Synthesis and Characterization of Nanocapsules of α-Fe(NiCoAl) Solid-solution

α-Fe(NiCoAl) solid-solution nanocapsules were prepared with pure powders of Fe, Ni, Co and Al by the plasma arc-discharging using a copper crucible. The shapes of the nanocapsules are in polyhedrons with the core/shell structure. The body centered cubic (BCC) phase is formed in the core. The size of the nanocapsules is in the range of 10-120 nm and the thickness of the shell is 4-11 nm. Saturation magnetization JS=150 Am2/kg and coercivity iHC=24.3 kA/m are achieved for the nanocapsules.     

Synthesis and Characterization of Nanocapsules of α-Fe(NiCoAl) Solid-solution

α-Fe(NiCoAl) solid-solution nanocapsules were prepared with pure powders of Fe, Ni, Co and Al by the plasma arc-discharging using a copper crucible. The shapes of the nanocapsules are in polyhedrons with the core/shell structure. The body centered cubic (BCC) phase is formed in the core. The size of the nanocapsules is in the range of 10～120 nm and the thickness of the shell is 4～11 nm. Saturation magnetization Js=150 Am2/kg and coercivity iHC=24.3 kA/m are achieved for the nanocapsules.     

Arsenic (III,V) removal from aqueous solution by ultrafine α-Fe2O3 nanoparticles synthesized from solvent thermal method

Ultrafine iron oxide (α-Fe₂O₃) nanoparticles were synthesized by a solvent thermal process and used to remove arsenic ions from both lab-prepared and natural water samples. The α-Fe₂O₃ nanoparticles assumed a near-sphere shape with an average size of about 5 nm. They aggregated into a highly porous structure with a high specific surface area of ∼162 m²/g, while their surface was covered by high-affinity hydroxyl groups. The arsenic adsorption experiment results demonstrated that they were effective, especially at low equilibrium arsenic concentrations, in removing both As(III) and As(V) from lab-prepared and natural water samples. Near the neutral pH, the adsorption capacities of the α-Fe₂O₃ nanoparticles on As(III) and As(V) from lab-prepared samples were found to be no less than 95 mg/g and 47 mg/g, respectively. In the presence of most competing ions, these α-Fe₂O₃ nanoparticles maintained their arsenic adsorption capacity even at very high competing anion concentrations. Without the pre-oxidation and/or the pH adjustment, these α-Fe₂O₃ nanoparticles effectively removed both As(III) and As(V) from a contaminated natural lake water sample to meet the USEPA drinking water standard for arsenic.     

Preparation and Characterization of Fe3O4 Magnetic Nano-particles by 60Co γ-ray Irradiation

By using a new method, ^60Co γ-ray irradiation, Fe3O4 magnetic nano-particles were successfully synthesized at room temperature under ambient pressure. The structure, morphology and magnetic properties of these nanoparticles were characterized by X-ray diffraction （XRD）, transmission electron microscope （TEM） and vibrating sample magnetometer （VSM）, respectively. The radiation formation mechanism was also discussed. The results show that the absorbed dose can greatly influence the structure, morphology and magnetic properties of the products. XRD and TEM studies show that the product prepared by γ-ray irradiation （10 kGy） is pure FesO4 phase and the mean diameter of these nano-particles is about 21 nm. The Fe3O4 nano-particles synthesized by γ-ray irradiation （10 kGy） are mainly in small cubic shape and the size uniformity of these particles is good.     

Location of different phases in oxidized ultrafine FeCr (70:30) alloy particles

Slow or fast oxidation of ultrafine FeCr alloy particles leads to a core/shell like microstructure (1). A slowly oxidized sample revealed FeO (wüstite) and spinel oxide FeCr₂O₄ to be located at the shell, which is built up of very small crystals (3–5 nm). The FeO phase is observed to be very stable, being still present 360 days after the oxidation. The core consists usually of a bcc FeCr alloy, however, some particles contain the σ-FeCr phase, which is the expected form during slow cooling of FeCr particles.A fast oxidized sample contains only two phases, namely °-Fe₂O₃ and CrO₃, which coexist at the shell, leaving the core empty or filled with a lightly scattering substance, e.g. a gas. The outer surface of the shell is CrO₃ free but consists of °-Fe₂O₃. However, CrO₃ is located at the core/shell interface and forms a homogeneous layer around the core and is therefore not mixed with °-Fe₂O₃, which is built up of 10–20 nm crystals.     

