Atomic scale study of the dehydration/structural transformation in micro and nanostructured brucite (Mg(OH)2) particles: Influence of the hydrothermal synthesis conditions

- Hydrothermal synthesis of brucite: 2 hydrazine/nitrate concentrations, same temperature/time.
- Differences in particle size, morphology, crystallinity, preferential orientations.
- Differences in kinetic of reaction during the dehydration process in the TEM.
- High concentration: larger crystals, better crystallinity, fast dehydration process.
- High concentration: bigger unit cell parameters, strong preferential orientation.

Micro and nanostructured brucite (Mg(OH2)) particles synthesized by hydrothermal method from solutions with high content of hydrazine (0.14 M) and nitrate (0.24 g) were compared with samples obtained from low hydrazine content (0.0002 M) and nitrate (0.12 g). The samples were heated at 180 °C for 4 h, 6 h and 12 h. XRD, TEM-HRTEM, SAED and image analysis techniques were used for the morphological and structural characterization. The effect of electron beam irradiation on the brucite dehydration was observed in atomic resolution images at 300 kV. Hexagonal crystals show differences in crystallinity, strains and kinetic of reaction. High hydrazine/nitrate samples have slightly larger crystals with better crystallinity, showing a strong preferential orientation. Rietveld refinements show how unit cell parameters are bigger in samples obtained with higher hydrazine/nitrate content, confirming also the preferential orientation along the 0 0 0 1 plane. Differences in the dehydration process show the rapid formation of a porous surface, the amorphised cortex or the presence of highly oriented strains in samples prepared from higher hydrazine/nitrate content. Conversely, crystals slightly smaller with randomly scattered defect surfaces showing the Mg(OH)2/MgO interphase in samples prepared with low hydrazine/nitrate content. Significant differences in the kinetic of reaction indicate how the dehydration process is faster in samples prepared with high hydrazine/nitrate content.

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