Chromium nitride (CrN)/carbon nitride (CN) and nano-tinanium nitride (TiN)/CN composites were prepared by in situ nitridation during the formation of amorphous CN (a-CN) matrix. The second crystalline phases CrN and TiN were distributed uniformly in a-CN phase. The CrN particle sizes ranged from submicrometers to several micrometers, and the average TiN particle diameter was found to be similar to 16 nm. Thermogravimetry was used to reveal the thermal stability of these composite materials. X-ray photoelectron spectroscopy showed that the relative proportion of sp(3) carbon-nitrided and sp(2) carbon-nitrided phase of the a-CN matrix was influenced by the different second phases.