Ag doped α-Fe2O3 nanoparticles: Synthesis,characterization and application as heterogeneous photocatalyst for removal of organic dye from aqueous media without any oxidizing agents

α-Fe₂O₃ and Ag doped α-Fe₂O₃ nanostructures were synthesized by wet chemical reflux method. XRD analysis established formation of α-Fe₂O₃ phase for un-doped nanostructures while for Ag-α-Fe₂O₃ the diffraction peaks shift slightly towards higher angle. FESEM suggests the development of fine nanostructures with particle size order of 40–70 ​nm for pristine α-Fe₂O₃ NPs, whereas comparatively larger size NPs with order of 60–110 ​nm for Ag-α-Fe₂O₃. The NPs were used as photocatalysts for degradation of eosin yellow and malachite green dyes in aqueous medium under visible light irradiation. Ag-α-Fe₂O₃ NPs efficiently decolourize about 98% dye molecules within 90 ​min.     

Support Morphology Effect on Selective Hydrogenation of 3-Nitrostyrene to 3-Vinylaniline over Pt/α-Fe2O3 Catalysts

Selective hydrogenation of substituted nitroaromatic compounds is an extremely important and challenging reaction. Supported metal catalysts attract much attention in this reaction because the properties of metal nanoparticles (NPs) can be modified by the nature of the support. Herein, the support morphology on the catalytic performance of selective hydrogenation of 3-nitrostyrene to 3-vinylaniline was investigated. Pt NPs supported on octadecahedral α-Fe₂O₃ supports with a truncated hexagonal bipyramid shape (Pt/α-Fe₂O₃-O) and rod-shaped α-Fe₂O₃ supports (Pt/α-Fe₂O₃-R) were prepared by glycol reduction method. Detailed characterizations reveal that the electronic structure and dispersion of Pt NPs can be modified by the supports. The Pt/α-Fe₂O₃-O catalyst exhibited superior catalytic performance for hydrogenation of 3-nitrostyrene because of its low coordinated Pt sites and the small Pt NPs size, which is benefit from the high-index exposed surfaces of truncated hexagonal bipyramid-shaped α-Fe₂O₃ support. The structural evolution during the catalytic reaction was investigated in detail by identical location transmission electron microscopy (IL-TEM) method, which found that the high cycling activity of Pt/α-Fe₂O₃-O catalyst during the cycle experiment results from the stability of Pt NPs.     

Activation of α-Fe2O3 for Photoelectrochemical Water Splitting Strongly Enhanced by Low Temperature Annealing in Low Oxygen Containing Ambient

Photoelectrochemical (PEC) water splitting is a promising method for the conversion of solar energy into chemical energy stored in the form of hydrogen. Nanostructured hematite (α-Fe₂O₃) is one of the most attractive materials for a highly efficient charge carrier generation and collection due to its large specific surface area and the short minority carrier diffusion length. In the present work, the PEC water splitting performance of nanostructured α-Fe₂O₃ is investigated which was prepared by anodization followed by annealing in a low oxygen ambient (0.03 % O₂ in Ar). It was found that low oxygen annealing can activate a significant PEC response of α-Fe₂O₃ even at a low temperature of 400 °C and provide an excellent PEC performance compared with classic air annealing. The photocurrent of the α-Fe₂O₃ annealed in the low oxygen at 1.5 V vs. RHE results as 0.5 mA cm⁻², being 20 times higher than that of annealing in air. The obtained results show that the α-Fe₂O₃ annealed in low oxygen contains beneficial defects and promotes the transport of holes; it can be attributed to the improvement of conductivity due to the introduction of suitable oxygen vacancies in the α-Fe₂O₃. Additionally, we demonstrate the photocurrent of α-Fe₂O₃ annealed in low oxygen ambient can be further enhanced by Zn-Co LDH, which is a co-catalyst of oxygen evolution reaction. This indicates low oxygen annealing generates a promising method to obtain an excellent PEC water splitting performance from α-Fe₂O₃ photoanodes.     

