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高介电常数材料CaCu3Ti4O12纳米晶相的熔盐合成法

Molten salt synthesis of nanocrystalline phase of high dielectric constant material CaCu3Ti4O12.

作者信息

Prakash B Shri, Varma K B R

机构信息

Materials Research Centre, Indian Institute of Science, Bangalore 560012, India.

出版信息

J Nanosci Nanotechnol. 2008 Nov;8(11):5762-9. doi: 10.1166/jnn.2008.213.

Abstract

Nanocrystalline powders of giant dielectric constant material, CaCu3Ti4O12 (CCTO), have been prepared successfully by the molten salt synthesis (MSS) using KCl at 750 degrees C/10 h, which is significantly lower than the calcination temperature (approximately 1000 degrees C) that is employed to obtain phase pure CCTO in the conventional solid-state reaction route. The water washed molten salt synthesized powder, characterized by X-ray powder diffraction (XRD), Scanning electron microscopy (SEM), and Transmission electron microscopy (TEM) confirmed to be a phase pure CCTO associated with approximately 150 nm sized crystallites of nearly spherical shape. The decrease in the formation temperature/duration of CCTO in MSS method was attributed to an increase in the diffusion rate or a decrease in the diffusion length of reacting ions in the molten salt medium. As a consequence of liquid phase sintering, pellets of as-synthesized KCl containing CCTO powder exhibited higher sinterability and grain size than that of KCl free CCTO samples prepared by both MSS method and conventional solid-state reaction route. The grain size and the dielectric constant of KCl containing CCTO ceramics increased with increasing sintering temperature (900 degrees C-1050 degrees C). Indeed the dielectric constants of these ceramics were higher than that of KCl free CCTO samples prepared by both MSS method and those obtained via the solid-state reaction route and sintered at the same temperature. Internal barrier layer capacitance (IBLC) model was invoked to correlate the observed dielectric constant with the grain size in these samples.

摘要

通过在750摄氏度下使用KCl进行10小时的熔盐合成(MSS),成功制备了具有巨大介电常数的材料CaCu3Ti4O12(CCTO)的纳米晶粉末,该温度显著低于传统固态反应路线中用于获得纯相CCTO的煅烧温度(约1000摄氏度)。经水洗的熔盐合成粉末,通过X射线粉末衍射(XRD)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)表征,证实为纯相CCTO,其晶粒尺寸约为150纳米,形状近乎球形。MSS法中CCTO形成温度/持续时间的降低归因于熔盐介质中反应离子扩散速率的增加或扩散长度的减小。由于液相烧结,合成的含KCl的CCTO粉末制成的颗粒比通过MSS法和传统固态反应路线制备的不含KCl的CCTO样品表现出更高的烧结性和更大的晶粒尺寸。含KCl的CCTO陶瓷的晶粒尺寸和介电常数随烧结温度(900摄氏度 - 1050摄氏度)的升高而增加。实际上,这些陶瓷的介电常数高于通过MSS法制备的不含KCl的CCTO样品以及通过固态反应路线制备并在相同温度下烧结的样品。采用内部势垒层电容(IBLC)模型将这些样品中观察到的介电常数与晶粒尺寸相关联。

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