图1：原理示意图      

电化学原位红外光谱分析是红外分析技术的一个重要分支，能够定性分析电催化(如CO2电还原等)反应、各种类型电池(如锂离子、锂硫电池等)充放电过程中电极表面的产物或中间产物随时间(电位)不断变化的趋势，是研究电化学反应机理以及电化学反应动力学的重要手段之一。

一 基本原理：

内反射模式:

(1)在单晶硅(Si)上化学镀或真空镀一层纳米金膜，纳米金属膜具有表面增强效应。

(2)纳米金膜可作为导电基底，在导电基底上滴涂或电沉积上电催化剂，作为工作电极。

(3)表面增强红外，可得到电催化剂吸附态产物以及中间产物信息。

 图2：内反射模式基本原理

外反射模式:

(1)在基底电极(如GCE)表面电沉积或滴涂电催化剂作为工作电极。

(2)工作电极距离晶体的距离可以调节。

(3)晶体可选Ge，ZnSe，CaF₂，Si等。

图3：外反射模式基本原理

二 附件组成：

(1)红外光谱仪主机适配底板,适配主流红外光谱仪。

(2)平面镜加曲面镜。

(3)入射角度调节系统。

(4)衰减全反射晶体。

(5)玻璃电化学池(单池或H型池)以及PEEK外反射池。

(6)电极(玻碳电极、对电极、参比电极)。

(7)距离调节系统。

三 主要特点：

(1)可变入射角光学台，30-80度连续可调，以保证不同电催化剂处于最大光通量状态。

(2)衰减全反射晶体上具有一层增透膜，光通量增大10％以上

(3)电化学池密封性能好，可通入反应气体。

(4)晶体拆卸简单，方便打磨清洗。

(5)晶体种类可选，如Si，CaF₂，ZnSe等。

(6)电化学单池或H型池，切换方便。

(7)提供现场技术服务。

(7)可根据客户需求定制反应池并提供可行性方案。

四  ATR Crystal characteristics for FTIR sampling

 
应用案例

CO₂电还原 J. Am. Chem. Soc.2022, 144, 259−269

氧气析出反应 J. Am. Chem. Soc. 2022, 144, 21, 9271–9279

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