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Various iron-based polycrystalline monoliths, Fe3O4, iron, and Fe3C, with hierarchically distributed pores have been synthesized from ionic precursors using a sol–gel process accompanied by phase separation. Propylene oxide acts as a proton scavenger to increase pH moderately and uniformly in a reaction solution, which leads to homogeneous gelation. On the other hand, poly(acrylamide) works as a phase separation inducer as well as a precipitation inhibitor. Appropriate choice of iron precursor, solvent, polymer, and epoxide allowed the formation of iron(III)-based xerogels with cocontinuous macroporous structures. The dried gels were amorphous, whereas heating in air above 300 °C led to the formation of α-Fe2O3. Calcination under an inert condition above 400 °C formed Fe3O4, iron, and Fe3C without collapse of macrostructures. Examination has been carried out using SEM, TG-DTA, FT-IR, Hg intrusion, pH measurement, X-ray diffraction, and N2 adsorption–desorption.
| Authors: | Yasuki Kido; Kazuki Nakanishi; Akira Miyasaka; Kazuyoshi Kanamori | |
| Journal: | Chemistry of Materials | |
| Year: | 2012 | |
| DOI: | 10.1021/cm300495j | |
| Publication date: | 15-05-2012 |
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