Renner Frank Uwe, Gründer Yvonne, Zegenhagen Jörg
European Synchrotron Radiation Facility, BP 220, 38043 Grenoble, France.
Rev Sci Instrum. 2007 Mar;78(3):033903. doi: 10.1063/1.2714046.
We report on a new electrochemical cell setup, combined with a portable UHV chamber, for in situ x-ray diffraction using synchrotron radiation. In contrast to more traditional electrochemical sample preparation schemes, atomically clean and well-ordered surfaces are routinely prepared by UHV methods, even in the case of reactive elements or alloys. Samples can be transferred from larger UHV systems into the portable chamber without exposure to ambient air. They can then be studied successively in UHV, in controlled gas atmospheres, and in contact with electrolyte solutions under applied electrochemical potential. The electrochemical setup employs a droplet geometry, which guarantees good electrochemical conditions during in situ x-ray measurements combined with voltammetry. We present first experimental results of Cu deposition on GaAs(001) and on freshly produced nanometric Pd(001) islands on Cu(0.83)Pd(0.17)(001), respectively.
我们报道了一种结合便携式超高真空腔的新型电化学电池装置，用于利用同步辐射进行原位X射线衍射。与更传统的电化学样品制备方案不同，即使对于活性元素或合金，超高真空方法也能常规制备出原子清洁且有序的表面。样品可以从大型超高真空系统转移到便携式腔室中，而无需暴露于环境空气中。然后，可以在超高真空、受控气体气氛以及在施加电化学势的情况下与电解质溶液接触的条件下对样品进行连续研究。该电化学装置采用液滴几何形状，这保证了在原位X射线测量与伏安法相结合的过程中具有良好的电化学条件。我们分别展示了铜在GaAs(001)以及在Cu(0.83)Pd(0.17)(001)上新鲜制备的纳米级Pd(001)岛状物上沉积的首批实验结果。
