Thermal Decomposition of Ferric Oxalate Tetrahydrate in Oxidative and Inert Atmospheres: The Role of Ferrous Oxalate as an Intermediate
作者： Pavla Hermankova , Martin Hermanek , Radek Zboril
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摘要: The thermal decomposition of ferric oxalate tetrahydrate Fe 2 (C O 4 ) 3 ·4H was studied in dynamic oxidative and inert atmospheres by using a simultaneous thermogravimetric (TG) differential scanning calorimetric (DSC) analytical device equipped with an evolved gas analyzer (EGA). Solid-state products formed during the were analyzed 57 Mossbauer spectroscopy, situ ex X-ray powder diffraction, magnetic measurements. In atmosphere, we observed formation tiny amount superparamagnetic iron oxide (most likely together majority ferrous (FeC remains undecomposed after first step, which finished at 210 °C. astonishing presence oxidic phase such low temperatures is highly probable side effect main reduction action electrons on III cations structure, thus resulting creation intermediate FeC . final product atmosphere mixture wustite (Fe x O), α-iron (α-Fe), magnetite ). Their proportion accurately reflects actual disproportionation/synproportionation/redisproportionation processes encouraged preserved size morphology initial crystals that are dependent temperature. proceeds three overlapped stages include dehydration, reductive as intermediate, decarboxylation to hematite (α-Fe principal experimental conditions also discussed evaluated from isothermal experiments carried out 180
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