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High‐Throughput and Time‐Resolved Energy‐Dispersive X‐Ray Diffraction (EDXRD) Study of the Formation of CAU‐1‐(OH) 2 : Microwave and Conventional Heating
Author(s) -
Ahnfeldt Tim,
Moellmer Jens,
Guillerm Vincent,
Staudt Reiner,
Serre Christian,
Stock Norbert
Publication year - 2011
Publication title -
chemistry – a european journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.687
H-Index - 242
eISSN - 1521-3765
pISSN - 0947-6539
DOI - 10.1002/chem.201003708
Subject(s) - thermogravimetric analysis , diffraction , crystallization , materials science , microwave , analytical chemistry (journal) , x ray crystallography , powder diffraction , sorption , spectroscopy , porosity , crystallography , aluminium , elemental analysis , chemistry , inorganic chemistry , organic chemistry , optics , metallurgy , physics , composite material , adsorption , quantum mechanics
Aluminium dihydroxyterephthalate [Al 8 (OH) 4 (OCH 3 ) 8 (BDC(OH) 2 ) 6 ] ⋅ x H 2 O (denoted CAU‐1‐(OH) 2 ) was synthesized under solvothermal conditions and characterized by X‐ray powder diffraction, IR spectroscopy, sorption measurements, as well as thermogravimetric and elemental analysis. CAU‐1‐(OH) 2 is isoreticular to CAU‐1 and its pores are lined with OH groups. It is stable under ambient conditions and in water, and it exhibits permanent porosity and two types of cavities with effective diameters of approximately 1 and 0.45 nm. The crystallization of CAU‐1‐(OH) 2 was studied by in situ energy‐dispersive X‐ray diffraction (EDXRD) experiments in the 120–145 °C temperature range. Two heating methods—conventional and microwave—were investigated. The latter leads to shorter induction periods as well as shorter reaction times. Whereas CAU‐1‐(OH) 2 is formed at all investigated temperatures using conventional heating, it is only observed below 130 °C using microwave heating. The calculation of the activation energy of the crystallization of CAU‐1‐(OH) 2 exhibits similar values for microwave and conventional synthesis.