Parinya Somrang . Comparative effect of crystallite size and calcination temperature on the thermal stability of spinel type metal oxide. Master's Degree(Chemical Engineering). Chulalongkorn University. : Chulalongkorn University, 2001.
Comparative effect of crystallite size and calcination temperature on the thermal stability of spinel type metal oxide
Abstract:
The nanostructured material zinc chromite, zinc manganite, zinc ferrite and zinc cobaltile were synthesized via the thermal reaction of zinc acetate and metal acetylacetonate, stoichiometric ratios of Zn/Metal equal to 0.5, in 1,4-butanediol at 300 ํC for 2 hours under autogenous pressure with different reaction heating rate of 2.5 and 1.0 ํC/min. Zinc chromite and zinc ferrite were directly formed after glycothermal reaction, while zinc manganite and zinc cobaltile which were formed via an undetermined intermediate phase had to be calcined at a desired temperature before forming spinel phase. It was found that the reaction heating rate affected significantly on the crystallite size of the as-synthesized products. The crystallite size of the as-synthesized products observed by TEM was close to that examined by XRD. This suggested that each particle was a single crystal. After calcination at various temperatures, the results indicated that the thermal stability of the spinel type metal oxides lied in the correlation of, ZnCr2O4>ZnMn2O4>ZnFe2O4~ZnCo2O4 The thermal stability of the product was designed from the ratio of the crystallite size of the product after calcined (d) to the crystallite size of the as-synthesized sample (d0). Teh spinel structure, before and after calcination, revealed the same performance even after calcined at high temperature