skip to main content
OSTI.GOV title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Hematite homogeneous core/shell hierarchical spheres: Surfactant-free solvothermal preparation and their improved catalytic property of selective oxidation

Abstract

Solvothermal synthesis is an efficient synthetic method for preparing nano and micromaterials. Preparation of hematite through alcoholysis of ferric ion under solvothermal condition has been carried out at low concentrations. In this paper, Fe{sub 2}O{sub 3} homogeneous core/shell hierarchical nanostructures were synthesized via solvothermal treatment of FeCl{sub 3}{center_dot}6H{sub 2}O and ethanol. The achievements of such structures can be attributed to two important factors: high temperature and high concentration. Besides, the crystal water and reaction time were also important factors to the synthesis of hematite. The prepared samples were characterized using X-ray powder diffraction, Raman spectra, scanning electron microscopy equipped with an energy-dispersive X-ray spectrometer, transmission electron microscopy and Brunauer-Emmett-Teller surface area and pore size distribution. X-ray photoelectron spectroscopy showed a satellite peak at 719.8 eV, which is the characteristic peak of Fe(III). The formation mechanism of the spheres and the effects of the reactant concentrations and reaction temperatures have been discussed. Moreover, the enhanced catalytic activity of the spheres has also been investigated through oxidation of benzyl alcohol to benzaldehyde with high conversion (42%) and selectivity (95%). - Graphical abstract: Fe{sub 2}O{sub 3} homogeneous core/shell hierarchical microspheres were synthesized by solvothermal method. Owing to the special structure, the synthesized Fe{submore » 2}O{sub 3} microspheres exhibit a superior catalytic activity in benzyl oxidation. Highlights: Black-Right-Pointing-Pointer Hierarchical Fe{sub 2}O{sub 3} core/shell microspheres were synthesized. Black-Right-Pointing-Pointer Microspheres were assembled by {beta}-FeOOH. Black-Right-Pointing-Pointer The sample exhibits a superior catalytic activity and selectivity. Black-Right-Pointing-Pointer The high activity and selectivity are due to the hierarchical core/shell structure.« less

Authors:
 [1]; ;  [1];  [1]
  1. Institute of Functional Nano and Soft Materials and Jiangsu Key Laboratory for Carbon-Based Functional Materials and Devices, Soochow University, Box 32, 199 Ren-ai Road, Suzhou Industrial Park, Suzhou 215123 (China)
Publication Date:
OSTI Identifier:
21612859
Resource Type:
Journal Article
Journal Name:
Journal of Solid State Chemistry
Additional Journal Information:
Journal Volume: 185; Other Information: DOI: 10.1016/j.jssc.2011.11.003; PII: S0022-4596(11)00596-2; Copyright (c) 2011 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA); Journal ID: ISSN 0022-4596
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; BENZALDEHYDE; BENZYL ALCOHOL; CRYSTALS; ETHANOL; FERRITES; HEMATITE; IRON CHLORIDES; IRON OXIDES; MICROSPHERES; OXIDATION; RAMAN SPECTRA; SCANNING ELECTRON MICROSCOPY; SHELLS; SURFACE AREA; SURFACTANTS; SYNTHESIS; TRANSMISSION ELECTRON MICROSCOPY; X-RAY DIFFRACTION; X-RAY PHOTOELECTRON SPECTROSCOPY; X-RAY SPECTROMETERS; ALCOHOLS; ALDEHYDES; AROMATICS; CHALCOGENIDES; CHEMICAL REACTIONS; CHLORIDES; CHLORINE COMPOUNDS; COHERENT SCATTERING; DIFFRACTION; ELECTRON MICROSCOPY; ELECTRON SPECTROSCOPY; FERRIMAGNETIC MATERIALS; HALIDES; HALOGEN COMPOUNDS; HYDROXY COMPOUNDS; IODIDES; IODINE COMPOUNDS; IRON COMPOUNDS; IRON HALIDES; IRON IODIDES; IRON ORES; MAGNETIC MATERIALS; MATERIALS; MEASURING INSTRUMENTS; MICROSCOPY; MINERALS; ORES; ORGANIC COMPOUNDS; OXIDE MINERALS; OXIDES; OXYGEN COMPOUNDS; PHOTOELECTRON SPECTROSCOPY; SCATTERING; SPECTRA; SPECTROMETERS; SPECTROSCOPY; SURFACE PROPERTIES; TRANSITION ELEMENT COMPOUNDS

