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Zr-Ce-SBA-15介孔材料的合成和形貌調(diào)控
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高等學(xué)校科技創(chuàng)新工程重大項(xiàng)目培育資金(708049);高等學(xué)校博士點(diǎn)專項(xiàng)基金(20060288008);江蘇省自然科學(xué)基金(BK2009392)


Synthesis and Morphological Control of Zr-Ce-SBA-15 Mesoporous Materials
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    摘要:

    以正硅酸乙酯(TEOS)為硅源,P123為模板劑,氯化氧鋯(ZrOCl2·8H2O)和硝酸亞鈰(Ce(NO3)3·6H2O)為鋯、鈰前驅(qū)體,在不外加無機(jī)酸的條件下,利用無機(jī)前驅(qū)鹽自身水解產(chǎn)生的弱酸性環(huán)境,水熱法一步合成Zr-Ce-SBA-15介孔材料。通過改變起始物料配比和調(diào)節(jié)合成溫度可以實(shí)現(xiàn)對(duì)產(chǎn)物的形貌進(jìn)行有效控制。利用小角X射線衍射 (LXRD)、透射電子顯微鏡 (TEM)、掃描電子顯微鏡 (SEM)、電感耦合等離子體原子發(fā)射光譜 (ICP-AES)和氮?dú)馕降仁侄螌?duì)所合成的樣品進(jìn)行了表征。結(jié)果表明:在 nZr(Ce):nSi物質(zhì)量的比分別為 0.03,0.05,0.10時(shí),合成的材料具有類似于SBA-15高度有序的二維六方相介孔結(jié)構(gòu),鋯、鈰物種被成功引入SBA-15材料的骨架中。當(dāng)nZr(Ce):nSi摩爾比為0.05,晶化溫度為100 ℃時(shí),Zr-Ce-SBA-15表現(xiàn)為六方板狀形貌。隨著晶化溫度的升高,Zr-Ce-SBA-15的形貌由六方板狀轉(zhuǎn)變成圓盤狀

    Abstract:

    The highly ordered mesoporous materials Zr-Ce-SBA-15 were synthesized by a hydrothermal route using tetraethyl orthosilicate (TEOS) as a silica source, Pluronic P123 as a template, zirconyl chloride and cerous nitrate as precursors under a moderate acidic condition. The main strategy of this method was to utilize the acidity self-generated in the aqueous solutions, where no addition of mineral acids was necessary. Through a simple adjustment of the initial reactant molar ratio in the synthesis gel and the crystallization temperature, the morphology of mesoporous materials could be controlled efficaciously. The as-synthesized materials were characterized by XRD, TEM, SEM, inductively coupled plasma atomic emission spectrometry (ICP-AES) and N2 adsorption. Results indicate that the Zr and Ce species are incorporated into the framework of SBA-15. The obtained Zr-Ce-SBA-15 materials with different nZr(Ce):nSi molar ratios of 0.03, 0.05 and 0.10 possess 2D-hexagonal P6mm mesoporous structure similar to SBA-15. In addition, the morphology of the bimetallic Zr-Ce-SBA-15 mesoporous materials varies with different nZr(Ce):nSi molar ratios and different crystallization temperatures. When the nZr(Ce):nSi ratio is 0.05 and the crystallization temperature 100 oC, the material of Zr-Ce-SBA-15 displays hexagonal-platelet morphology. With increasing of crystallization temperature, the morphology of the bimetallic Zr-Ce-SBA-15 mesoporous materials is changed from hexagonal-platelet to circular-platelet.

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袁金芳,李健生,申戰(zhàn)輝,顧 娟,李慧君,孫秀云,王連軍. Zr-Ce-SBA-15介孔材料的合成和形貌調(diào)控[J].稀有金屬材料與工程,2011,40(3):473~478.[Yuan Jinfang, Li Jiansheng, Shen Zhanhui, Gu Juan, Li Huijun, Sun Xiuyun, Wang Lianjun. Synthesis and Morphological Control of Zr-Ce-SBA-15 Mesoporous Materials[J]. Rare Metal Materials and Engineering,2011,40(3):473~478.]
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  • 收稿日期:2010-03-25
  • 最后修改日期:2010-12-28
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