水热-热分解法合成系列MCo2O4自组装纳米材料
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上海市自然科学基金资助项目(15ZR1428500)


Hydrothermal and Thermo-Decomposition Synthesis of Self-assembled MCo2O4 Nanomaterial
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    摘要:

    以硝酸钴和二价M (M=Zn2+,Cu2+,Ni2+)盐为原料,草酸盐为沉淀剂,通过水热过程获取MCo2(C2O4)3复合草酸盐中间体,对中间体在400~500 ℃范围内进行热处理2 h,获得自组装的MCo2O4纳米粒子超结构材料.采用热失重(TGA)、 X射线衍射(XRD)和透射电镜(TEM)分析手段,对中间体及目标产品的热稳定性、结晶度、形貌、结构进行表征.结果表明:中间体主要经历脱结晶水和草酸盐热分解两个过程,其热分解温度应高于370 ℃;获得的钴酸盐为纳米粒子的自组装超结构,纳米粒子颗粒细小均匀,粒度在15~30 nm之间;目标产品的形貌、结晶度与样品的本性及助剂的种类存在相关性.

    Abstract:

    Using cobalt salt and M salt (M=Zn2+,Cu2+,Ni2+) as raw material and oxalate as precipitant,a series of mixed oxalate precipitates MCo2(C2O4)3 were prepared as intermediates with a hydrothermal approach.Then these intermediates were pyrolyzed at 400~500 ℃ about 2 hours and finally self-assembled nanoparticles super-structure material of MCo2O4 was achieved.A thermo-gravimetric analyzer (TGA),X-ray diffraction (XRD) device and transmission electron microscopy (TEM) were applied to characterize the heat stability,crystallization,morphology and structure of intermediates and target product.The results show that the thermo-gravimetric process of intermediates includes two stages:the loss of crystal water and the thermo-decomposition of oxalate,and the thermal-decomposition temperature should be set more than 370 ℃.The prepared products are superstructure material assembled by fine and homogeneous polyhedral particles,with the particle size of 15~30 nm.The morphology and crystallization of target product are influenced by the intrinsic properties of samples and the types of additives.

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马杰,季婷婷,贾奎法,侯炎炎.水热-热分解法合成系列MCo2O4自组装纳米材料[J].上海理工大学学报,2015,37(6):520-526.

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  • 收稿日期:2014-09-18
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  • 在线发布日期: 2016-01-07