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一种利用表面活性剂辅助模板溶胶-凝胶法合成介孔Dy2O3纳米晶体的简单路线。

A simple route utilizing surfactant-assisted templating sol-gel process for synthesis of mesoporous Dy2O3 nanocrystal.

作者信息

Sreethawong Thammanoon, Chavadej Sumaeth, Ngamsinlapasathian Supachai, Yoshikawa Susumu

机构信息

The Petroleum and Petrochemical College, Chulalongkorn University, Soi Chula 12, Phyathai Road, Pathumwan, Bangkok 10330, Thailand.

出版信息

J Colloid Interface Sci. 2006 Aug 1;300(1):219-24. doi: 10.1016/j.jcis.2006.03.060. Epub 2006 May 2.

Abstract

A simple route of combined sol-gel process with surfactant-assisted templating technique was successfully employed for the first time to synthesize nanocrystalline mesoporous Dy(2)O(3) with narrow monomodal pore size distribution under mild conditions. The nanocrystalline Dy(2)O(3) with monomodal mesoporous characteristic was ultimately achieved by controlling the hydrolysis and condensation steps of dysprosium n-butoxide modified with acetylacetone in the presence of laurylamine hydrochloride surfactant aqueous solution. The synthesized material was methodically characterized by thermogravimetry and differential thermal analysis (TG-DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), selected-area electron diffraction (SAED), N(2) adsorption-desorption, Brunauer-Emmett-Teller (BET) surface area analysis, and Barrett-Joyner-Halenda (BJH) pore size distribution analysis. The particle size of the synthesized Dy(2)O(3) in nanosized range obtained from the SEM and HRTEM micrographs was in good accordance with the crystallite size estimated from the XRD result. The N(2) adsorption-desorption result exhibited hysteresis pattern with single loop, indicating the existence of monomodal mesopore. The extremely narrow pore size distribution with mean pore diameter in the mesopore region of the synthesized Dy(2)O(3) was also confirmed by the BJH result.

摘要

首次成功采用溶胶 - 凝胶法与表面活性剂辅助模板技术相结合的简单路线,在温和条件下合成了具有窄单峰孔径分布的纳米晶介孔Dy(2)O(3)。通过在月桂胺盐酸盐水溶液存在下控制乙酰丙酮改性的正丁醇镝的水解和缩合步骤,最终获得了具有单峰介孔特征的纳米晶Dy(2)O(3)。通过热重分析和差示热分析(TG - DTA)、X射线衍射(XRD)、扫描电子显微镜(SEM)、高分辨率透射电子显微镜(HRTEM)、选区电子衍射(SAED)、N(2)吸附 - 脱附、Brunauer - Emmett - Teller(BET)表面积分析和Barrett - Joyner - Halenda(BJH)孔径分布分析对合成材料进行了系统表征。从SEM和HRTEM显微照片获得的纳米尺寸范围内合成Dy(2)O(3)的粒径与XRD结果估计的微晶尺寸非常吻合。N(2)吸附 - 脱附结果显示出具有单环的滞后模式,表明存在单峰介孔。BJH结果也证实了合成Dy(2)O(3)在介孔区域平均孔径的极窄孔径分布。

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