Catalytic effect investigation of α-Fe2O3 and α-Fe2O3-CMS nanocomposites on the thermal behavior of NC/DEGDN mixture: DSC measurements and kinetic modeling

In this work, the thermal behavior and kinetics of energetic systems containing α-Fe₂O₃ and iron oxide–carbon mesospheres (α-Fe₂O₃-CMS) with nitrocellulose (NC)/diethylene glycol dinitrate (DEGDN)-based composites have been investigated using differential scanning calorimetry DSC and four isoconversional kinetic methods, respectively. The obtained results indicate that NC/DEGDN show only one decomposition peak, corresponding to the decomposition of the nitrate esters. Furthermore, the introduction of α-Fe₂O₃ and α-Fe₂O₃-CMS have lowered the peak temperature by 3.1 °C and 4.7 °C, respectively. Besides, the activation energy of the thermal decomposition of NC/DEGDN was decreased by 11.9 kJ/mol and 27.97 kJ/mol, after the introduction of α-Fe₂O₃ NPs and α-Fe₂O₃ NPs supported on CMS. These results confirm the good catalytic effect of the added catalysts on the thermal decomposition of the NC/DEGDN mixtures. However, the best catalytic effect was provided by the α-Fe₂O₃-CMS. Furthermore, the three considered systems were found to decompose according to different integral models g(α).     

Efficient photocatalytic degradation of methyl orange dye using facilely synthesized α-Fe2O3 nanoparticles

In this paper, α-Fe₂O₃ nanoparticles were fabricated via the combustion process using glucose and sucrose as organic fuels for the first time. The fabricated products were characterized using XRD, FT-IR, HR-TEM, and UV–vis spectrophotometer. The average crystallite size of the α-Fe₂O₃ samples, which were synthesized using glucose and sucrose fuels, is 27.25 and 6.13 nm, respectively. The HR-TEM images confirmed the presence of spherical and irregular shapes with an average diameter of 31.92 and 8.83 nm for the α-Fe₂O₃ samples, which were synthesized using glucose and sucrose fuels, respectively. The optical energy gap of the α-Fe₂O₃ samples, which were synthesized using glucose and sucrose fuels, is 2.00 and 2.48 eV, respectively. Additionally, the synthesized α-Fe₂O₃ samples were employed as a photocatalyst for the degradation of methyl orange dye under UV irradiations in the absence and presence of hydrogen peroxide. The optimum pH, irradiation time, and dose of α-Fe₂O₃ that achieved the highest degradation efficiency in the presence of hydrogen peroxide (82.17 % in the case of using an α-Fe₂O₃ sample which was synthesized using glucose or 95.31 % in the case of using an α-Fe₂O₃ sample which was synthesized using sucrose) are 3, 100 min, and 0.05 g, respectively.     

α-Fe2O3 nanoflowers: synthesis,characterization, electrochemical sensing and photocatalytic property

Nanoflower structured α-Fe₂O₃ was synthesized by adding hexamine to an aqueous solution of ferrous sulphate followed by drying and annealing at 600 °C for 6 h. X-ray diffraction analysis, Fourier-transformed infrared spectroscopy, Raman and DRS UV–visible absorption spectroscopy showed the formation of α-Fe₂O₃ with good crystalline nature. Field emission-scanning electron microscopy investigation revealed that the α-Fe₂O₃ has flower-like morphology, which is composed of nanorods. Cyclic voltammetry and chronoamperometry were used to investigate their electrochemical sensing property towards uric acid (UA). α-Fe₂O₃ exhibited enhanced sensing behavior with respect to that of bare GCE. Additionally, the α-Fe₂O₃ nanoflowers exhibit better photocatalytic activity of up to 71.7 % against rhodamine B (RhB) in short time of 60 min under visible light irradiation. It is found that the smaller crystallite size and flower-like morphology play a vital role in allowing an interaction between α-Fe₂O₃ and UA or RhB dye which enhances both the electrochemical sensing and photocatalytic activity.     

