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十二胺辅助稀土及贵金属纳米材料的水热制备
李成印
学位类型硕士
导师杨军
2016-07
学位授予单位中国科学院研究生院
学位授予地点北京
学位专业化学工程
关键词十二胺 水热 纳米材料 稀土氢氧化物 中空结构
摘要

基于十二胺与金属离子间存在的相互作用,以水热合成方式,探索具有特定形貌的稀土及贵金属基纳米材料的制备途径。本文涵盖纳米材料制备、材料形貌及结构表征、形成机制分析以及相关性能测试。以稀土金属硝酸盐为前驱体,借助十二胺辅助的水热法成功制备了La(OH)3,Nd(OH)3,Pr(OH)3,Sm(OH)3,Gd(OH)3,和Er(OH)3的棒状纳米结构。该制备策略需先于室温下将稀土前驱物的水溶液与十二胺的乙醇溶液混合,然后升温进行水热处理。通过改变水热过程的反应时间及水/乙醇的体积比,探究了水热条件对纳米结构形貌的影响。在相同制备条件下,使用Ce的前驱体时直接得到球形CeO2纳米结构。此外,将所得的稀土氢氧化物在空气中高温焙烧处理,可制得相应的稀土氧化物纳米棒。以AgNO3为前驱体,在室温下先将其与十二胺在水/乙醇的混合溶剂中形成相应的络合前体,然后在加热条件进行水热还原即可制备具有中空结构的Ag纳米颗粒(hAgNPs)。通过多种表征手段对所制备的hAgNPs的结构和化学组成进行了详细分析,同时也对中空结构的可能形成机理进行了推断。以RuCl3和IrCl3·3H2O为前驱体,采用十二胺辅助的水热制备方式成功得到粒径在1~3 nm的超细Ru/Ir纳米颗粒。借助多种手段对Ru/Ir纳米颗粒的化学组成及结构进行了详细表征,并通过改变加入前驱体的量以调控颗粒中Ru/Ir元素的摩尔比。此外,还将碳载型Ru/Ir超细纳米颗粒用作电解水析氧反应(OER)的催化剂,发现当控制Ru/Ir的摩尔比约0.5:0.5时,OER催化过程中同时表现出高的催化活性和稳定性。

其他摘要

Based on the interaction between dodecylamine (DDA) and metal ions, rare earth and noble metal-based nanomaterials with special morphologies, were successfully synthesized via a hydrothermal process. This thesis covers the preparation of nanomaterials, morphology and structure characterization, formation mechanism analysis and related performance tests.Nanosized rare earth (RE) hydroxides including La(OH)3, Nd(OH)3, Pr(OH)3, Sm(OH)3, Gd(OH)3, and Er(OH)3 with rod-like morphology are fabricated via a convenient hydrothermal approach. This strategy calls for the first preparation of metal complexes between RE nitrates and dodecylamine (DDA) in water/ethanol mixture at room temperature and subsequent hydrothermal treatment at elevated temperature. The influence of reaction time and water/ethanol volume ratios on the morphology and size of as-prepared RE hydroxides are investigated. CeO2 nanoparticles with spherical shape could be directly obtained by hydrothermal treatment of complexes formed between Ce precursor and DDA. In addition, by further calcinating the RE hydroxides at high temperature in air, RE oxide nanorods could be readily produced.Hollow structure silver nanoparticles (hAgNPs) were prepared via a hydrothermal method, involving an initial formation of metal complexes from AgNO3 precursors and dodecylamine in a water/ethanol mixture at room temperature and a subsequent reduction in an autoclave at elevated temperature. A number of characterization techniques were used to characterize the structure and chemical composition of the as-formed hAgNPs, and to understand the mechanism behind the formation.Carbon-supported ultrafine nanoparticles, with a mean diameter of 1-3 nm, were synthesized via a DDA-assisted hydrothermal strategy. The strategy is similar to the preparation of hAgNPs, while using RuCl3 and IrCl3·3H2O as precursors. A quantity of characterization techniques was used to characterize the structure and chemical composition of the nanoparticles. The catalytic performance of the synthesized Ru, Ir and Ru-Ir hybrid in the oxygen evolution reaction (OER) were also examined. When the Ru/Ir molar ratio was controlled at 0.5:0.5, the bimetallic catalyst exhibited high OER catalytic activity and stability simultaneously.

语种中文
文献类型学位论文
条目标识符http://ir.ipe.ac.cn/handle/122111/22924
专题研究所(批量导入)
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李成印. 十二胺辅助稀土及贵金属纳米材料的水热制备[D]. 北京. 中国科学院研究生院,2016.
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