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Microwave Synthesis of Hybrid Inorganic–Organic Porous Materials: Phase‐Selective and Rapid Crystallization
Author(s) -
Jhung Sung Hwa,
Lee JinHo,
Forster Paul M.,
Férey Gérard,
Cheetham Anthony K.,
Chang JongSan
Publication year - 2006
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.200600270
Subject(s) - hydrothermal circulation , hydrothermal synthesis , tetragonal crystal system , materials science , microwave , nickel , crystallization , porosity , phase (matter) , chemical engineering , metal , hybrid material , microwave irradiation , nanotechnology , chemistry , metallurgy , organic chemistry , composite material , physics , quantum mechanics , engineering
Microwave synthesis of two porous nickel glutarates was compared with conventional hydrothermal synthesis. The cubic nickel glutarate, [Ni 20 (C 5 H 6 O 4 ) 20 (H 2 O) 8 ]⋅40 H 2 O ( 1 ), was synthesized by conventional electrical heating in several hours or days, depending on synthesis temperature. Crystallization was greatly accelerated by microwave irradiation, in which more stable, tetragonal nickel glutarate, [Ni 22 (C 5 H 6 O 4 ) 20 (OH) 4 (H 2 O) 10 ]⋅38 H 2 O ( 2 ), was formed within a few minutes, suggesting the efficiency of the microwave technique in the synthesis of porous hybrid materials. The cubic phase 1 is formed preferentially at low pH, low temperature, and especially under conventional electrical heating. In contrast, the tetragonal phase 2 is obtained favorably at high pH, high temperature, and especially with microwave irradiation. This work demonstrates that the microwave method provides not only the very fast synthesis of a hybrid material, but also the possibility to discover a new porous hybrid material not yet identified by conventional hydrothermal synthesis. The hydrothermal formation of metal–organic hybrid materials in a matter of minutes is an important step towards developing commercially viable routes for producing this valuable class of materials.