Papac Meagan C, Talley Kevin R, O'Hayre Ryan, Zakutayev Andriy
National Renewable Energy Laboratory, Materials Science Center, Golden, Colorado 80401, USA.
Department of Metallurgical and Materials Engineering, Colorado School of Mines, Golden, Colorado 80401, USA.
Rev Sci Instrum. 2021 Jun 1;92(6):065105. doi: 10.1063/5.0024875.
We demonstrate an instrument for spatially resolved measurements (mapping) of electrochemical impedance under various temperatures and gas environments. Automated measurements are controlled by a custom LabVIEW program, which manages probe motion, sample motion, temperature ramps, and potentiostat functions. Sample and probe positioning is provided by stepper motors. Dry or hydrated atmospheres (air or nitrogen) are available. The configurable heater reaches temperatures up to 500 °C, although the temperature at the sample surface is moderated by the gas flow rate. The local gas environment is controlled by directing flow toward the sample via a glass enclosure that surrounds the gold wire probe. Software and hardware selection and design are discussed. Reproducibility and accuracy are quantified on a Ba(Zr,Y)O proton-conducting electrolyte thin film synthesized by pulsed laser deposition. The mapping feature of the instrument is demonstrated on a compositionally graded array of electrocatalytically active Ba(Co,Fe,Zr,Y)O thin film microelectrodes. The resulting data indicate that this method proficiently maps property trends in these materials, thus demonstrating the reliability and usefulness of this method for investigating electrochemically active thin films.
我们展示了一种用于在各种温度和气体环境下对电化学阻抗进行空间分辨测量（测绘）的仪器。自动测量由定制的LabVIEW程序控制，该程序管理探头运动、样品运动、温度斜坡以及恒电位仪功能。样品和探头的定位由步进电机提供。可提供干燥或潮湿的气氛（空气或氮气）。可配置的加热器可达到高达500°C的温度，不过样品表面的温度会受到气体流速的调节。通过围绕金线探头的玻璃外壳将气流导向样品来控制局部气体环境。讨论了软件和硬件的选择与设计。在通过脉冲激光沉积合成的Ba(Zr,Y)O质子传导电解质薄膜上对重现性和准确性进行了量化。在具有成分梯度的电催化活性Ba(Co,Fe,Zr,Y)O薄膜微电极阵列上展示了该仪器的测绘功能。所得数据表明，该方法能够有效地测绘这些材料的性能趋势，从而证明了该方法在研究电化学活性薄膜方面的可靠性和实用性。
