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一种高效的微波辅助合成方法,用于生产水溶性胺封端的 Si 纳米颗粒。

An efficient microwave-assisted synthesis method for the production of water soluble amine-terminated Si nanoparticles.

机构信息

Department of Chemistry, University of California, One Shields Avenue, Davis, CA 95616, USA.

出版信息

Nanotechnology. 2012 Jul 27;23(29):294006. doi: 10.1088/0957-4484/23/29/294006. Epub 2012 Jun 28.

Abstract

Silicon nanoparticles can be considered a green material, especially when prepared via a microwave-assisted method without the use of highly reactive reducing agents or hydrofluoric acid. A simple solution synthesis of hydrogen-terminated Si- and Mn-doped Si nanoparticles via microwave-assisted synthesis is demonstrated. The reaction of the Zintl salt, Na(4)Si(4), or Mn-doped Na(4)Si(4), Na(4)Si(4(Mn)), with ammonium bromide, NH(4)Br, produces small dispersible nanoparticles along with larger particles that precipitate. Allylamine and 1-amino-10-undecene were reacted with the hydrogen-terminated Si nanoparticles to provide water solubility and stability. A one-pot, single-reaction process and a one-pot, two-step reaction process were investigated. Details of the microwave-assisted process are provided, with the optimal synthesis being the one-pot, two-step reaction procedure and a total time of about 15 min. The nanoparticles were characterized by transmission electron microscopy (TEM), x-ray diffraction, and fluorescence spectroscopies. The microwave-assisted method reliably produces a narrow size distribution of Si nanoparticles in solution.

摘要

硅纳米粒子可以被认为是一种绿色材料,特别是在微波辅助方法下制备时,不使用高反应性的还原剂或氢氟酸。通过微波辅助合成,展示了一种通过简单溶液合成方法制备氢封端的 Si 和 Mn 掺杂的 Si 纳米粒子。Zintl 盐 Na(4)Si(4)或 Mn 掺杂的 Na(4)Si(4)(Na(4)Si(4)(Mn))与溴化铵 NH(4)Br 反应,生成小的可分散纳米粒子以及沉淀的较大颗粒。烯丙胺和 1-氨基-10-十一烯与氢封端的 Si 纳米粒子反应,提供了水溶性和稳定性。研究了一锅单步反应和一锅两步反应过程。提供了微波辅助过程的详细信息,最佳合成是一锅两步反应程序,总时间约为 15 分钟。通过透射电子显微镜 (TEM)、X 射线衍射和荧光光谱对纳米粒子进行了表征。微波辅助方法可靠地在溶液中产生了具有较窄粒径分布的 Si 纳米粒子。

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