A mild solvothermal route to α-Fe2O3 nanoparticles

A mild solvothermal route has been developed to synthesize α-Fe₂O₃ nanoparticles using Fe(NO₃)₃ as a starting material. The results from XRD and TEM indicate the α-Fe₂O₃ powders possess a rhombohedrally centered hexagonal structure, and the size of particles from alcohothermal method at 160 °C is about 50-100 nm.     

Hydrothermal fabrication of various morphological α-Fe2O3 nanoparticles modified by surfactants

Two kinds of various morphological α-Fe₂O₃ nanoparticles modified by anionic surfactant (sodium dodecylsulfonate, SDS) and cationic surfactant (hexadecyipyridinium chloride, HPC), respectively, have been synthesized via hydrothermal method, using simple inorganic salt (NH₄)₃Fe(C₂O₄)₃ and alkali NaOH as starting precursors. Meanwhile, α-Fe₂O₃ nanoparticles without surfactant are also fabricated under the same conditions for comparison. The resultant products were characterized by means of Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), transmission electron micrograph (TEM) combined with electron diffraction (ED) and magnetization measurements. It is interesting that the obtained α-Fe₂O₃ nanoparticles without surfactant are polyhedral with average particle size of 90 ± 35 nm; while the obtained α-Fe₂O₃ nanoparticles modified by SDS are ellipsoidal with mean particle size of major axis: ca. 420 nm; minor axis: ca. 205 nm and those modified by HPC are spherical with mean particle size of ca. 185 nm observed from TEM. In addition, magnetic hysteresis measurements reveal that the α-Fe₂O₃ nanoparticles modified by two surfactants show enhancement in coercivity (H_c) and the remanent magnetization (M_r) compared with those of the obtained α-Fe₂O₃ nanoparticles without surfactant at room temperature. The experimental results suggest that the surfactants not only significantly influence the size and shape of the particles, but also their magnetic properties.     

Preparation of cobalt-zinc ferrite (Co0.8Zn0.2Fe2O4) nanopowder via combustion method and investigation of its magnetic properties

Cobalt-zinc ferrite (Co_0.8Zn_0.2Fe₂O₄) was prepared by combustion method, using cobalt, zinc and iron nitrates. The crystallinity of the as-burnt powder was developed by annealing at 700 °C. Crystalline phase was investigated by XRD. Using Williamson-Hall method, the average crystallite sizes for nanoparticles were determined to be about 27 nm before and 37 nm after annealing, and residual stresses for annealed particles were omitted. The morphology of the annealed sample was investigated by TEM and the mean particle size was determined to be about 30 nm. The final stoichiometry of the sample after annealing showed good agreement with the initial stoichiometry using atomic absorption spectrometry. Magnetic properties of the annealed sample such as saturation magnetization, remanence magnetization, and coercivity measured at room temperature were 70 emu/g, 14 emu/g, and 270 Oe, respectively. The Curie temperature of the sample was determined to be 350 °C using AC-susceptibility technique.     

The interaction of oxygen with high loaded Ru/γ-Al2O3 catalyst

The interaction of oxygen with the Ru/γ-Al₂O₃ catalyst comprising metal particle with sizes of 1-16 nm, was examined over a temperature range 20-400 °C. The catalyst loaded with 10.8 wt.% Ru was prepared by incipient wetness from RuCl₃ precursor. The structure of the Cl-containing catalyst and the catalyst after elimination Cl⁻ ions was characterized using H₂ and O₂ chemisorption, O₂ uptake, BET, XRD and TEM. The Cl⁻ ions in the catalyst decreased the H₂ and O₂ chemisorption capacity of Ru and caused large discrepancies between the mean particle size calculated from gas chemisorption and from TEM. Exposure to O₂ at 100-200 °C caused oxidation of small Ru particles, while larger particles were covered with very thin Ru_xO_y skin (undetected by XRD and TEM). The O/Ru ratio increased up to 200 °C implying high affinity of the small Ru particles to oxygen. Oxidation at 250 °C led to the formation of poorly crystalline RuO₂ particles with a mean size of 4 nm, and coverage of large Ru particles with 1.6 nm thick oxide layer. At 300 and 400 °C crystallization of the RuO₂ phase, as well as significant agglomeration of oxide particles was observed. However, even at 400 °C, metallic Ru was detected by XRD, TEM and SAED suggesting that large metal particles were not fully oxidized under the used conditions. Also, the O₂ uptake at 400 °C was lower than expected for oxidation of Ru metal to RuO₂. For the catalyst after elimination Cl ions the O₂ uptake (O/Ru ratio = 1.50) was higher, than for sample with large amount of Cl ions (O/Ru ratio = 1.34), indicating that the presence of Cl inhibits ruthenium oxidation in the Ru/Al₂O₃ catalyst.     

