Thermal co-decomposition of silver(I) acetylacetonate and tin(II) hexafluoroacetylacetonate has been examined by using thermal gravimetry, differential scanning calorimetry and complementary analyses of gaseous products and solid residues by Fourier transform infrared and Raman spectroscopy, X-ray diffraction and scanning electron microscopy. It is revealed that poorly stable silver(l) acetylacetonate mixed with tin(II) hexafluoroacetylacetonate does not undergo thermal decomposition at around 120 degrees C, but takes part in a room-temperature solid-state interaction with the Sn counterpart, which is ensued by an exothermal process at 109 degrees C and subsequent co-decomposition involving a pronounced stage at around 275 degrees C. All steps lead to carbonaceous Ag/SnO2 composites containing crystalline Ag at 200 degrees C, Ag and SnO2 at 400 degrees C, and Ag, SnO2, Ag4Sn and Ag6.2Sn at 600 degrees C. The intermetallic Ag6.2Sn compound is judged to arise from nanostructured environment of alloying Ag and Sn. (C) 2013 Elsevier B.V. All rights reserved.