单薄层池原位微分电化学池
微分电化学质谱仪(Differential Electrochemical Mass Spectrometry,简称DEMS)是一种原位电化学方法,通过检测挥发性产物,可以获得界面的定性、定量信息,成为研究电化学反应机理不可或缺的重要工具之一。DEMS系统将电化学反应装置与质谱仪连用,由电化学反应产生的挥发性产物从疏水透气的膜接口进入质谱仪的真空系统管路中,通过质谱仪获得不同质荷比离子的电流随时间的变化。在电化学反应机理研究中,循环伏安法(CV)是一种较为常用的电化学手段,从获得的CV图形中可以获得丰富的电化学信息,因此,CV被频繁地用于DEMS研究中。利用DEMS进行电化学研究时,由质谱仪检测 CV 扫面过程中所生成的挥发性产物的离子电流信号随时间的变化,再通过时间轴向电势轴的变换即获得离子电流随电势变化的图形 (MSCV),为电催化反应机理研究提供更全面更深入的信息。
图1:单薄层池工作原理
性能优点:
1. 高收集效率,高灵敏度
2. 可加质子交换膜避免对电极产物的干扰
3. 可用于碳纸,泡沫铜等负载型催化剂
4. 正芯或偏芯可选
具体应用如:
1. CO2电催化还原气相产物(CO,CH4,C2H4,CH3OH等)瞬时检测,相对法拉第效率测定
2. 硝酸根电催化还原中NO,N2O,NH2OH,NH3,N2等中间产物或最终产物原位检测
3. 电解水OER同位素标记18O,LOM或AEM反应机理确认
4. 甲醇电氧化反应中间产物或最终产物(HCHO,HCOOH,CO等)瞬时检测及各产物电流效率计算
5. 氢同位素标记,氢气析出反应(HER)机理解析
6. 碳材料稳定性评估(高电位下CO,CO2检测)
7. 其他(光催化,光电催化,氧还原,氢氧化,氯气析出,有机电合成等)
应用案例:
1. 硝酸根电还原中间体检测
Angew. Chem. Int. Ed. 10.1002/anie.201915992
2. 电解水OER同位素标记18O,LOM或AEM反应机理确认
J. Am. Chem. Soc. 2021, 143, 17, 6482-6490
3. 甲醇电氧化反应
Journal of Power Sources 509 (2021) 230397
4. 氢同位素标记, 氢气析出反应(HER)机理解析
Nature catalysis, 2022,5,66-73
5. CO2电还原
ACS catal. 2019,9,1383-1388
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