A 40 kHz pulsed plasma metalorganic chemical vapour deposition process using tetrakis (diethylamido) titanium as precursor was investigated by means of in situ methods. Mass and energy distributions were measured separately for ions and neutral particles utilizing a two-stage differentially pumped mass spectrometer equipped with an energy analyser. Using ammonia as an additional nitrogen source, the reduction in C x H + y ion flux and the dominance of NH + x ions correlate with a reduction in carbon incorporation in the Ti-C-N layers. The texture of the fine-grained films deposited at 150°C depends on the energy of incident ions. The measured ion energy distributions, different to some extent for different ionic species, give reason to assume that most of the ions detected are generated in the cathode layer.