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Chromium mixed cadmium oxalate (CMCO) [Cr:Cd (C2O4).3H2O] crystals are grown by gel diffusion method using silica hydro gel as growth media at ambient temperature. The optimum condition for growth is established by varying the parameters such as specific gravity, pH, gel aging, concentration of reactants and ratio of mixture Cd+2 to Cr+3. Energy dispersive X‐ray spectroscopy (EDX) confirms the existence of Cd+2 and Cr+3 ions in the crystal lattice of CMCO. Thermo‐gravimetric analysis (TGA) reveal that, the CMCO are thermally stable up to 950 °C, which confirms the presence of three water molecules in the crystal lattice of CMCO. FT‐IR spectrum exhibits the presence of OH, carboxyl group and metal‐oxygen bonding. In this study, the occupation of vacancies of Cd+2 ions by Cr+3 cations in the lattice of mixed cadmium oxalate crystals without altering the morphology of the parent crystal is confirmed.

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