题名模板法制备空心结构金属氧化物材料及其表征
作者俞凌杰
学位类别硕士
答辩日期2008-05-27
授予单位中国科学院过程工程研究所
授予地点过程工程研究所
导师袁方利
关键词模板法 空心 金属氧化物 制备
其他题名Preparation and Characterization of Hollow Structure Metal Oxide through Template Method
学位专业化学工程
中文摘要空心结构金属氧化物材料由于其特殊的结构和优异的电、磁等性能,使得它在催化、气体传感、生物医药等领域有着广泛的应用前景。模板法作为一种有效的方法已被广泛应用到空心结构材料的制备中。本论文利用模板法开展了Fe3O4空心结构微球和单晶空心八面体Co3O4材料的制备研究。首先,本论文利用乙二醇为溶剂热反应介质,以六水合氯化铁和无水乙酸铵为反应物,成功制备出Fe3O4空心结构微球,并利用XRD、SEM、TEM和VSM等手段对产物的结构、形貌和磁性能进行了表征。结果表明,所得Fe3O4空心微球尺寸约为400nm且形貌均匀,分散性好。系统研究了反应温度、反应物浓度、不同表面活性剂和不同无机铵盐等参数对产物的影响,提出了气泡模板辅助的Ostwald熟化法一步制备Fe3O4空心结构微球的机理。本实验所采用的方法既避免了传统的软模板法中采用大量有机表面活性剂作为胶束模板而容易造成环境污染的缺点,同时又克服了单独依靠Ostwald熟化过程所需反应时间长的不足,而利用无机铵盐原位产生的氨气气泡为模板并结合Ostwald熟化机理,是一种相对简捷环保的途径。在此基础上,又将此方法进一步推广到铁氧体材料的制备中,成功得到了MFe2O4(M=Mn,Co,Zn)三种空心微球。 另外,本论文还进一步沿用胶体碳球硬模板法,利用碳球在CoCl2溶液中的吸附及煅烧工艺制备了单晶空心八面体结构的Co3O4材料,研究了CoCl2溶液浓度、不同钴盐、不同溶剂体系等参数对产物形貌的影响,进一步发现了吸附的Cl-离子对Co3O4产物形貌所起的关键作用。
英文摘要Metal oxides with hollow structure have extensive potential applications in catalysis, gas sensors and biomedical fields due to their peculiar structure and excellent electronic and magnetic properties. Template method as one of the effective approach has been widely used in the preparation of hollow structure materials. In this paper, Fe3O4 hollow microspheres and Co3O4 single-crystal hollow octahedral materials were prepared by template method. First, Fe3O4 hollow microspheres were successfully obtained in the glycol solvothermal medium using FeCl3•6H2O and NH4Ac as reactants. XRD, SEM, TEM and VSM were employed to characterize the structure, morphology and magnetic property of the as-synthesized Fe3O4 hollow microspheres. The results showed that the product has uniform morphology and good dispersion with the size of approximately 400nm. Following the study on the effects of temperature, concentration, different surfactants and ammonium salts, the mechanism of bubble-assist Ostwald ripening to prepare Fe3O4 hollow microspheres by one step was proposed. Compared to conventional soft template method, this approach avoided using a mass of organic surfactants and overcame the disadvantage of long time only by Ostwald ripening process. It employs bubbles generated in situ as template combined with Ostwald ripening process and is considered as one of the relative green and simple route which was also extended to obtain MFe2O4(M=Mn,Co,Zn)hollow microspheres. Furthermore, Co3O4 single-crystal hollow octahedral materials were also prepared by calcination of colloidal carbon spheres after adsorption in CoCl2 solution. The effects of concentration, different cobalt salts and solvent were studied, and the key role of the Cl- anion on the morphology of product was further discovered.
语种中文
公开日期2013-09-13
页码87
内容类型学位论文
源URL[http://ir.ipe.ac.cn/handle/122111/1214]  
专题过程工程研究所_研究所(批量导入)
推荐引用方式
GB/T 7714
俞凌杰. 模板法制备空心结构金属氧化物材料及其表征[D]. 过程工程研究所. 中国科学院过程工程研究所. 2008.
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