In a conventional XRD goniometer device the diffraction intensity is determined consecutively over the diffraction angle range. The development of efficient and highly sensitive image-plate detectors enables the fast and instantaneous recording of the diffraction pattern up to 140° 2θ. In addition a linear position sensitive detector (linear-PSD) with a restricted range of diffraction angle of several degrees enabling high angular resolution was used. These two types of detection instruments were applied for the in-situ study of comparatively rapid electrochemical processes on electrode surfaces at different angle of incidence. The advantages and disadvantages of these detection systems and the related measurement procedures will be discussed in detail. The use of an appropriate in-situ electrochemical cell is essential. The electric potential and current were recorded during the measurement series. The detection of the phase formation especially in the uppermost electrode surface region up to a depth of a few micrometers was achieved by variation of the penetration depth by different angles of incidence. The phase composition in the irradiated region was determined quantitatively during the electrochemical reaction by means of the Rietveld refinement method. However, the observed values are strongly influenced by the layered structure of the sample and by the different absorption coefficients of the phases. Furthermore, the absorption of the diffraction pattern of the electrode material gives information on the absorption properties of the reaction layers. Up to now our studies are focussed on different composed lead electrodes in sulphate containing electrolytes with various additives and the electrodeposition of metals on different substrates.

Figure 1: In-situ XRD traces of galvanostatically deposited copper on a nickel substrate with increasing deposition time. 

Acknowledgements: This work was supported within the K plus programme by the Austrian Research Promotion Agency and the government of Lower Austria.

• Legal notice:
  

  Copyright (c) Pielaszek Research, all rights reserved.
  The above materials, including auxiliary resources, are subject to Publisher's copyright and the Author(s) intellectual rights. Without limiting Author(s) rights under respective Copyright Transfer Agreement, no part of the above documents may be reproduced without the express written permission of Pielaszek Research, the Publisher. Express permission from the Author(s) is required to use the above materials for academic purposes, such as lectures or scientific presentations.
  In every case, proper references including Author(s) name(s) and URL of this webpage: https://science24.com/paper/14862 must be provided.