Beker Anne France, Sun Hongyu, Lemang Mathilde, van Omme J Tijn, Spruit Ronald G, Bremmer Marien, Basak Shibabrata, Pérez Garza H Hugo
DENSsolutions B.V., Informaticalaan 12, 2628 ZD, Delft, The Netherlands.
Nanoscale. 2020 Nov 12;12(43):22192-22201. doi: 10.1039/d0nr04961a.
The field of electrochemistry promises solutions for the future energy crisis and environmental deterioration by developing optimized batteries, fuel-cells and catalysts. Combined with in situ transmission electron microscopy (TEM), it can reveal functional and structural changes. A drawback of this relatively young field is lack of reproducibility in controlling the liquid environment while retaining the imaging and analytical capabilities. Here, a platform for in situ electrochemical studies inside a TEM with a pressure-driven flow is presented, with the capability to control the flow direction and to ensure the liquid will always pass through the region of interest. As a result, the system offers the opportunity to define the mass transport and control the electric potential, giving access to the full kinetics of the redox reaction. In order to show the benefits of the system, copper dendrites are electrodeposited and show reliable electric potential control. Next, their morphology is changed by tuning the mass transport conditions. Finally, at a liquid thickness of approximately 100 nm, the diffraction pattern revealed the 1,1,1 planes of the copper crystals, indicating an atomic resolution down to 2.15 Å. Such control of the liquid thickness enabled elemental mapping, allowing us to distinguish the spatial distribution of different elements in liquid.
电化学领域有望通过开发优化的电池、燃料电池和催化剂来解决未来的能源危机和环境恶化问题。结合原位透射电子显微镜（TEM），它可以揭示功能和结构变化。这个相对年轻的领域的一个缺点是，在保持成像和分析能力的同时，控制液体环境缺乏可重复性。在此，我们展示了一个用于在配备压力驱动流的TEM内进行原位电化学研究的平台，该平台能够控制流动方向并确保液体始终通过感兴趣的区域。因此，该系统提供了定义质量传输和控制电势的机会，从而能够研究氧化还原反应的完整动力学。为了展示该系统的优势，我们电沉积了铜树枝晶，并展示了可靠的电势控制。接下来，通过调整质量传输条件改变了它们的形态。最后，在液体厚度约为100 nm时，衍射图案显示出铜晶体的1,1,1平面，表明原子分辨率低至2.15 Å。对液体厚度的这种控制实现了元素映射，使我们能够区分液体中不同元素的空间分布。
