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Departamento de Química Inorgánica, Cristalografía y Mineralogía, Facultad de Ciencias, Campus de Teatinos, Universidad de Málaga, 29071 Málaga, Spain
E-mail of corresponding author: mdruiz{at}uma.Es
The intercalation complex of a low-defect ("well-crystallized") kaolinite from Cornwall, England, with hydrazine was studied by high-temperature X-ray diffraction (HTXRD), differential thermal analysis (DTA), and thermogravimetry (TG). The X-ray pattern at room temperature indicated that intercalation of hydrazine into kaolinite causes an increase of the basal spacing from 7.14 to 10.4 å, as previously reported. Heating between 25200°C produces a structural rearrangement of the complex, which initially causes a contraction of the basal spacing from 10.4 to 9.6 å. In a second stage, the basal spacing reduces to 8.5 å. Finally, in a third stage, a reduction in spacing occurs through a set of intermediate phases, interpreted as interstratifications of intercalated and non-intercalated 1:1 layers. Evidence for these changes was observed by DTA, where three endothermic reactions are observed at low temperature. This behavior suggests that intercalated molecules occupy several well-defined sites in the interlayer of the kaolinite complex. The intercalated molecules deintercalate in an ordered fashion, which explains the successive and discontinuous contraction of the basal spacing of the complex. Heating between 200400°C caused a limited increase in stacking order of the kaolinite structure, whereas dehydroxylation of kaolinite and the disappearance of its X-ray reflections occurred between 450640°C.
Key Words: DTA-TG HTXRD Hydrazine Intercalation Complex Kaolinite
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