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Title: Effect of iron oxide loading on the phase transformation and physicochemical properties of nanosized mesoporous ZrO{sub 2}

Abstract

Highlights: ► Modified preparation method for nanosized iron oxide supported ZrO{sub 2} catalysts. ► Systematic study of effect of high iron oxide loading over ZrO{sub 2}. ► Influence of iron oxide on the stabilization of tetragonal ZrO{sub 2} phase. ► A mesoporous nature of zirconia changed upon changing iron oxide loading. ► Surface to bulk migration of iron oxide evidenced by XPS technique. -- Abstract: Mesoporous ZrO{sub 2}-supported iron oxide materials were prepared with nominal loadings of iron oxide of 5, 10, 15 and 20 wt.% using a modified co-precipitation method. The physicochemical properties of the catalysts were characterized by thermogravimetric analysis, differential scanning calorimetry, X-ray diffraction, Raman spectroscopy, high resolution transmission electron microscopy, N{sub 2} adsorption, X-ray photoelectron spectroscopy and infrared spectroscopy methods. A delay in the ZrO{sub 2} phase transformation as a result of the incorporation of iron was determined using TG/DSC measurements. XRD, Raman spectroscopy and HRTEM results revealed that an increase of iron oxide loading from 5 to 15 wt.% enhanced the transformation of the monoclinic to tetragonal phase. Unexpectedly, 20 wt.% iron oxide loading was required for complete tetragonal structure stabilization due to the mesoporosity of the ZrO{sub 2} support. Iron oxide loadings from 5more » to 15 wt.% showed an increase in the BET-surface area due to the presence of amorphous iron oxide on the surface. XPS and FTIR results indicated that increasing the iron oxide content to 20 wt.% resulted in stabilization of the tetragonal zirconia phase as a result of surface-to-bulk migration and incorporation of Fe{sup 3+} ions in the ZrO{sub 2} lattice.« less

Authors:
 [1];  [1];  [2];  [1];  [3];  [1]
  1. Chemistry Department, Faculty of Science, King Abdulaziz University, P.O. Box 80203, 21589 Jeddah (Saudi Arabia)
  2. (Egypt)
  3. Petrochemicals Research Institute (PRI), King Abdulaziz City for Science and Technology (KACST), P.O. Box 6086, 11442 Riyadh (Saudi Arabia)
Publication Date:
OSTI Identifier:
22215586
Resource Type:
Journal Article
Journal Name:
Materials Research Bulletin
Additional Journal Information:
Journal Volume: 47; Journal Issue: 11; Other Information: Copyright (c) 2012 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA); Journal ID: ISSN 0025-5408
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 77 NANOSCIENCE AND NANOTECHNOLOGY; ABSORPTION SPECTROSCOPY; ADSORPTION; CALORIMETRY; FOURIER TRANSFORMATION; INFRARED SPECTRA; IRON IONS; IRON OXIDES; MONOCLINIC LATTICES; NANOSTRUCTURES; PHASE TRANSFORMATIONS; RAMAN SPECTROSCOPY; STABILIZATION; SURFACE AREA; SYNTHESIS; THERMAL GRAVIMETRIC ANALYSIS; TRANSMISSION ELECTRON MICROSCOPY; X-RAY DIFFRACTION; X-RAY PHOTOELECTRON SPECTROSCOPY; ZIRCONIUM OXIDES

Citation Formats

Basahel, S.N., Ali, Tarek T., Chemistry Department, Faculty of Science, Sohag University, 82524 Sohag, Narasimharao, K., Bagabas, A.A., and Mokhtar, M., E-mail: mmokhtar2000@yahoo.com. Effect of iron oxide loading on the phase transformation and physicochemical properties of nanosized mesoporous ZrO{sub 2}. United States: N. p., 2012. Web. doi:10.1016/J.MATERRESBULL.2012.07.003.
Basahel, S.N., Ali, Tarek T., Chemistry Department, Faculty of Science, Sohag University, 82524 Sohag, Narasimharao, K., Bagabas, A.A., & Mokhtar, M., E-mail: mmokhtar2000@yahoo.com. Effect of iron oxide loading on the phase transformation and physicochemical properties of nanosized mesoporous ZrO{sub 2}. United States. doi:10.1016/J.MATERRESBULL.2012.07.003.
Basahel, S.N., Ali, Tarek T., Chemistry Department, Faculty of Science, Sohag University, 82524 Sohag, Narasimharao, K., Bagabas, A.A., and Mokhtar, M., E-mail: mmokhtar2000@yahoo.com. Thu . "Effect of iron oxide loading on the phase transformation and physicochemical properties of nanosized mesoporous ZrO{sub 2}". United States. doi:10.1016/J.MATERRESBULL.2012.07.003.
@article{osti_22215586,
title = {Effect of iron oxide loading on the phase transformation and physicochemical properties of nanosized mesoporous ZrO{sub 2}},
author = {Basahel, S.N. and Ali, Tarek T. and Chemistry Department, Faculty of Science, Sohag University, 82524 Sohag and Narasimharao, K. and Bagabas, A.A. and Mokhtar, M., E-mail: mmokhtar2000@yahoo.com},
abstractNote = {Highlights: ► Modified preparation method for nanosized iron oxide supported ZrO{sub 2} catalysts. ► Systematic study of effect of high iron oxide loading over ZrO{sub 2}. ► Influence of iron oxide on the stabilization of tetragonal ZrO{sub 2} phase. ► A mesoporous nature of zirconia changed upon changing iron oxide loading. ► Surface to bulk migration of iron oxide evidenced by XPS technique. -- Abstract: Mesoporous ZrO{sub 2}-supported iron oxide materials were prepared with nominal loadings of iron oxide of 5, 10, 15 and 20 wt.% using a modified co-precipitation method. The physicochemical properties of the catalysts were characterized by thermogravimetric analysis, differential scanning calorimetry, X-ray diffraction, Raman spectroscopy, high resolution transmission electron microscopy, N{sub 2} adsorption, X-ray photoelectron spectroscopy and infrared spectroscopy methods. A delay in the ZrO{sub 2} phase transformation as a result of the incorporation of iron was determined using TG/DSC measurements. XRD, Raman spectroscopy and HRTEM results revealed that an increase of iron oxide loading from 5 to 15 wt.% enhanced the transformation of the monoclinic to tetragonal phase. Unexpectedly, 20 wt.% iron oxide loading was required for complete tetragonal structure stabilization due to the mesoporosity of the ZrO{sub 2} support. Iron oxide loadings from 5 to 15 wt.% showed an increase in the BET-surface area due to the presence of amorphous iron oxide on the surface. XPS and FTIR results indicated that increasing the iron oxide content to 20 wt.% resulted in stabilization of the tetragonal zirconia phase as a result of surface-to-bulk migration and incorporation of Fe{sup 3+} ions in the ZrO{sub 2} lattice.},
doi = {10.1016/J.MATERRESBULL.2012.07.003},
journal = {Materials Research Bulletin},
issn = {0025-5408},
number = 11,
volume = 47,
place = {United States},
year = {2012},
month = {11}
}