Abstract: A process for the preparation of nanodimensional particles of oxides and sulphides of metals and metal clusters in a carbonaceous matrix. Inorganic salts of metals are thoroughly mixed with one or more of the polymers polyphenylene sulphide, polyphenylene oxide, polyphenylene selenide, polyphenylene telluride and polyacrylonitrile in a solvent mixture. The mixture is dried and pellets are made from the dried mixture by applying compaction loads in the range of 4000 to 8000 and more preferably 5000 to 5500 psi followed by heating at a temperature in the range of 400.degree. to 800.degree. C. in an inert atmosphere. The above pellets are cooled to room temperature slowly.