Temperature dependence of magnetic property and photocatalytic activity of Fe3O4/hydroxyapatite nanoparticles

Fe₃O₄/hydroxyapatite (HAP) nanoparticles have been developed as a novel photocatalyst support, based on the embedment of magnetic Fe₃O₄ particles into HAP shell via homogeneous precipitation method. The resultant nanoparticles were characterized by transmission electron microscope (TEM) and X-ray diffraction (XRD). These particles were almost spherical in shape, rather monodisperse and have a unique size of about 25 nm in diameter. The effect of calcination temperature on magnetic property and photocatalytic activity of Fe₃O₄/HAP nanoparticles was investigated in detail. The obtained results showed that the Fe₃O₄/HAP nanoparticles calcined at 400 °C possessed good magnetism and photocatalytic activity in comparison with that calcined at other temperatures.     

Hydrothermal synthesis of nanocrystalline VO2 from poly(diallyldimethylammonium) chloride and V2O5

Novel vanadium dioxide nanorods were fabricated from V₂O₅ in the presence of a reducing agent, the poly(diallyldimethylammonium chloride) (PDDA) via a hydrothermal method at 180 °C for 48 h. The samples produced were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), infrared spectroscopy (FTIR), nitrogen adsorption (BET) and thermogravimetry (TG/DTG). The nanorods obtained are approximately 50 nm wide and from 300 to 500 nm long and presents high surface area (42 m² g⁻¹). The nanocrystalline B phase VO₂ is not produced by hydrothermal treatment in the absence of the PDDA polyelectrolyte.     

Formation of NiFe2O4 nanoparticles by mechanochemical reaction

Preparation of nanosized NiFe₂O₄ particles by mechanochemical reaction(NiO+α-Fe₂O₃) and subsequent thermal treatment was investigated using X-ray diffraction (XRD). Thermal treatment of the as-milled powder at 700 °C for 1 h led to the formation of NiFe₂O₄ nanoparticles with an average crystal size of about 23 nm. Effect of thermal treatment temperature on the crystal size of the nanoparticles was studied. The mechanism of nanoparticles growth was primarily discussed. The activation energy of NiFe₂O₄ nanoparticle formation during calcination was calculated to be 16.6 kJ/mol.     

One-step hydrothermal process to prepare highly crystalline Fe3O4 nanoparticles with improved magnetic properties

Hydrothermal process was successfully used to synthesize Fe₃O₄ powder using ferrous chloride (FeCl₂) and diamine hydrate (H₄N₂·H₂O) as starting materials by carefully controlling the reaction conditions. The as-prepared Fe₃O₄ sample was characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM), and its magnetic properties were evaluated on a vibrating sample magnetometer (VSM). The nanoscale (40 nm) Fe₃O₄ powder obtained at 140 °C for 6 h possessed a saturation magnetization of 85.8 emu/g, a little lower than that of the correspondent bulk Fe₃O₄ (92 emu/g). It is suggested that the well-crystallized Fe₃O₄ grains formed under appropriate hydrothermal conditions should be responsible for the increased saturation magnetization in nanosized Fe₃O₄.     