Citation Formats

Suoyuan, Lian, School of Chemical Engineering and Materials, Dalian Polytechnic University, Dalian 116034, Haitao, Li, Xiaodie, He, Kang Zhenhui, E-mail: zhkang@suda.edu.cn, Liu Yang, E-mail: yangl@suda.edu.cn, and Lee, Shuit Tong. Hematite homogeneous core/shell hierarchical spheres: Surfactant-free solvothermal preparation and their improved catalytic property of selective oxidation. United States: N. p., 2012. Web. doi:10.1016/j.jssc.2011.11.003.
Suoyuan, Lian, School of Chemical Engineering and Materials, Dalian Polytechnic University, Dalian 116034, Haitao, Li, Xiaodie, He, Kang Zhenhui, E-mail: zhkang@suda.edu.cn, Liu Yang, E-mail: yangl@suda.edu.cn, & Lee, Shuit Tong. Hematite homogeneous core/shell hierarchical spheres: Surfactant-free solvothermal preparation and their improved catalytic property of selective oxidation. United States. https://doi.org/10.1016/j.jssc.2011.11.003
Suoyuan, Lian, School of Chemical Engineering and Materials, Dalian Polytechnic University, Dalian 116034, Haitao, Li, Xiaodie, He, Kang Zhenhui, E-mail: zhkang@suda.edu.cn, Liu Yang, E-mail: yangl@suda.edu.cn, and Lee, Shuit Tong. 2012. "Hematite homogeneous core/shell hierarchical spheres: Surfactant-free solvothermal preparation and their improved catalytic property of selective oxidation". United States. https://doi.org/10.1016/j.jssc.2011.11.003.
@article{osti_21612859,
title = {Hematite homogeneous core/shell hierarchical spheres: Surfactant-free solvothermal preparation and their improved catalytic property of selective oxidation},
author = {Suoyuan, Lian and School of Chemical Engineering and Materials, Dalian Polytechnic University, Dalian 116034 and Haitao, Li and Xiaodie, He and Kang Zhenhui, E-mail: zhkang@suda.edu.cn and Liu Yang, E-mail: yangl@suda.edu.cn and Lee, Shuit Tong},
abstractNote = {Solvothermal synthesis is an efficient synthetic method for preparing nano and micromaterials. Preparation of hematite through alcoholysis of ferric ion under solvothermal condition has been carried out at low concentrations. In this paper, Fe{sub 2}O{sub 3} homogeneous core/shell hierarchical nanostructures were synthesized via solvothermal treatment of FeCl{sub 3}{center_dot}6H{sub 2}O and ethanol. The achievements of such structures can be attributed to two important factors: high temperature and high concentration. Besides, the crystal water and reaction time were also important factors to the synthesis of hematite. The prepared samples were characterized using X-ray powder diffraction, Raman spectra, scanning electron microscopy equipped with an energy-dispersive X-ray spectrometer, transmission electron microscopy and Brunauer-Emmett-Teller surface area and pore size distribution. X-ray photoelectron spectroscopy showed a satellite peak at 719.8 eV, which is the characteristic peak of Fe(III). The formation mechanism of the spheres and the effects of the reactant concentrations and reaction temperatures have been discussed. Moreover, the enhanced catalytic activity of the spheres has also been investigated through oxidation of benzyl alcohol to benzaldehyde with high conversion (42%) and selectivity (95%). - Graphical abstract: Fe{sub 2}O{sub 3} homogeneous core/shell hierarchical microspheres were synthesized by solvothermal method. Owing to the special structure, the synthesized Fe{sub 2}O{sub 3} microspheres exhibit a superior catalytic activity in benzyl oxidation. Highlights: Black-Right-Pointing-Pointer Hierarchical Fe{sub 2}O{sub 3} core/shell microspheres were synthesized. Black-Right-Pointing-Pointer Microspheres were assembled by {beta}-FeOOH. Black-Right-Pointing-Pointer The sample exhibits a superior catalytic activity and selectivity. Black-Right-Pointing-Pointer The high activity and selectivity are due to the hierarchical core/shell structure.},
doi = {10.1016/j.jssc.2011.11.003},
url = {https://www.osti.gov/biblio/21612859}, journal = {Journal of Solid State Chemistry},
issn = {0022-4596},
number = ,
volume = 185,
place = {United States},
year = {Sun Jan 15 00:00:00 EST 2012},
month = {Sun Jan 15 00:00:00 EST 2012}
}