Improve the catalytic activity of α-Fe2O3 particles in decomposition of ammonium perchlorate by coating amorphous carbon on their surface

Sphere- and pod-like α-Fe₂O₃ particles have been selectively synthesized using NH₃·H₂O and NaOH solution to adjust the pH value of the designed synthetic system, respectively. The sphere-like α-Fe₂O₃ particles with diameter about 25 nm on average were encapsulated into carbon shells to fabricate a novel core-shell composite (α-Fe₂O₃@C) through the coating experiments. The catalytic performance of the products on the thermal decomposition of ammonium perchlorate (AP) was investigated by thermal gravimetric analyzer (TG) and differential thermal analysis (DTA). The thermal decomposition temperatures of AP in the presence of pod-like α-Fe₂O₃, sphere-like α-Fe₂O₃ and α-Fe₂O₃@C are reduced by 72, 81 and 109 °C, respectively, which show that α-Fe₂O₃@C core-shell composites have higher catalytic activity than that of α-Fe₂O₃.     

Ultrathin-layer α-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> deposited under hematite for solar water splitting

This work proposes a new strategy to prepare a hematite (α-Fe₂O₃) bilayer photoanode by hydrothermally depositing α-Fe₂O₃ (B) on the α-Fe₂O₃ (A) films prepared by electrochemical deposition. Compact smooth surfaced α-Fe₂O₃ (A) films were electrochemically deposited on FTO (SnO₂:F) substrates from an aqueous bath. The α-Fe₂O₃ (A), α-Fe₂O₃ (B), and α-Fe₂O₃/α-Fe₂O₃ bilayer films’ characteristics were defined by X-ray diffraction (XRD) measurements, field emission scanning electron microscopy (FESEM), and energy-dispersive X-ray (EDX) spectroscopy. Pure crystalline α-Fe₂O₃ (B) films with a typical anisotropic-like nanoparticle formation, which exhibited nanostructured rods covering the substrate and formed the characteristic mesoporous film morphology, were hydrothermally deposited on α-Fe₂O₃ (A) films prepared by electrochemical depositing in a solution bath at 25 °C and a potential of ??0.15 V. The photocurrent measurements exhibited increased intrinsic surface states (or defects) at the α-Fe₂O₃ (A)/α-Fe₂O₃ (B) interface. The photoelectrochemical performance of the α-Fe₂O₃ (A)/α-Fe₂O₃ (B) structure was examined by chronoamperometry, which found that the α-Fe₂O₃ (A)/α-Fe₂O₃ (B) structure exhibited greater photoelectrochemical activity than the α-Fe₂O₃ (A) and α-Fe₂O₃ (B) thin films. The highest photocurrent density was obtained for the bilayer α-Fe₂O₃ (A)/α-Fe₂O₃ (B) films in 1 M NaOH electrolyte. This great photoactivity was ascribed to the highly active surface area, and to the externally applied bias that favored the transfer and separation of photogenerated charge carriers in α-Fe₂O₃ (A)/α-Fe₂O₃ (B). The improved photocurrent density was attributed to an appropriate band edge alignment of semiconductors and to enhanced light absorption by both semiconductors. The best performing samples were α-Fe₂O₃ (A)/α-Fe₂O₃ (B), which reached the maximum incident photon conversion efficiencies (IPCE) of 400 nm at the potential of 0.1 V. In this case, the IPCE values were 3-fold higher than those of the α-Fe₂O₃ (A) and α-Fe₂O₃ (B) films.     

Chitosan-mediated synthesis of mesoporous α-Fe2O3 nanoparticles and their applications in catalyzing selective oxidation of cyclohexane

This paper reports the chitosan-mediated synthesis of porous hematite nanoparticles with FeCl₃ as the precursor via a hydrothermal approach at 160 °C. A series of porous chitosan/iron oxide hybrid nanoparticles were obtained via changing the ratio of chitosan to FeCl₃, FeCl₃ concentration and pH value of the reaction solution, and producing porous iron oxide nanoparticles after calcination. The as-prepared samples were characterized by means of X-ray diffraction, transmission electron microscopy, thermal gravimetric analysis, Fourier transform infrared, and N₂ sorption. The particle sizes of these metal oxides were less than 100 nm, and the pore sizes were in the range of 2–16 nm. It was demonstrated that chitosan played a key role in the formation of the porous structures. The resultant α-Fe₂O₃ nanoparticles were used as the support to immobilize Au or Pd nanoparticles, producing Au/α-Fe₂O₃ or Pd/α-Fe₂O₃ nanoparticles. The as-prepared α-Fe₂O₃ nanocatalyst exhibited high selectivity towards cyclohexanone and cyclohexanol for catalyzing cyclohexane oxidation with O₂ at 150°C.     

