Sodium hexafluorosilicate (Na 2 SiF 6 ) powder has been used as a silicon source for formation of Si 3 N 4 coatings by the hybrid precursor system-chemical vapor deposition (HYSY-CVD) route. The quantitative effect of processing time, temperature, gas flow rate, and process atmosphere (N 2 and N 2 :5% NH 3 ) upon the fractional weight loss during the decomposition of Na 2 SiF 6 was studied using a standard L 9 Taguchi experimental design and analysis of variance. The decomposition kinetics of Na 2 SiF 6 (s) was studied theoretically and experimentally in the temperature range of 550-650ºC by applying the shrinking core model. It was found that regardless of atmosphere type, the reaction order is n 0.12 and that a two-stage mixed mechanism consisting of chemical reaction and boundary layer gas transfer controls the decomposition rate. The determined fractional weight loss during Na 2 SiF 6 decomposition in nitrogen atmosphere is about 1.05-1.5 orders of magnitude greater than that in N 2 :NH 3 . The gas flow rate affects the dissociation activation energy, being of 121, 109, and 94 kJ/mol in N 2 and of 140, 120, and 115 kJ/mol in N 2 :NH 3 , for the flow rates of 20, 60, and 100 cm 3 /min, respectively, in both atmosphere types. A good agreement is observed by comparing experimental weight loss data with model predictions.