School of Chemistry, University of Bristol, Cantocks Close, Bristol BS81TS, UK.
Langmuir. 2010 May 18;26(10):6989-94. doi: 10.1021/la904225k.
Reversed-micelle synthesis has been used to generate CTAB-stabilized gold (Au-NPs) and silver nanoparticles (Ag-NPs). By inducing a phase transition and subsequent separation of the background supporting microemulsion, it has been possible to extract and purify the NPs from the reaction medium. After addition of excess water, the NPs concentrate into an upper octane-rich phase, with impurities and reaction debris (in particular CTAB) partitioning into the water-rich lower phase. UV and (1)H NMR showed that 82% of the original mass of Au-NPs can be purified from the excess CTAB and other salt impurities. The concentrated and purified NPs can be dried down, by solvent removal, and then redispersed in octane. Using the complementary techniques small-angle neutron and X-ray scattering (SANS and SAXS), the structures of microemulsions both with and without nanoparticles prior to separation, and in both upper and lower phases after separation, have been elucidated. The approach has also been applied to the synthesis and recovery of silver nanoparticles, but on a larger scale. This new approach compares favorably with existing methods as it uses no additional organic solvents, has a low-energy demand, and requires no specialist surfactants. The new advance here is that by using a colloidal system to prepare and support the nanoparticles as a structured solvent, a simple soft purification method becomes accessible, which is otherwise impossible with a normal molecular solvent.
反胶束合成已被用于生成 CTAB 稳定的金(Au-NPs)和银纳米粒子(Ag-NPs)。通过诱导相转变和随后分离背景支撑的微乳液,可以从反应介质中提取和纯化纳米粒子。加入过量水后,纳米粒子浓缩到富含辛烷的上层相中,杂质和反应残渣(特别是 CTAB)分配到富含水的下层相中。UV 和(1)H NMR 表明,82%的原始 Au-NPs 质量可以从过量的 CTAB 和其他盐杂质中纯化出来。浓缩和纯化的纳米粒子可以通过溶剂去除干燥,然后重新分散在辛烷中。使用互补的小角中子和 X 射线散射(SANS 和 SAXS)技术,阐明了在分离之前以及在分离之后的上层相和下层相中的纳米粒子存在和不存在的微乳液的结构。该方法也已应用于银纳米粒子的合成和回收,但规模更大。与现有的方法相比,这种新方法具有以下优点:不使用额外的有机溶剂,能耗低,不需要专用表面活性剂。这里的新进展是,通过使用胶体体系来制备和支撑纳米粒子作为结构化溶剂,可以使用一种简单的软纯化方法,否则使用普通的分子溶剂是不可能的。