用原位电镜技术研究银纳米线与硫溶液的液相反应机理
收稿日期: 2016-10-24
网络出版日期: 2016-12-05
基金资助
项目受国家自然科学基金（No.21433013）和中国科学院国际合作局对外合作重点项目（No.121E32KYSB20150004）资助.
In-situ TEM Study of the Liquid-Phase Reaction of Ag Nanowires with a Sulfur Solution
Received date: 2016-10-24
Online published: 2016-12-05
Supported by
Project supported by the National Natural Science Foundation of China (No. 21433013) and the CAS-DOE Joint Research Program (No. 121E32KYSB20150004).
荣根兰 , 张心怡 , 胥燕 , 张跃钢 . 用原位电镜技术研究银纳米线与硫溶液的液相反应机理[J]. 化学学报, 2016 , 74(12) : 980 -983 . DOI: 10.6023/A16100562
Using transmission electron microscopy (TEM) to directly observe a dynamic chemical reaction process in liquid-phase environment is a big challenge because it is difficult to keep liquid reactants under vacuum.In this work,we reported a liquid-based cell that enables in-situ observation of a solution reaction process under TEM.The novel liquid cell design not only realizes the self-alignment of top/bottom windows,but also achieves an adjustable liquid layer thickness down to nanometer scale.The cell consists of top and bottom frames,both of which are fabricated from silicon wafers using conventional micro-fabrication techniques.The transparent observation windows are made of silicon nitride (SiNx) membranes.In a typical assembling process,an ethanol solution containing silver nanowires and an ethanol solution containing saturated sulfur were sequentially dropped into the liquid tank of the bottom-frame of a liquid cell by using 1 mL syringe.Then,the liquid tank was covered by the top-frame with a window direction of 90 degrees,and an epoxy was used to seal the edge between the top-frame and bottom-frame.Using this assembled liquid cell,we performed in-situ TEM observation of the chemical reaction between Ag nanowires and sulfur in ethanol solution.Additional ex-situ X-ray diffraction (XRD) and Raman spectroscopy were also performed to study the reaction intermediates and final products.Instead of a simple reaction process in which sulfur diffuses into Ag to form the final product of Ag2S,we found that the real reaction process involves the formation of a soluble intermediate phase (Ag2S4),which led to a partial dissolution of Ag nanowires in ethanol solution during reaction.These results well demonstrate that the in-situ TEM technique is a powerful tool to reveal the "real" chemical reaction mechanism.The experimental technique developed here could also be used to study a broad range of dynamic phenomena in liquid environment.
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