The influence of hematite nano-crystals on the thermal stability of polystyrene

A synthetic procedure based on thermal hydrolysis of iron(III) chloride solutions for the preparation of hematite (α-Fe₂O₃) sol consisting of nano-crystals (NCs) is described. The α-Fe₂O₃ NCs were characterized by transmission electron microscopy and X-ray diffraction measurements. Incorporation of α-Fe₂O₃ NCs into polystyrene (PS) was based on the transfer of α-Fe₂O₃ NCs from the aqueous phase to the organic solvent. A significant shift in the glass transition temperature of PS by 17 °C towards higher temperatures was observed after incorporation of α-Fe₂O₃ NCs. Also, the thermal stability of PS was improved by about 100 °C in the presence of 3.6 wt% of α-Fe₂O₃ NCs.     

A Green,Low-Cost and Efficient Photocatalyst: Atomic-Hydrogenated α-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>

The environmental-friendly hematite iron oxide (α-Fe₂O₃) has important application prospects in the photocatalysis field owing to its narrow indirect band gap. Here, we report a band gap engineering of α-Fe₂O₃ by incorporation of electrochemically-generated atomic hydrogen at moderate conditions. The ultraviolet–visible spectra show the reduction of the α-Fe₂O₃ band gap after hydrogenation and the absorption region from 200–800 nm is enhanced, especially in the visible light region. First principles calculation reveals the mixing of the new hybrid energy level with the valence band top resulting in a decrease in the band gap of α-Fe₂O₃. Further photocatalytic degradation experiments of dyes demonstrate that the photocatalytic efficiency of α-Fe₂O₃ can be greatly enhanced by the atomic hydrogen incorporation. The hydrogenated α-Fe₂O₃ can be easily recycled by magnets and has good photocatalytic stability. These findings offer possibilities for utilizing this inexpensive and earth-abundant oxide materials in the pollution controlling areas.     

Influence of cubic α-Fe2O3 particles on the thermal stability of poly(methyl methacrylate) synthesized by in situ bulk polymerization

Poly(methyl methacrylate)/α-Fe₂O₃ composites were prepared by in situ bulk radical polymerization of methyl methacrylate in the presence of the cubic α-Fe₂O₃ particles using 2,2′-azobisisobutyronitrile as initiator. The cubic α-Fe₂O₃ particles were synthesized by forced hydrolysis of FeCl₃ and characterized by X-ray diffraction analysis and transmission electron microscopy. The molar masses and molar mass distribution of synthesized PMMA samples were determined by gel permeation chromatography. The influence of α-Fe₂O₃ filler particles on the thermal properties of the PMMA matrix was investigated using thermogravimetry and differential scanning calorimetry. The molar mass and polydispersity of PMMA extracted from composite samples were not influenced by cubic α-Fe₂O₃ particles. The obtained composites have better thermal and thermooxidative stability than pure PMMA. On the other hand, the values of the glass transition temperature of composite samples were identical to the glass transition temperature of pure PMMA.     

Combination of α-Fe2O3, CdS and reduced graphene oxide: high-performance and recyclable visible light photocatalysis