Synthesis and characterization of Bi2Fe4O9 powders

Bi₂Fe₄O₉ have been successfully prepared using ethylenediaminetetraacetic (EDTA) acid as a chelating agent and ethylene glycol as an esterification agent. Heating of a mixed solution of EDTA, ethylene glycol, and nitrates of iron and bismuth at 140 °C produced a transparent polymeric resin without any precipitation, which after pyrolysis at 250 °C was converted to a powder precursor for Bi₂Fe₄O₉. The precursors were heated at 400–800 °C in air to obtain Bi₂Fe₄O₉ powder and differential scanning calorimetry (DSC), thermogravimetric (TG), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) techniques were used to characterize the precursors and the derived oxide powders. XRD analysis showed that well-crystallized and single-phase Bi₂Fe₄O₉ with orthorhombic symmetry was obtained at 700 °C for 2 h and BiFeO₃ and Fe₂O₃/FeCO₃ were intermediate phases before the formation of Bi₂Fe₄O₉. Bi₂Fe₄O₉ powders show weak ferromagnetism at room temperature.     

The effect of Cu content on the structure of Ni1−xCuxFe2O4 spinels

A series of Ni_1−xCu_xFe₂O₄ (0 ≤ x ≤ 0.5) spinels were synthesized employing sol-gel combustion method at 400 °C. The decomposition process was monitored by thermal analysis, and the synthesized nanocrystallites were characterized by X-ray diffraction, transmission electron microscopy, infra-red and X-ray photoelectron spectroscopy. The decomposition process and ferritization occur simultaneously over the temperature range from 280 °C to 350 °C. TEM indicates the increase of lattice parameter and particle size with the increase of copper content in accordance with the XRD analysis. Cu²⁺ can enter the cubic spinel phase and occupy preferentially the B-sites within x = 0.3, and redundant copper forms CuO phase separately. A broadening of the O 1s region increases with the increment of copper content compared to pure NiFe₂O₄, showing different surface oxygen species from the spinel and CuO. Cu²⁺ substitution favors the occupancy of A-sites by Fe³⁺.     

Preparation and characterization of the TiO2 ultrafine particles by detonation method

Utilizing the raw materials of TiOSO₄, NaOH, NH₄NO₃ and RDX, the TiO₂ ultrafine particles were prepared under high pressure and high temperature by detonation method. The structure, composition and size distribution of the TiO₂ ultrafine particles were systematically characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results indicated the as-prepared TiO₂ ultrafine particles exhibited spherical-like grains and that the average size of particles was 25 ± 5 nm. After being heated at 700 °C for 1 h, TiO₂ particles have entirely completed the anatase-rutile phase transition, which means that detonation method can effectively enhance the anatase-rutile phase transition by lowering the transition temperature. The size of TiO₂ nanoparticles can be effectively controlled because the as-prepared nanoparticles do not have enough time to grow to large and perfect crystallites during the detonation process.     

Synthesis of submicron-sized spherical Y2O3 powder for transparent YAG ceramics

Spherical monodispersed, submicron-sized Y₂O₃ powder was prepared via a homogeneous precipitation method using nitrate and urea as raw materials. The structure, phase evolution and morphology of Y₂O₃ precursor and the calcined powder were studied by FTIR, TG/DTA, XRD and SEM methods. The sphere size of the precursor was about 250 nm and that of Y₂O₃ powder calcined at 800 °C for 2 h was about 200-210 nm. With the spherical Y₂O₃ powder and a commercial Al₂O₃ ultrafine powder, high transparent YAG ceramics was fabricated by vacuum sintering at 1780 °C for 6 h through a solid-state reaction method. The in-line transmittances of the as-fabricated YAG ceramics at the wavelength of 1064 nm and 400 nm were 82.8% and 79.5%, respectively, which were much higher than that of the YAG ceramics with a commercial Y₂O₃ powder and a commercial Al₂O₃ ultrafine powder directly. The superior properties are attributed to the good morphology, dispersibility and uniform grain size of the as-prepared spherical Y₂O₃ powder, which matches that of the commercial Al₂O₃ powder.     

