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Sol-gel synthesis of mesoporous assembly of Nd_2O_3 nanocrystals with the aid of structure-directing surfactant

机译:结构导向表面活性剂的溶胶-凝胶法合成Nd_2O_3纳米晶的介孔组装

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The aim of this work was to demonstrate a simple route to synthesize mesoporous assembly of nanocrystalline neodymium oxide (Nd_2O_3) with predominant pore size distribution in the mesopore region, which was successfully done for the first time under mild conditions by a modified sol-gel process with the aid of structure-directing surfactant. Properly manipulated hydrolysis and condensation steps of neodymium n-butoxide modified with acetylacetone in the presence of laurylamine hydrochloride surfactant aqueous solution were performed to obtain the assembled Nd_2O_3 nanocrystal. Various techniques, including thermogravimetric and differential thermal analyses (TG-DTA), X-ray diffraction (XRD), N_2 adsorption-desorption, Brunauer-Emmett-Teller (BET) surface area analysis, Barrett-Joyner-Halenda (BJH) pore size distribution analysis, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected-area electron diffraction (SAED), were used to characterize the synthesized Nd_2O_3 nanocrystal. The N_2 adsorption-desorption isotherm of the synthesized Nd_2O_3 nanocrystal calcined at 500 deg C exhibited single hysteresis loop with IUPAC type IV-like pattern, indicating the existence of foremost mesopore. BJH pore size distribution result revealed that the synthesized Nd_2O_3 nanocrystals possessed mostly mesopore due to their assembly with a small extent of macropore, resulting in very small mean pore diameter in the mesopore region. The particle size determined from both SEM and TEM micrographs was also extremely small of approximately 10 nm.
机译:这项工作的目的是证明一种简单的方法来合成介孔组装的纳米晶氧化钕(Nd_2O_3),其在介孔区域具有主要的孔径分布,这是通过改良的溶胶-凝胶工艺在温和条件下首次成功完成的。借助结构导向表面活性剂。在月桂胺盐酸盐表面活性剂水溶液存在下,对乙酰丙酮改性的正丁醇钕进行适当的水解和缩合步骤,得到组装好的Nd_2O_3纳米晶。各种技术,包括热重分析和差热分析(​​TG-DTA),X射线衍射(XRD),N_2吸附-解吸,Brunauer-Emmett-Teller(BET)表面积分析,Barrett-Joyner-Halenda(BJH)孔径分布分析,扫描电子显微镜(SEM),透射电子显微镜(TEM)和选择区域电子衍射(SAED)用来表征合成的Nd_2O_3纳米晶体。在500℃煅烧的合成Nd_2O_3纳米晶体的N_2吸附-解吸等温线表现出具有IUPAC IV型图案的单滞后回线,表明存在最重要的中孔。 BJH孔径分布结果表明,合成的Nd_2O_3纳米晶体由于具有大孔程度的组装而大部分具有中孔,导致中孔区域的平均孔径很小。由SEM和TEM显微照片确定的粒度也非常小,约为10nm。

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