Synthesis of nanostructured high specific surface area iron (III) oxide using a home-made supercritical carbon dioxide dryer

Document Type : Research Article

Authors

Department of Chemical, Petroleum, and Gas Engineering, Iran University of Science and Technology, Tehran, Iran

Abstract

This study aimed to produce nanostructured iron (III) oxide with a high surface area and high porosity. Iron (III) oxide was synthesized using the sol-gel method. The resulting gels were dried using two different methods, i.e., ambient drying (at 80 oC) and supercritical carbon dioxide drying. The produced iron oxide aerogel and xerogel were then calcined at 350 oC for 4 hours. The physico-chemical properties of the iron (III) oxide nanostructures were investigated using X-ray diffraction (XRD), nitrogen adsorption-desorption, and field emission scanning electron microscopy (FE-SEM) analyses. The results showed that the iron (III) oxide aerogel consisted of spherical nanoparticles. The X-ray diffraction pattern demonstrated the aerogel had a crystalline phase of pure hematite (α-Fe2O3). In addition, the produced aerogel had a specific surface area of 140 m2/g, the volume of porosities was 0.32 cm3/g, and the average diameter of pores was 8.9 nm. The produced xerogel also had a specific surface area of 65 m2/g, a volume of porosities of 0.18 cm3/g, and an average pore diameter of 10.8 nm. Therefore, the results of BET analysis confirmed that drying of iron oxide nanostructures using the supercritical drying method can lead to better preservation of its porous structure.

Keywords

Main Subjects


[1] Moral M., Rueda M., Mato R. Martín Á., "View Cell Investigation of Silica Aerogels During Supercritical Drying: Analysis of Size Variation and Mass Transfer Mechanisms", J. Supercritical Fluids, 92: 24-30 (2014).
[2] Stergar J. Maver1U., "Review of Aerogel-Based Materials in Biomedical Applications", J. Sol-Gel Sci Technol, 77: 738-752 (2016).
[3] Smirnova I. Gurikov P., "Aerogels in Chemical Engineering : Strategies toward Tailor-Made Aerogels", J. Review of Chemical and Biomolecular Engineering, 8: 307-334 (2018).
[4] Pierre C. Pajonk M., "Chemistry of Aerogels and Their Applications", J. Chem. Rev, 102: 4243-4266 (2002).
[5] Ganesan K., Budtova T., Ratke L., Gurikov P., Baudron V., Preibisch I., Niemeyer P., Smirnova I. Milow B., "Review on the Production of Polysaccharide Aerogel Particles", J. Materials, 11: 21-44 (2018).
[6] Ziegler C., Wolf A., Liu W., Herrmann K., Gaponik N., Eychmgller A., "Modern Inorganic Aerogels", J. Angew.Chem. Int. Ed, 56: 13200-13221 (2017).
[7] Kawagishi K., Saito H., Furukawa H. Horie K.,"Superior Nanoporous Polyimides via Supercritical CO2 Drying of Jungle-Gym-Type Polyimide Gels", J. of Macromol Rapid Commun, 28: 96-100 (2007).
[8] Pierre C., "History of Aerogels", J. Materials and Technologies, Springer. New York, NY, 3-18, (2011).
[9] Barrios B., Calderon J., "Aerogel Composites : A Review" J. Polymers, 11: 726 (2019).
[10] Mißfeldt F., Gurikov P., Lo..lsberg W., Weinrich D., Lied F., Fricke M., Smirnova I., "Continuous Supercritical Drying of Aerogel Particles: Proof of Concept", J. Ind. Eng. Chem. Res, 59: 11284-11295 (2020).
[11] Gonzáleza A., Camino-Reya C., Alnaiefb M., Zetzla C. Smirnovaa I., "Supercritical Drying of Aerogels Using CO2: Effect of Extraction Time on the End Material Textural Properties", J. Supercritical Fluids, 66: 297-30617 (2012).
[12] Sui R. Charpentier P., "Synthesis of Metal Oxide Nanostructures by Direct Sol−Gel Chemistry in Supercritical Fluids", J. Chem. Rev, 112: 3057-3082 (2012).
[13] Gash A., Tillotson T., Satcher J., John J. Poco F., "Use of Epoxides in the Sol-Gel Synthesis of Porous Iron (III) Oxide Monoliths from Fe (III) Salts", J. Chem. Mater, 13: 999-1007 (2001).
[14] Gash E., Satcher H., Simpson L. "Strong Akaganeite Aerogel Monoliths Using Epoxides: Synthesis and Characterization", J. Chem. Mater, 15: 3268-3275 (2003).
[15] Kido Y., Nakanishi K., Miyasaka A., Kanamori K., "Synthesis of Monolithic Hierarchically Porous Iron-Based Xerogels from Iron (III) Salts via an Epoxide-Mediated Sol−Gel Process," J. Chem. Mater, 24: 2071-2077 (2012).
[17] Cornell R. M., Schwertmann U., "The Iron Oxides: Structure, Properties, Reactions, Occurrences and Uses", Wiley-VCH, Weinheim, (2003).
[19] Tillotson T. M., Gash A. E., Simpson R. L., Hrubesh L. W., Satcher Jr J. H., Poco J. F., "Nanostructured Energetic Materials Using Sol–Gel Methodologies ", J. Non-Cryst. Solids, 285: 338-345 (2001).
[20] Bommel J. Haan B., "Drying of Silica Gels with Supercritical Carbon Dioxide", J. Materials Science, 29: 943-948 (1994).
[22] Kazemi H., Shahhosseini S., Bazyari A., Amiri M., "A study on the effects of textural properties of γ-Al2O3 support on CO2 capture capacity of Na2CO3 ", J. Process Safety and Environmental Protection, 138: 176-185 (2020).
[23] Arvaneh R., Fard A. A., Bazyari A., Alavi S. M., Abnavi F. J., "Effects of Ce, La, Cu, and Fe promoters on Ni/MgAl2O4 catalysts in steam reforming of propane", J. Korean Journal of Chemical Engineering, 36: 1033-1041 (2019).
[24] Azizzadeh Fard, A., Bazyari, A., Alavi, S. M., Aghamiri, A. R., "The effects of cobalt and cerium promoters on hydrogen production performance of alumina‐supported nickel catalysts in propane steam reforming", J. Chemical Technology & Biotechnology, 95: 3241-3251 (2020).
[25] Tomić1 Z., Marija M., Vuksanović1, Veljović2Đ., Đokić1 V. Aleksandar D., "Photocatalytic Degradation of Bisphenol with α-Fe2O3 Fibers and Particles ", J. Science of Sintering, 51: 265-276 (2019).