1. Thermogravimetric analysis of layered double hydroxides intercalated with sulfate and alkaline cations [M62+Al3(OH)18][A+(SO4)2] 12H2O (M2+ = Mn, Mg, Zn; A+ = Li, Na, K)
- Author
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Neffer Arvey Gomez Gomez, Anne Raquel Sotiles, and Fernando Wypych
- Subjects
Thermogravimetric analysis ,Materials science ,Layered double hydroxides ,Infrared spectroscopy ,Thermal treatment ,engineering.material ,Condensed Matter Physics ,Alkali metal ,Amorphous solid ,Crystallography ,engineering ,Physical and Theoretical Chemistry ,Fourier transform infrared spectroscopy ,Chemical composition - Abstract
The synthesized phases with chemical composition $$\left[ {{\text{M}}^{2 + }_{6} {\text{Al}}_{3} \left( {\text{OH}} \right)_{18} } \right]\left[ {{\text{A}}^{ + } \left( {{\text{SO}}_{4} } \right)_{2} } \right]12{\text{H}}_{2} {\text{O}}$$ (M2+ = Mn, Mg, Zn; A+ = Li, Na or K) were evaluated in relation to their thermal behavior by thermogravimetric analysis (TGA), X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR). In the shigaite (M2+ = Mn), natroglaucocerinite (M2+ = Zn) and motukoreaite (M2+ = Mg) phases, the TGA measurements indicated that all samples were dehydrated up to 200 °C in two steps, followed by dehydroxylation above 300 °C. After the thermal treatment at 1000 °C, formation of oxides/spinels were observed for the shigaite and natroglaucocerinite phases, while for motukoreaite, oxides, spinels and MgSO4 were detected. XRD indicated a reduction in the basal distance from around 11 A for the fully hydrated phases to around 7 A for the dehydrated phases. The thermal treatments of some samples at 100 °C, 150 °C and 200 °C indicated that in all phases, intercalated sulfate and alkaline metal ions can be dehydrated and rehydrated. As indicated by FTIR, at 200 °C sulfate could be grafted to the layers and at 300 °C, for all the phases, a stable mixture of amorphous materials was obtained, which could not be rehydrated.
- Published
- 2019