A magnetic heterogeneous α-Fe₂O₃/CdS-RGO (RGO: reduced graphene oxide) composite photocatalyst was synthesized using the one-step hydrothermal method. The α-Fe₂O₃ and CdS nanoparticles with a diameter range of 20~60 nm were synchronously loaded/distributed on the surface of RGO. The as-synthesized α-Fe₂O₃/CdS-RGO nanocomposites were analyzed using X-ray diffraction, Fourier transform-infrared spectra, BET surface area, scanning electron microscopy, transmission electron microscopy, UV–Vis diffusive reflectance spectra and Raman spectroscopy. Compared with the pure CdS, α-Fe₂O₃ and α-Fe₂O₃/CdS nanoparticles, the α-Fe₂O₃/CdS-RGO nanocomposites expanded the adsorption range of visible-light, and showed significant photocatalytic performance and cyclic stability for degradation of methylene blue in visible light. Also, the remarkable catalytic performances mainly depend on its special structure of the α-Fe₂O₃/CdS-RGO, which enabled the effective separation of the electron–hole pairs. These attractive features make the α-Fe₂O₃/CdS-RGO nanocomposite to be a photocatalyst with great application potential in water pollutants treatment.     

Study of Microwave Torch Plasmachemical Synthesis of Iron Oxide Nanoparticles Focused on the Analysis of Phase Composition

This work presents the results obtained on the single-step route towards the synthesis of iron oxide nanoparticles in a microwave plasma torch. The torch is supplied by 660 sccm of Ar mixed with 1 sccm of Fe(CO)₅ and a variable amount of O₂. The influence of oxygen addition on the phase composition of the synthesized powder was studied. Magnetite and maghemite phases could not be distinguished using the standard X-ray diffraction (XRD) analysis. Therefore, a combined XRD and Raman spectra analysis had to be applied, which is based on fitting of selected diffraction peaks and spectral features. According to XRD and Raman spectroscopy, the powder synthesized from Ar/Fe(CO)₅ consisted about 50 % of magnetite, Fe₃O₄, the rest being α-Fe and FeO. An increase in oxygen flow rate led to an increase in γ-Fe₂O₃ percentage, at the expense of α-Fe, FeO and Fe₃O₄. Almost pure γ-Fe₂O₃ was synthesized at oxygen flow rates 25–75× higher than the flow rate of Fe(CO)₅. A further increase in the oxygen flow rate led to α-Fe₂O₃ and ε-Fe₂O₃ production. The distributions of nanoparticles’ (NPs) diameters were obtained using transmission electron microscopy (TEM) and dynamic light scattering (DLS). The mean diameter of the NPs measured by TEM was 13 nm while the DLS measurements led to the mean diameter of 12 nm. About 90 % of all particles had the diameter in the range of 5–21 nm but a few larger particles were observed in TEM micrographs.     

Novel sol–gel method for preparation of high concentration ε-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>/SiO<Subscript>2</Subscript> nanocomposite

ε-Fe₂O₃/SiO₂ nanocomposite was prepared by novel solgel method using single precursor for both nanoparticles and matrix. This method allows to prepare the samples free of α-Fe₂O₃ with 40% of Fe₂O₃ in SiO₂. Nanoparticles of 12 nm diameter were obtained by annealing at 1,000 °C. The samples were characterized by powder X-ray diffraction and transmission electron microscopy. Mössbauer spectroscopy identified ε-Fe₂O₃ as the only magnetically ordered phase at room temperature. Magnetic measurements revealed progressive necking of hysteresis loops measured at 300 and 2 K. In both cases the intrinsic coercivity reaches only 0.25 T. Measurements up to 14 T shows monotonous decreasing trend of saturated magnetization with increasing temperature.     

Synthesis of porous hematite nanorods loaded with CuO nanocrystals as catalysts for CO oxidation

Porous hematite (α-Fe2O3) nanorods with the diameter of 20-40 nm and the length of 80-300 nm were synthesized by a simple surfactant-assisted method in the presence of cetyltrimethylammonium bromide (CTAB).The α-Fe2O3 nanorods possess a mesostructure with a pore size distribution in the range of 5-12 nm and high surface area,exhibiting high catalytic activity for CO oxidation.CuO nanocrystals were loaded on the surface of porous α-Fe2O3 nanorods by a deposition-precipitation method,and the catalysts exhibited superior activity for catalytic oxidation of CO,as compared with commercial α-Fe2O3 powders supported CuO catalyst.The enhanced catalytic activity was attributed to the strong interaction between the CuO nanocrystals and the support of porous α-Fe2O3 nanorods.     

