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

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 degrees 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 0001 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. (C) 2016 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.This present research was funded by the Community of Madrid under the GEOMATERIALES II project (S2013/MIT-2914), by the Complutense University of Madrid’s Research Group: “The alteration and conservation of stone heritage” (921349), the Autonomous Region Program of Madrid, MULTIMAT-CHALLENGE (ref. S2013/MIT‐2862), the Innovation and Education Ministry ref. (MAT2013-47460-C5-5-P), the Mat201019837/C06-05 and the Ministry of Education, Science and Technological Development of Serbia (OI 1612046) projects. The authors are indebted to the Petrophysical Laboratory IGEO, affiliated with the Moncloa Campus of International Excellence CEI-09-009(UCM-UPM), the Heritage Laboratory Network in Science and Technology for Heritage Conservation (RedLabPat,) and the Materials Science Department (Carlos III University of Madrid)