One-pot synthesis of α-Fe2O3 nanospheres by solvothermal method
© Wang et al.; licensee Springer. 2013
Received: 19 March 2013
Accepted: 22 April 2013
Published: 6 May 2013
We have successfully prepared α-Fe2O3 nanospheres by solvothermal method using 2-butanone and water mixture solvent for the first time, which were about 100 nm in diameter and composed of very small nanoparticles. The as-prepared samples were characterized using X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The results showed that the product was α-Fe2O3 nanosphere, and the temperature was an important factor on the formation of α-Fe2O3 nanospheres.
In the past decade, iron oxides have attracted an enormous amount of interest because of their great scientific and technological importance in catalysts, pigments, and gas sensors [1–3]. Among these iron oxides, α-Fe2O3, which is the most stable iron oxide with n-type semiconducting properties under ambient conditions, is the most researched and most frequently polymorphed in nature as the mineral hematite. Hematite has a rhombohedrally centered hexagonal structure of the corundum type with a close-packed oxygen lattice in which two-thirds of the octahedral sites are occupied by Fe3+ ions . Recently, a lot of researches have been carried out on α-Fe2O3 due to its low cost and nontoxic property as an anode material for lithium-ion secondary batteries [5–7]. In fact, all researches have almost focused on the preparation of α-Fe2O3 nanostructured materials, because nanoscale materials often exhibit physical and chemical properties that differ greatly from their bulk counterparts. Various α-Fe2O3 with nanostructures have been prepared, such as nanoparticles [5, 8–10], nanorods , nanotubes , flower-like structures , hollow spheres , nanowall arrays , dendrites , thin film [17, 18], and nanocomposites [19–21].
In this work, we report one-pot method to prepare α-Fe2O3 nanospheres by solvothermal method using 2-butanone and water mixture solvent for the first time. The product is α-Fe2O3 nanosphere with an average diameter of approximately 100 nm, which is composed of a lot of very small nanoparticles. The temperature takes an important influence on the formation of α-Fe2O3 nanospheres.
In a typical experimental synthesis, 0.1 g of Fe(NO3)3∙9H2O (≥ 99.0%) was dissolved in 3 mL of deionized H2O under stirring. Then, 37 mL of 2-butanone was added to the above solution. The mixture was stirred for about 10 min and then was sealed in a Teflon-lined stainless steel autoclave (50-mL capacity). The autoclave was maintained in an oven at 140°C for 12 h. The crude product was washed with anhydrous ethanol three times and finally dried in a vacuum chamber at 60°C for 10 h. The products were characterized by powder X-ray diffraction (XRD) performed on a Philips X'Pert diffractometer (Amsterdam, Netherlands) with CuKα radiation (λ = 1.54178 Ǻ). Scanning electron microscopy (SEM) images were taken on a JEOL JSM-6700F scanning electron microscope (Tokyo, Japan). Transmission electron microscopy (TEM) images and high-resolution TEM (HRTEM) images were obtained on the JEOL-2010 transmission electron microscope operating at 200 kV. The corresponding selected area electron diffraction (SAED) patterns were taken on a JEOL 2010 high-resolution TEM performing at 200 kV. The samples used for SEM, TEM, and HRTEM characterization were dispersed in absolute ethanol and were slightly ultrasonicated before observation.
Results and discussion
In conclusion, we have successfully prepared α-Fe2O3 nanospheres by solvothermal method using 2-butanone and water mixture solvent for the first time, which are about 100 nm in diameter and are composed of very small Fe2O3 nanoparticles. The temperature takes an important influence on the formation of the α-Fe2O3 nanospheres. The as-fabricated α-Fe2O3 nanospheres are expected to be applied in nanocatalysts, nanosensors, and lithium-ion secondary batteries.
CW got his PhD degree in 2012. He has devoted his effort in the research of two- and three-dimensional new materials for several years. His research interests focused on the fabrication and application of two and three-dimensional new materials. He has published his works in several important international journals. KT has main interest in superconductivity with high-temperature superconductors. YC mainly researches the preparation of new catalysts.
This work was supported by the National Natural Science Foundation of China (grant nos.: 91022033, 21171158, and 50903018) and the Foundation of Anhui Educational Committee (grant no.: KJ2012A217).
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