Research Institute for Science and Technology, Tokyo University of Science, 2641 Yamazaki, Noda, Chiba 278-8510, Japan.
Nanoscale. 2010 Aug;2(8):1441-7. doi: 10.1039/c0nr00141d. Epub 2010 May 26.
This article examines the effect(s) of the 2.45-GHz microwave (MW) radiation in the synthesis of silver nanoparticles in aqueous media by reduction of the diaminesilver(i) complex, Ag(NH(3))(2), with carboxymethylcellulose (CMC) in both batch-type and continuous-flow reactor systems with a particular emphasis on the characteristics of the microwaves in this process and the size distributions. This microwave thermally-assisted synthesis is compared to a conventional heating (CH) method, both requiring a reaction temperature of 100 degrees C to produce the nanoparticles, in both cases leading to the formation of silver colloids with different size distributions. Reduction of the diaminesilver(i) precursor complex, Ag(NH(3))(2), by CMC depended on the solution temperature. Cooling the reactor during the heating process driven with 390-Watt microwaves (MW-390W/Cool protocol) yielded silver nanoparticles with sizes spanning the range 1-2 nm. By contrast, the size distribution of Ag nanoparticles with 170-Watt microwaves (no cooling; MW-170W protocol) was in the range 1.4-3.6 nm (average size approximately 3 nm). The overall results suggest the potential for a scale-up process in the microwave-assisted synthesis of nanoparticles. Based on the present data, a flow-through microwave reactor system is herein proposed for the continuous production of silver nanoparticles. The novel flow reactor system (flow rate, 600 mL min(-1)) coupled to 1200-Watt microwave radiation generated silver nanoparticles with a size distribution 0.7-2.8 nm (average size ca. 1.5 nm).
本文研究了 2.45GHz 微波(MW)辐射在水溶液中通过还原二胺银(I)配合物[Ag(NH3)2]+与羧甲基纤维素(CMC)合成银纳米粒子的影响,该反应在批式和连续流动反应器系统中进行,特别强调了微波在该过程中的特性和尺寸分布。与传统加热(CH)方法相比,这种微波热辅助合成需要 100°C 的反应温度来制备纳米粒子,两种方法都导致形成具有不同尺寸分布的银胶体。还原二胺银(I)前体配合物[Ag(NH3)2]+取决于溶液温度。在 390 瓦特微波(MW-390W/Cool 方案)驱动的加热过程中冷却反应器,得到的银纳米粒子尺寸范围为 1-2nm。相比之下,在 170 瓦特微波(无冷却;MW-170W 方案)下的 Ag 纳米粒子的尺寸分布在 1.4-3.6nm 之间(平均尺寸约为 3nm)。总体结果表明,在微波辅助合成纳米粒子方面具有扩大规模的潜力。基于目前的数据,提出了一种用于连续生产银纳米粒子的微波辅助合成的流动式反应器系统。该新型流动式反应器系统(流速为 600mLmin-1)与 1200 瓦特微波辐射相结合,生成的银纳米粒子尺寸分布为 0.7-2.8nm(平均尺寸约为 1.5nm)。