研究。记录到在 377°C 处有一个很好分辨的发光峰,可归因于深陷阱。随着 γ 辐射的增加,TL 强度呈线性增加,这表明 ZrO2 可能作为剂量计材料使用。

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