Three transition metals, Ni, Mo, and Ti, were reacted with SiCN at high temperatures, and the reaction products characterized by X-ray diffraction. It was concluded that TiN is the most suitable interconnect material for the measurement of the electrical conductivity of SiCN at temperatures up to 1400°C. The TiN interconnects were produced by an in situ process on H-shape specimens of SiCN, with an appropriate correction factor (which was obtained by finite-element analysis) for the four-point measurement of the electrical resistance. The process consisted of placing a small drop of a slurry constituted from liquid Ceraset™ (the precursor for SiCN) and Ti metal powder (50 wt%) on the contact point. The droplet was photo-cured and pyrolyzed. The TiN interconnect was generated during the pyrolysis. Finally, as an example, the measurement of the conductivity of a SiCNO sample up to 1300°C is reported. A more complete study of the relationship between the conductivity and the composition of SiCNO will be reported separately.