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Single crystal particles of mesoporous (Nb, Ta)_2O_5

机译:中孔(Nb,Ta)_2O_5的单晶颗粒

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Mesoporous Nb-Ta mixed oxide, (Nb, Ta)_2O_5, with whormhole mesopore structure was prepared by using a block co-polymer template and metal chlorides in ethanol. The mesoporous (Nb, Ta)_2O_5 calcined at 673 K for 20 h showed 140 m~2·g~(-1) of BET surface area and 3.0 nm of pore size. The amorphous wall of the mesoporous (Nb, Ta)_2O_5 was crystallized by further calcination at 923 K for 1 h. The BET surface area and pore size estimated by N_2 adsorption isotherm of the crystallized (Nb, Ta)_2O_5 were 48 m~2·g~(-1) and 10.0 nm, respectively. Detailed analysis of transmission electron microscope (TEM) and electron diffraction (ED) revealed that each particle of sub-micron size was a mesoporous single crystal. The pore size and crystallinity observed by TEM were in good agreement with N_2 adsorption-desorption isotherms and powder X-ray diffraction patterns. Similar mesoporous (Nb, Ta)_2O_5 single crystal particles were also obtained by using amorphous precursor prepared by ligand-assisted templating method. Therefore, mixing two similar elements, Nb and Ta, is suspected to be beneficial for crystallization with sustaining the mesoporores.
机译:利用嵌段共聚物模板和乙醇中的金属氯化物制备了具有孔洞中孔结构的介孔Nb-Ta混合氧化物(Nb,Ta)_2O_5。在673 K下煅烧20 h的中孔(Nb,Ta)_2O_5的BET表面积为140 m〜2·g〜(-1),孔径为3.0 nm。通过在923 K下进一步煅烧1 h,使中孔(Nb,Ta)_2O_5的非晶壁结晶。通过结晶的(Nb,Ta)_2O_5的N_2吸附等温线估算的BET表面积和孔径分别为48 m〜2·g〜(-1)和10.0 nm。透射电子显微镜(TEM)和电子衍射(ED)的详细分析表明,每个亚微米尺寸的颗粒都是中孔单晶。 TEM观察到的孔径和结晶度与N_2吸附-解吸等温线和粉末X射线衍射图谱吻合良好。使用配体辅助模板法制备的非晶态前驱体,也获得了类似的中孔(Nb,Ta)_2O_5单晶颗粒。因此,怀疑将两种相似的元素Nb和Ta混合有利于维持介孔的结晶。

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