Synthesis and characterization of nanosized SrBi2Ta2O9 powder by a novel sol-gel process

Chemically homogeneous SrBi₂Ta₂O₉ (SBT) sol was synthesized using ethoxy tantalum, strontium acetate, and bismuth subnitrate as starting materials, methoxyethylene as a solvent and acetic acid (HOAc) as a catalyst. Single-phased perovskite phase SBT ferroelectric ultrafine powder was obtained after the dried gel was treated at 350°C for 30 min and calcined at 800°C for 1 h. FT-IR, XRD, TEM and TG-DTA were employed to investigate the transformation processes of sol to gel and gel to ultrafine SBT powder. Acetic acid not only acts as an acid catalyst, but also changes the alkoxide precursor as a ligand at a molecular level. Bidentate acetates replace OR groups and are directly bounded to the tantalum, leading to the formation of Ta (OR)_x(OAc)_5−x. The perovskite SBT phase formed via intermediate phase Bi₃TaO₇ and a Bi-deficient pyrocholore phase.     

Preparation and combustion properties of α-Fe2O3 coated Zr particles

Zirconium particles with irregular morphology and broad size distribution were uniformly coated by spherical α-Fe₂O₃ crystal grain via a facile route without polymer or surfactant as directing agents. The synthesized α-Fe₂O₃/Zr composite particles were characterized by X-ray diffraction, scanning electron microscopy, energy dispersion X-ray, UV-vis spectroscopy and Raman spectroscopy. The synthesis mechanism could be explained by cooperated heterogeneous nucleation and solid state transformation reaction. The combustion properties of α-Fe₂O₃/Zr composite particles were investigated. Compared with Zr particles, the combustion lasting time decreased from 16 s of Zr particles to 0.13 s of α-Fe₂O₃/Zr composite particles, and the top point of temperature reached in combustion increased from 2004 °C of Zr particles to 2378 °C of α-Fe₂O₃/Zr particles.     

Preparation and magnetic properties of spindle porous iron nanoparticles

Spindle porous iron nanoparticles were firstly synthesized by reducing the pre-synthesized hematite (α-Fe₂O₃) spindle particles with hydrogen gas. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption/desorption isotherms and vibrating sample magnetometry (VSM). A lattice shrinkage mechanism was employed to explain the formation process of the porous structure, and the adsorbed phosphate was proposed as a protective shell in the reduction process. N₂ adsorption/desorption result showed a Brunauer-Emmett-Teller (BET) surface area of 29.7 m²/g and a continuous pore size distribution from 2 nm to 100 nm. The magnetic hysteresis loop of the synthesized iron particles showed a saturation magnetization of 84.65 emu/g and a coercivity of 442.36 Oe at room temperature.     

Synthesis of nanocrystalline Mo2C via sodium co-reduction of MoCl5 and CBr4 in benzene

Molybdenum carbide (Mo₂C) has been synthesized via a sodium co-reduction of molybdenum pentachloride (MoCl₅) and carbon tetrabromide (CBr₄) in benzene at 350 °C for 12 h. X-ray diffraction (XRD) pattern indicated that the product was mainly hexagonal Mo₂C with a small amount of cubic Mo₂C. The lattice constants of the hexagonal Mo₂C were a=3.009 and c=4.736 Å. Transmission electron microscopy (TEM) study showed that the product consisted of slightly conglomerated particles of about 30 nm in size.     

