A simple one-step NaCl-assisted microwave-solvothermal method has been developed for the preparation of monodisperse α-Fe2O3 mesoporous microspheres. In this approach, Fe(NO3)3 · 9H2O is used as the iron source, and polyvinylpyrrolidone (PVP) acts as a surfactant in the presence of NaCl in mixed solvents of H2O and ethanol. Under the present experimental conditions, monodisperse α-Fe2O3 mesoporous microspheres can form via oriented attachment of α-Fe2O3 nanocrystals. One of the advantages of this method is that the size of α-Fe2O3 mesoporous microspheres can be adjusted in the range from ca. 170 to ca. 260 nm by changing the experimental parameters. High photocatalytic activities in the degradation of salicylic acid are observed for α-Fe2O3 mesoporous microspheres with different specific surface areas.

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Monodisperse α-Fe2O3 Mesoporous Microspheres: One-Step NaCl-Assisted Microwave-Solvothermal Preparation, Size Control and Photocatalytic Property

Selective catalytic reduction (SCR) of NO with NH3 over manganese substituted iron titanate catalysts was fully studied. The low temperature SCR activity was greatly enhanced when partial Fe was substituted by Mn, although the N-2 selectivity showed some decrease to a certain extent. The Mn substitution amounts showed obvious influence on the catalyst structure, redox behavior and NH3/NOx adsorption ability of the catalysts. Among FeaMn1-aTiOx (a = 1, 0.75, 0.5, 0.2, 0) serial catalysts, Fe0.5Mn0.5TiOx with the molar ratio of Fe:Mn = 1: 1 showed the highest SCR activity, because the interaction of iron, manganese and titanium species in this catalyst led to the largest surface area and the highest porosity, the severest structural distortion and most appropriate structural disorder, the enhanced oxidative ability of manganese species, the highest mobility of lattice oxygen, the proper ratio of Bronsted acid sites and Lewis acid sites together with the enhanced NOx adsorption capacity. (C) 2009 Elsevier B.V. All rights reserved.

Effect of manganese substitution on the structure and activity of iron titanate catalyst for the selective catalytic reduction of NO with NH3

Mesoporous non-siliceous oxides have attracted great interest due to their unique properties and potential applications. Since the discovery of mesoporous silicates in 1990s, organic–inorganic assembly processes by using surfactants or block copolymers as soft templates have been considered as a feasible path for creating mesopores in metal oxides. However, the harsh sol–gel conditions and low thermal stabilities have limited the expansion of this method to various metal oxide species. Nanocasting, using ordered mesoporous silica or carbon as a hard template, has provided possibilities for preparing novel mesoporous materials with new structures, compositions and high thermal stabilities. This review concerns the synthesis, composition, and parameter control of mesoporous non-siliceous oxides. Four synthesis routes, i.e. soft-templating (surfactants or block copolymers as templates), hard-templating (mesoporous silicas or carbons as sacrificial templates), colloidal crystal templating (3-D ordered colloidal particles as a template), and super lattice routes, are summarized in this review. Mesoporous metal oxides with different compositions have different properties. Non-siliceous mesoporous oxides are comprehensively described, including a discussion of constituting elements, synthesis, and structures. General aspects concerning pore size control, atomic scale crystallinity, and phase control are also reviewed.

Synthesis of non-siliceous mesoporous oxides

Effects of Fe-doping on the photocatalytic activity of mesoporous TiO2 powders prepared by an ultrasonic method.

α-Fe2O3 has been synthesized with an ordered mesoporous structure and crystalline walls that exhibit a near-single crystal-like order. The unique magnetic behavior of the material, distinct from bulk nanoparticles of α-Fe2O3 or mesoporous Fe2O3 with disordered walls, has been established. Magnetic susceptibility, Mossbauer, and neutron diffraction data show that the material possesses the same long-range magnetic order as bulk α-Fe2O3, despite the wall thickness being less than the 8 nm limit below which magnetic ordering breaks down in nanoparticulate α-Fe2O3, yet the Morin transition of bulk α-Fe2O3 is absent. It is also shown by TEM, PXRD, and EXAFS that α-Fe2O3 with the same ordered mesoporous structure but disordered walls contains small crystalline domains. Mossbauer and magnetic susceptibility data demonstrate that this material exhibits no long-range magnetic order but superparamagnetic behavior.

Ordered mesoporous Fe2O3 with crystalline walls.

Synthesis of mesoporous iron oxides has been reported using a sonochemical technique. Iron(III) ethoxide was used as an inorganic precursor and CTAB as an organic structure directing agent. After sonication the surfactant was removed by calcination and solvent extraction methods. FTIR spectra demonstrated the removal of the surfactant from the pores of the mesoporous iron oxide. The calcinated material was characterized by XRD, TEM, TGA, and BET surface area measurements. The surface area after solvent extraction is found to be 274 m2/g. The magnetic and catalytic properties of the materials have been studied. The as-prepared amorphous Fe2O3 has shown a paramagnetic behavior, while after calcination at 350 °C it changes to γ-Fe2O3 with good magnetic properties. The catalytic activity of mesoporous iron oxide was studied in the reaction of cyclohexane oxidation under mild conditions. The mesoporous Fe2O3 catalyst has shown high conversion of cyclohexane into cyclohexanone and cyclohexanol, with a high sele...

Sonochemical Synthesis of Mesoporous Iron Oxide and Accounts of Its Magnetic and Catalytic Properties

Synthesis of a composite mesoporous iron−titanium oxide by ultrasound irradiation is here reported. Iron(III) ethoxide and titanium(IV) isopropoxide were used as precursors, and dodecylamine was used as the templating agent. The synthesis was completed in 6 h in one stage. The product was characterized by XRD, TEM, DSC, TGA, XPS, EDX, and BET methods. Magnetic properties were studied by magnetization and Mossbauer spectroscopy. Short-range ordered structure of the product was demonstrated by low-angle XRD measurements. After heat treatment, this structure collapsed and crystalline phases of γ-Fe2O3 oxide and anatase of TiO2 were observed. The calcinated material showed slight magnetic properties corresponding to the amount of iron oxide. The removal of the surfactant by extraction with diluted nitric acid resulted in the increase of surface area to 650 m2/g and the pore volume to 0.45 mL/g. The catalytic properties of the material were examined in the oxidation of cyclohexane under mild conditions, and a ...

A Mesoporous Iron−Titanium Oxide Composite Prepared Sonochemically

Ultrasound radiation has been recently used for the synthesis of mesoporous materials (MSPM). The main advantages are manifested in the short preparation time and thicker walls leading to a more hydrothermally stable structure.1 This preparation method has already been reviewed.2 The discovery of MSP materials led immediately to the development of many experimental methods for the deposition of materials, especially catalytic materials, into the mesopores. Impregnation, thermal spreading, ion adsorption, and the most recent method3 in which colloidal gold solution is premixed with the precursors for the preparation of the MSPM, are among the methods used for the insertion of materials into the mesopores. Sonochemistry was also employed for this purpose. We will outline in this article the use of the sonochemical processes for the insertion of nanomaterials into the pores of MSPM. We will explain how this process is conducted, to what extent the materials are deposited in the pores and what is the mechanis...

N. Perkas

Papers

Sonochemical Synthesis of Mesoporous Iron Oxide and Accounts of Its Magnetic and Catalytic Properties

A Mesoporous Iron−Titanium Oxide Composite Prepared Sonochemically

The Sonochemical Insertion of Nanomaterials into Mesostructures

The Sonochemical Insertion of Nanomaterials into Mesostructures