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NiSb纳米颗粒的热液路线制备及电催化析氢性能研究
钱银银,杨 静,李焕然,邢诗琪,杨 晴*
作者单位E-mail
钱银银 中国科学技术大学化学系合肥微尺度物质科学国家实验室合肥 230026  
杨 静 中国科学技术大学化学系合肥微尺度物质科学国家实验室合肥 230026  
李焕然 中国科学技术大学化学系合肥微尺度物质科学国家实验室合肥 230026  
邢诗琪 中国科学技术大学化学系合肥微尺度物质科学国家实验室合肥 230026  
杨 晴* 中国科学技术大学化学系合肥微尺度物质科学国家实验室合肥 230026 qyoung@ustc.edu.cn 
摘要:
本文发展了一种简单经济的过渡金属锑化物热液合成路线,在160 oC的温和条件下,由商业易得的乙酰丙酮基镍和三苯基铋在油胺介质中还原制备出NiSb纳米颗粒. 反应中,还原剂甲硼烷-叔丁基胺络合物的使用能够有效促进金属源的快速还原,用以促进NiSb纳米颗粒的生成. 结构表征显示,所制备的NiSb产物为六方相(空间群P63/mmc)颗粒状纳米晶,其粒径约为10 nm. 该合成方法可拓展用于CoSb和Ag3Sb等纳米颗粒的温和制备. 电催化析氢性能研究显示,NiSb纳米颗粒具有良好的电化学析氢反应性能. 结果显示,当阴极电流密度达到50 mA/cm2和10 mA/cm2时所需要的过电位分别为531和437 mV. 同时,NiSb纳米颗粒还具有较小的电荷转移阻抗和优良的循环稳定性能.
关键词:  热液合成路线,NiSb纳米颗粒,配体交换,电催化析氢反应
DOI:10.1063/1674-0068/cjcp1805113
分类号:
基金项目:
Solution-based Synthesis of NiSb Nanoparticles for Electrochemical Activity in Hydrogen Evolution Reaction
Yin-yin Qian,Jing Yang,Huan-ran Li,Shi-qi Xing,Qing Yang*
Abstract:
A cost-effective, facile solution-based hot-injection synthetic route has been developed to synthesize NiSb nanoparticles in oleylamine (OAm) using commercially available inexpensive precursor with reducing toxicity at a relatively low temperature of 160 oC. Especially, an organic reductant of borane-tert-butylamine complex is intentionally involved in the reaction system to promote a fast reduction of metallic Ni and Sb for the formation of the NiSb nanoparticles. Structural characterizations reveal that the NiSb nanoparticles are hexagonal phase with space group P63/mmc and they are composed of small granules with size about 10 nm that tend to form agglomerates with porous-like geometries. This is the first report on the generation of transition metal antimonide via solution-based strategy, and the asfabricated nanoparticles possess actively electrocatalytic hydrogen evolution reaction (HER) property in acidic electrolytes when the long-chain ligand of OAm adhered on the surface of the nanoparticles is exchanged by ligand-removal and exchange procedure. It is found that the NiSb nanoparticles as a new kind of non-noble-metal HER electrocatalysts only require overpotentials of 437 and 531 mV to achieve high current densities of 10 and 50 mA/cm2 respectively, as well as exhibit low charge transfer resistance and excellent HER stability.
Key words:  Hot-injection synthetic route, NiSb nanoparticles, Ligand-removal and exchange, Hydrogen evolution reaction activity