Synthesis and electrochemical characterizations of nano-La2O3-coated nanostructure LiMn2O4 cathode materials for rechargeable lithium batteries

LiMn₂O₄ spinel cathode materials were coated with 1.0, 2.0 and 3.0 wt.% of La₂O₃ by polymeric process, followed by calcinations at 850 °C for 6 h in air. The surface coated LiMn₂O₄ cathode materials were physically characterized using X-ray diffraction, scanning electron microscopy, transmission electron microscopy and XPS. XRD patterns of La₂O₃-coated LiMn₂O₄ revealed that the coating did not affect the crystal structure and space group Fd3m of the cathode materials, compared to the uncoated LiMn₂O₄. The surface morphology and particle agglomeration were investigated using scanning electron microscopy and the TEM image showed a compact coating layer on the surface of the core materials that had average thickness of about 100 nm. XPS data illustrated that the La₂O₃ was completely coated over the surface of the LiMn₂O₄ core cathode materials. The galvanostatic charge and discharge of the uncoated and La₂O₃-coated LiMn₂O₄ cathode materials were carried out in the potential range of 3.0 and 4.5 V at 30 °C and 60 °C. Among them, 2.0 wt.% of La₂O₃-coated spinel LiMn₂O₄ cathode has improved the structural stability, high reversible capacity and excellent electrochemical performances of the rechargeable lithium batteries.     

Preparation and characterization of Y3Al5O12 (YAG) nano-powder by co-precipitation method

YAG precursor was synthesized by a co-precipitation method from a mixed solution of aluminum and yttrium nitrates with aqueous ammonia as the precipitator. The structure, phase evolution and morphology of YAG precursor and the sintered powders were studied by means of IR, TG/DTA, XRD, TEM methods. It was found the precursor with approximate composition of Al(OH)₃·0.3[Y₂(OH)₅·(NO₃)₂·2H₂O] directly transformed to pure-YAG phase at 800 °C and no intermediate phases were detected. YAG nanocrystalline powders from sintering the precursor at different temperatures were less-aggregated and the diameters of the grains were about 40-100 nm. BET surface area of the particles decreased with increase of calcination temperature and the powder sintered at 800 °C can be used for fabrication of transparent YAG ceramics.     

Synthesis and photoluminescence properties of SrLu2O4:Eu superfine phosphor

Superfine powder SrLu₂O₄:Eu³⁺ was synthesized with a precursor prepared by an EDTA - sol-gel method at relatively low temperature using metal nitrate and EDTA as starting materials. The heat decomposition mechanism of the precursor, formation process of SrLu₂O₄:Eu³⁺and the properties of the particles were investigated by thermo-gravimetric (TG) - differential thermal analysis (DTA), X-ray diffraction (XRD), transmission electron microscopy (TEM) and photoluminescence (PL) analyses. The results show that pure SrLu₂O₄:Eu³⁺ superfine powder has been produced after the precursor was calcinated at 900 °C for 2 h and has an elliptical shape and an average diameter of 80-100 nm. Upon excitation with 250 nm light, all the SrLu₂O₄:Eu³⁺ powders show red and orange emissions due to the 4f-4f transitions of Eu³⁺ ions. The highest photoluminescence intensity at 610 nm was found at a content of about 6 mol% Eu³⁺. Splitting of the ⁵D₀-⁷F₁ emission transition revealed that the Eu³⁺ ions occupied two nonequivalent sites in the crystallite by substituting Lu³⁺ ions.     

Nanoneedles of maghemite iron oxide prepared from a wet chemical route

Nanometer-sized maghemite iron oxide (γ-Fe₂O₃) particles were produced first by synthesis of a precursor, γ-FeO(OH), in a surfactant-less microemulsion and subsequent heat treatment of the γ-FeO(OH). The precursors and γ-Fe₂O₃ powder were characterized using thermogravimetric analysis (TGA), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Susceptometer from Quantum Design (SQUID) measurements. TGA and XRD analysis indicated the formation of single cubic phase when the samples were heat-treated at 240 °C. TEM reveals that the γ-Fe₂O₃ particles are needle-shaped with an aspect ratio of ∼20; typically 5-10 nm wide and over 150 nm long. It was found that these microemulsion-derived γ-Fe₂O₃ nanoneedles possess an intrinsic coercivity of 28 Oe at 300 K and 950 Oe at 2 K.