Cryptocrystal layers of ammonium silicon fluoride (NH4)(2)SiF6 were synthesized on silicon wafers by dry etching method using vapor of the mixture of HF and HNO3 Solutions at room temperature. Crystalline layers having thicknesses of up to 8 mum have been produced at growth rates of around 1 m/h. The crystallinity was analyzed by X-ray diffraction that indicates an isometric hexoctahedral system (4/m-32/m) with Fm3m space grouping of (NH4)(2)SiF6 cryptohalite crystals. These results have been confirmed by the presence of vibrational absorption bands of (NH4)(2)SiF6 species by Fourier transform infrared (FTIR) spectroscopic measurements. Strong absorption bands were observed in the infrared at 480, 725, 1433 and 3327 cm(-1) and assigned to N-H and Si-F related vibrational modes of (NH4)(2)SiF6. Annealing above 150 degreesC leads to the formation of individual crystals with sizes up to 20 mum on the surface, thus indicating the possibility of forming solid compound layers with fine grain sizes on silicon. (C) 2004 Elsevier B.V. All rights reserved.