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In Situ X-ray Diffraction Studies of the Crystallization of Layered Manganese Thioantimonates(III) under Hydrothermal Conditions
- Source :
- Chemistry of Materials. 13:1383-1390
- Publication Year :
- 2001
- Publisher :
- American Chemical Society (ACS), 2001.
-
Abstract
- The solvothermal synthesis of the layered compound Mn2Sb2S5·DAP (DAP = 1,3-diaminopropane) has been studied using in situ energy-dispersive X-ray diffraction. The results clearly demonstrate that the induction time strongly depends on the reaction temperature. At lower temperatures two crystalline intermediates could be detected. The decay of the second intermediate and the product growth show a strong correlation. A detailed analysis of the extent of reaction α suggests that a small fraction of the intermediate is either dissolved or converted into an amorphous state. The experimentally determined extent of reaction α versus time was compared with various theoretical models. The reaction exponents indicate similar mechanisms for temperatures between 105 and 125 °C. The best agreement is obtained with a first-order reaction and/or phase-boundary-controlled mechanisms. A rigorous analysis reveals that it is highly likely that with increasing α the mechanism changes, suggesting consecutive and/or parallel k...
- Subjects :
- chemistry.chemical_classification
Reaction mechanism
Materials science
General Chemical Engineering
Solvothermal synthesis
General Chemistry
Activation energy
law.invention
Amorphous solid
Crystallography
chemistry
Extent of reaction
law
X-ray crystallography
Materials Chemistry
Crystallization
Inorganic compound
Subjects
Details
- ISSN :
- 15205002 and 08974756
- Volume :
- 13
- Database :
- OpenAIRE
- Journal :
- Chemistry of Materials
- Accession number :
- edsair.doi...........822a0f0d13eb251b40fcc543376d9efd