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Near-field optical techniques such as nano-FTIR spectroscopy enable spectroscopic characterization of samples with a high sensitivity and a spatial resolution at the nanoscale. In this work we realized nano-FTIR spectroscopy by elastic scattering of infrared light from a probe tip of an atomic force microscope operated in tapping mode, with broadband infrared synchrotron radiation provided by the Metrology Light Source (MLS). We apply this technique to characterize the protective oxidation layers of different Silicon Carbides (SiCs) treated by chlorine gas. The process using chlorine-donors has been developed to separate toxic heavy metals from sewage sludge ash (SSA) and to increase the plant-availability of phosphors in the SSA in order to produce P-fertilizers. Nitrified SiC showed the highest resistant strength against chlorine corrosion at 1000 °C compared to the other SiCs. In order to discuss this behavior high resolution imaging has been performed on the interfacial layer between bulk-SiC and the protective oxidation layer on sub-micrometer scale. The formation of a SixNiyO protective layer, which might be the reason for the higher corrosion resistance, was observed using nano-FTIR spectroscopy.
The present study shows the potential of high-resolution imaging and nano-Fourier-transform infrared (nano-FTIR) spectroscopy for corrosion science. The protective oxidation layers of different chlorine-gas treated silicon
carbides (SiCs) were characterized with these techniques. A nitrified SiC showed the highest resistant strength against chlorine corrosion at 1000 °C compared to the other SiCs. Nano-FTIR spectroscopy with a lateral resolution below 40 nm detected differences in the crystallinity of the bulk-SiC and in the transitional region to the protective layer. Furthermore, high-resolution imaging provides deep insight in the interfacial layer between bulk-SiC and the protective oxidation layer on sub-micrometer scale.