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Chapter 3 Experimental methods The current section gives a brief overview of the experimental methods applied in the present thesis. Further details are found in Hummelgård et al. [15] (paper 1) and Sandin et al. [14] (paper 4). 3.1 Preparation of mixed oxide coatings using spin- coating In Hummelgård et al. [15], we studied the effect of modifying a conventional DSA coating (Ru0.3Ti0.7O2) by addition of Co to obtain a coating with 31% less Ru and the overall composition Ru0.2Co0.1Ti0.7O2 (based on the composition of the coat- ing solution). The electrodes were prepared by depositing the coating solution onto polished Ti discs, which were then spun at 1400 rpm on a spin-coating device to produce an even coating layer. Afterwards, the electrode was first dried in a fur- nace kept at 80 ◦C for 10 minutes before being calcined at 470 ◦C for 10 minutes in the same furnace. This process was either performed once, or repeated 3 or 7 times, before a final calcination for 60 minutes at the highest temperature. This spin-coating method makes it possible to control the amount of coating solution that is applied in each layer. It was estimated (based on the measured weight in- crease and the concentration-weighted density of the oxide coating[196]) that this produced coatings with thicknesses of 0.5 μm, 1.45 μm or 3.4 μm. The coating was then characterized by use of atomic force microscopy (AFM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and differential scanning calorimetry (DSC) as well as by electrochemical measurements. 43PDF Image | Studies of Electrode Processes in Industrial Electrosynthesis
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