一、超分辨电化学显微镜的关键作用当前,超高时间&空间分辨率的化学反应测量已经成为能源、材料、催化、环境与生命科学等众多领域的关注焦点。这些被测量的化学反应一般发生在界面上,但有些发生在材料体相以及溶液中。超分辨电化学显微镜(SRECM)技术对物理高分辨表征技术(微观物理信息—结构&成分)实现了不可或缺的有益补充(微观化学信息—反应动力学&速率),建立了之前难以获得的精准构效关系。以扫描电化学液池显微镜(SECCM)技术为例,它能够直接绘制二维材料、表面缺陷及晶界等不同位置的催化活性差异(参见Nature, 2023, 620, 782;Nature, 2021, 593, 67;Science, 2017, 358, 1187;Nat. Mater., 2021, 20, 1000等)。同样,扫描电化学显微镜(SECM)技术能够实现催化反应中间体、动力学速率以及催化剂活性位点密度的定量测量(参见Nat. Catal., 2021, 4, 654;Nat. Catal., 2021, 4, 615等)。(见第六部分—超分辨电化学显微镜应用案例)这些先进的SRECM技术为我们提供了在微观尺度上理解化学反应的窗口,同时也为精确设计和优化催化剂、材料以及理解反应动力学机制提供了有力工具。二、系统组成 以超分辨电化学显微镜为核心,通过一站式完整解决方案&完全自主研发产品,实现化学反应的高分辨测量(也称化学高分辨)。包含以下五个单元:测量&控制单元、屏蔽&防震单元、操作&观测单元、理化实验单元、探针制备单元。三、六大主力型号最强型号MT-SRECM600——超分辨电化学显微镜与共聚焦拉曼显微镜联用四、电化学显微镜技术SRECM技术支持(√)选配(●) 基于电化学工作站(双通道)循环伏安(CV)√线性扫描伏安(LSV)√电流-时间曲线(i-t)√多电位阶跃(ESTEP)√开路电位-时间曲线(OCPT)√iR降补偿√探针渐进(PAC)√探针渐远(PWC)√跳跃成像√跳跃成像+局部CV√跳跃成像+局部LSV√ 跳跃成像+局部i-t√跳跃成像+局部ESTEP√跳跃成像+局部多参数(电位-阻抗-电容)测量●表面探寻扫描电化学显微镜(SI-SECM)√恒高度成像√ 恒电流成像√基于膜片钳放大器(单通道) 循环伏安(CV)√线性扫描伏安(LSV)√电流-时间曲线(i-t)√多电位阶跃(ESTEP)√探针渐进(PAC)√探针渐远(PWC)√跳跃成像√跳跃成像+局部CV√跳跃成像+局部LSV√ 跳跃成像+局部i-t√跳跃成像+局部ESTEP√恒高度成像 √恒电流成像√五、电化学工作站技术电化学技术支持(√)选配(●)电位扫描循环伏安(CV)√多扫速循环伏安(MVCV)√分段循环伏安(MSCV)√线性扫描伏安(LSV) √塔菲尔曲线(TAFEL)√电位阶跃/脉冲 阶梯波伏安(SCV)√计时电流(CA)√计时电量(CC)√差分脉冲伏安(DPV)√常规脉冲伏安(DNPV)√ 方波伏安(SWV)√多电位阶跃(ESTEP)√恒电流技术 计时电位(CP)√电流扫描计时电位(CPCR)√多电流阶跃(ISTEP) √电位溶出分析(PSA)√基于时间 电流-时间曲线(i-t)√差分脉冲电流检测(DPA)√双差分脉冲电流检测(DDPA)√三脉冲电流检测(TPA)√积分脉冲电流检测(IPAD)√扫描-阶跃混合方法(SSF)√开路电位-时间曲线(OCPT)√交流技术 交流(含相敏)伏安(ACV)√二次谐波交流(相敏)伏安(SHACV)√傅里叶变换交流伏安(FTACV)√交流阻抗测量(IMP)●交流阻抗-时间曲线(IMPT)●交流阻抗-电位测量(IMPE)●其他技术电化学噪声测量(ECN) √外部信号记录√任意波形输入√外部电位输入√第三方开发√六、超分辨电化学显微镜应用案例七、代表作Accelerating the Discovery of Efficient High-Entropy Alloy Electrocatalysts: High-Throughput Experimentation and Data-Driven Strategies, Nano Lett. 2024, 24, 11632..Modulating the Surface Concentration and Lifetime of Active Hydrogen in Cu-Based Layered Double Hydroxides for Electrocatalytic Nitrate Reduction to Ammonia, ACS Catel. 2024, 14, 12042.Accelerating the Discovery of Oxygen Reduction Electrocatalysts: High‐Throughput Screening of Element Combinations in Pt‐Based High‐Entropy Alloys, Angew. Chem. Int. Ed. 2024, 63, e202407116.Benchmarking the Intrinsic Activity of Transition Metal Oxides for the Oxygen Evolution Reaction with Advanced Nanoelectrodes, Angew. Chem. Int. Ed. 2024, 63, e202404663(hot paper).Thermally Enhanced Relay Electrocatalysis of Nitrate-to-Ammonia Reduction over Single-Atom-Alloy Oxides, J. Am. Chem. Soc. 2024, 146, 7779.Electrochemical Visualization of an Ion-Selective Membrane Using a Carbon Nanoelectrode, ACS Sens. 2023, 8, 2713.Nanoscale electrochemical approaches to probing single atom electrocatalysts, Curr Opin Electroche. 2023, 39, 101299.Combination of Rapid Intrinsic Activity Measurements and Machine Learning as a Screening Approach for Multicomponent Electrocatalysts, Acs Appl. Mater. Inter. 2023, 15, 42532.The Microstructure-Activity Relationship of Metal-Organic Framework-Based Electrocatalysts for the 0xygen Evolution Reaction at the Single-Particle Level, Acs Mater Lett. 2023, 5, 1902.Precise Polishing and Electrochemical Applications of Quartz Manopipette-Based Carbon Nanoelectrodes, Anal Chem. 2022, 94, 14092.Nitrogen-skinned carbon nanocone enables non-dynamic electrochemistry of individual metal particles, Sci China Chem. 2022, 65, 2031.
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