Dowsett Mark G, Adriaens Annemie
Department of Physics, Warwick University, Coventry CV4 7AL, UK.
Anal Chem. 2006 May 15;78(10):3360-5. doi: 10.1021/ac052125y.
We describe the construction of an electrochemical cell of the Bragg type suitable for in situ synchrotron X-ray measurements on rough, heterogeneous metals such as cultural heritage alloys and simulants with corroding or passivated surfaces. The cell features a working electrode, which may be moved under remote control from a position close to an X-ray window to full immersion in the electrolyte. A pocket of electrolyte in contact with the bulk can be maintained on the working electrode surface at all times. Its thickness (typically 100-200 microm) can be controlled by adjusting the working electrode position and, independently, altering the conformation of the X-ray window with hydrostatic pressure. Alternatively, the electrode may be lowered into the bulk of the electrolyte. Early results from the cell showing a time-resolved study of the reduction of nantokite to cuprite in sodium sesquicarbonate, accompanied by corrosion potential measurements obtained in parallel, are presented here.
我们描述了一种布拉格型电化学池的构建，该电化学池适用于对粗糙、异质金属（如文化遗产合金以及具有腐蚀或钝化表面的模拟物）进行原位同步加速器X射线测量。该电池具有一个工作电极，可通过远程控制从靠近X射线窗口的位置移动到完全浸入电解液中。工作电极表面始终可保持与主体接触的一小部分电解液。其厚度（通常为100 - 200微米）可通过调整工作电极位置并独立地通过静水压力改变X射线窗口的形态来控制。或者，电极可降至电解液主体中。本文展示了该电池的早期结果，即对倍半碳酸钠中氯铜矿还原为赤铜矿的时间分辨研究，并同时进行了腐蚀电位测量。
