Octahedral iron phosphate hydroxide microcrystals: Fast microwave-hydrothermal preparation, influencing factors and the shape evolution

Journal Article · Sat Sep 15 04:00:00 EDT 2012 · Materials Research Bulletin

DOI:https://doi.org/10.1016/J.MATERRESBULL.2012.05.020· OSTI ID:22215741

Zhou, Quanyi ^[1]; Ni, Yonghong ^[1]; Ni, Hui ^[1]; Ma, Xiang ^[2]; Zhou, Yunyou ^[1]

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1. College of Chemistry and Materials Science, Anhui Key Laboratory of Functional Molecular Solids, Anhui Normal University, Wuhu 241000 (China)
2. Centers of Modern Analyses, Nanjing University, Nanjing 210093 (China)

Graphical abstract: Octahedral Fe{sub 4}(PO{sub 4}){sub 3}(OH){sub 3} microcrystals have been successfully prepared by a microwave-assisted hydrothermal route at 170 °C for 20 min. The morphology of Fe{sub 4}(PO{sub 4}){sub 3}(OH){sub 3} could be tuned by the Na{sub 2}SO{sub 3}/HAc molar ratio. Highlights: ► Fe{sub 4}(PO{sub 4}){sub 3}(OH){sub 3} octahedra had been hydrothermally prepared under the microwave assistance. ► The morphology of the final product could be tuned by the original molar ratio of Na{sub 2}SO{sub 3}/HAc. ► Low or high temperatures were unfavorable for the formation of Fe{sub 4}(PO{sub 4}){sub 3}(OH){sub 3} octahedra. ► The time-dependent shape evolution of the final product was investigated. -- Abstract: Octahedral Fe{sub 4}(PO{sub 4}){sub 3}(OH){sub 3} microcrystals have been successfully prepared by a microwave-assisted hydrothermal route at 170 °C for 20 min, employing FeCl{sub 3}·6H{sub 2}O and NaH{sub 2}PO{sub 4}·2H{sub 2}O as the starting materials in the presence of proper amounts of Na{sub 2}SO{sub 3} and acetic acid (HAc). The phase and morphology of the as-prepared product were characterized by means of powder X-ray diffraction (XRD), energy dispersive spectrometry (EDS), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Some factors influencing the formation of octahedral Fe{sub 4}(PO{sub 4}){sub 3}(OH){sub 3} microcrystals were systematically investigated, including the reaction temperature, time, and the molar ratio of Na{sub 2}SO{sub 3}/HAc.

• OSTI ID: 22215741
• Journal Information: Materials Research Bulletin, Journal Name: Materials Research Bulletin Journal Issue: 9 Vol. 47; ISSN MRBUAC; ISSN 0025-5408
• Country of Publication: United States
• Language: English

Related Subjects

36 MATERIALS SCIENCE
CRYSTAL GROWTH
CRYSTALS
HYDROTHERMAL SYNTHESIS
INORGANIC COMPOUNDS
IRON PHOSPHATES
SCANNING ELECTRON MICROSCOPY
SODIUM HYDRIDES
X-RAY DIFFRACTION
X-RAY PHOTOELECTRON SPECTROSCOPY