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Solvothermal methods have been widely used to synthesize different kinds of materials. However, only little is known about how precursor solutions react to form solid precipitates via this method. In the present study, in situ microcalorimetry is first used to investigate the formation mechanism under solvothermal conditions, where ZnFe2O4 synthesized using a solvothermal method was selected as the model sample. Some novel results are obtained, such as with the experimental temperature increase, (1) the homogeneous solution transforms to
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