Synthesis and electrochemical properties of regular hexahedron α-Fe2O3

Synthesis of α-Fe₂O₃ compound with regular hexahedron shape is firstly reported. X-ray diffraction and scan electron microscope are used to characterize the structure and morphology of the prepared sample, respectively. The average edge length of hexahedron is about 0.9 μm. A reaction mechanism has been proposed. The pH value is a crucial factor for the formation and shape of α-Fe₂O₃. Moreover, electrochemical impedance spectroscopy and charge-discharge test of α-Fe₂O₃ as anode material in lithium ion batteries are evaluated. The data indicate that the synthesized regular hexahedron α-Fe₂O₃ can show better electrochemical properties than that of the commercial.     

Influence of temperatures and starting materials used to prepare α-Fe2O3 on its catalytic activity at the thermal decomposition of KClO4

In order to elucidate the influence of preparative history of α-Fe₂O₃ on its reactivity, the catalytic thermal decomposition of KClO₄ by α-Fe₂O₃ was studied by means of DTA and X-ray techniques. The catalysts were prepared by the calcination of three iron salts, Fe(OH)(CH₃COO)₂, FeSO₄ ? 7H₂O and Fe₂(SO₄)₃ ? αH₂O, at temperatures of 500–1200°C in air. The lower the preparation temperature of αFe₂O₃, the larger the specific surface area and reversely the smaller the crystalline size. KClO₄ without α-Fe₂O₃ was found to begin fusion and decomposition simultaneously at about 530°C. The addition of αFe₂O₃ resulted in promotion of the decomposition reaction of KClO₄; a lowering of 30–110°C in the initial decomposition temperature and a solid-phase decomposition before fusion of KClO₄. The influence of preparative history of α-Fe₂O₃ on the decomposition mainly depended on the preparation temperature rather than the starting material. The initial decomposition temperature of KClO₄ increased with an increase of the preparation temperature of α-Fe₂O₃. The effect of α-Fe₂O₃ was discussed on the basis of the charge transfer and the oxygen abstraction models.     

Binary α-Fe2O3–Co3O4 nanostructures for advanced oxidation process: Role of synergy for enhanced catalysis

Iron and its binary oxides are meticulously exploited for environmental remediations. However, only limited studies have been carried out on the degradation of industrial organics by advanced oxidation process. In this study, iron oxide, cobalt oxide, and iron–cobalt binary oxides were synthesized by a modified hydrothermal method as heterogeneous Fenton-like catalysts for the removal of methylene blue (MB) from wastewaters. The oxide nanostructures were characterized by different analytical techniques. Studying the effects of various parameters such as catalyst dose, MB concentration, and H₂O₂ concentration, the reaction conditions were optimized to enhance the removal of MB dye. The results revealed that α-Fe₂O₃–Co₃O₄ shows much higher activity than both Co₃O₄ and α-Fe₂O₃ for the degradation of MB at room temperature and beyond. The binary α-Fe₂O₃–Co₃O₄ shows degradation efficiency of 96.4% at 65 °C within 60 min. Furthermore, the binary α-Fe₂O₃–Co₃O₄ catalyst retains its activity for up to four successive cycles. A probable mechanism is also proposed, involving the generation of ‧OH radical as well as Fe²⁺/Fe³⁺ or Co²⁺/Co³⁺ redox couple of the binary α-Fe₂O₃–Co₃O₄ catalyst.     

Synthesis of Silica@α-Fe2O3 nanospheres by surface-initiated ATRP

We reported a new method to prepare Silica@α-Fe₂O₃ nanospheres by surface-initiated atom transfer radical polymerization (ATRP). Firstly, polymerizable surfactants-modified α-Fe₂O₃ nanoparticles were prepared in water-toluene microemulsion. Then, as-synthesized α-Fe₂O₃ nanoparticles acted as the macro-monomer of surface-initiated ATRP on silica nanospheres to make target product. Morphological characterization of the product was performed using transmission electron microscopy (TEM). Fourier transform infrared (FTIR), X-ray photoelectron spectroscopy (XPS) and diffuse reflectance UV-vis spectroscopy were used to verify the incorporation of α-Fe₂O₃ nanoparticles on silica nanosphere.