Melting of thin γFe–C films having (100), (110) and (111) surfaces in terms of molecular dynamics simulation

Structural changes associated with melting of thin γFe–C films having (100), (110) and (111) surfaces have been investigated by molecular dynamics simulation. Structures of thin film and bulk models of γFe containing about 0–4 at.% C were calculated at constant temperatures between 1000 and 1800 K. The liquidus temperature for each thin film model decreased with increasing the C concentration. Comparison between the atomic number density distributions of Fe and C showed: (i) The atomic number density of C near the surface increases before the formation of liquid near the surface. (ii) This increase becomes more prominent as temperature rises. (iii) Melting of γFe–C alloy would be rate-controlled by diffusion of C from the solid phase to the solid–liquid interface. These findings suggest that the increase in the C concentration enhances atomic vibrations of Fe near the surface and promotes melting of Fe at lower temperatures. Furthermore, it has been concluded from Lindemann’s law of melting that surface melting occurs in γFe–C alloy having (110) surface more easily.     

Structural behavior of laser-irradiated γ-Fe2O3 nanocrystals dispersed in porous silica matrix : γ-Fe2O3 to α-Fe2O3 phase transition and formation of ε-Fe2O3

The effects of laser irradiation on γ-Fe₂O₃ 4 ± 1 nm diameter maghemite nanocrystals synthesized by co-precipitation and dispersed into an amorphous silica matrix by sol-gel methods have been investigated as function of iron oxide mass fraction. The structural properties of γ-Fe₂O₃ phase were carefully examined by X-ray diffraction and transmission electron microscopy. It has been shown that γ-Fe₂O₃ nanocrystals are isolated from each other and uniformly dispersed in silica matrix. The phase stability of maghemite nanocrystals was examined in situ under laser irradiation by Raman spectroscopy and compared with that resulting from heat treatment by X-ray diffraction. It was concluded that ε-Fe₂O₃ is an intermediate phase between γ-Fe₂O₃ and α-Fe₂O₃ and a series of distinct Raman vibrational bands were identified with the ε-Fe₂O₃ phase. The structural transformation of γ-Fe₂O₃ into α-Fe₂O₃ occurs either directly or via ε-Fe₂O₃, depending on the rate of nanocrystal agglomeration, the concentration of iron oxide in the nanocomposite and the properties of silica matrix. A phase diagram is established as a function of laser power density and concentration.     

Unique magnetic properties of single crystal γ-Fe2O3 nanowires synthesized by flame vapor deposition

Single crystal γ-Fe(2)O(3) nanowires with 40-60 nm diameters were grown for the first time by single-step atmospheric flame vapor deposition (FVD) with axial growth rates up to 5 μm/minute. Because of their superior crystallinity, these FVD γ-Fe(2)O(3) nanowires are single magnetic domains with room temperature coercivities of 200 Oe and saturation magnetizations of 68 emu/g.     

Characterization of oxygen passivated iron nanoparticles and thermal evolution to γ-Fe2O3

Nanocrystalline iron powders have been prepared by the inert gas evaporation method. After preparation the material has been passivated by pure oxygen and air exposure. In the present paper we describe new characterization studies of this sample by Transmission Electron Microscopy (TEM), X-ray Diffraction (XRD), X-ray Absorption Spectroscopy (XAS), Electron Energy Loss Spectroscopy (EELS) and Mössbauer Spectroscopy (MS), giving a complete chemical and structural characterization of the nanocomposite material in order to correlate its microstructure with its singular magnetic behavior.This nanocomposite was later heated following different thermal treatments. It was found that the sample heated successively in high vacuum (10^–7 torr) at 383 K for 1 h and under a residual oxygen pressure of 4 × 10^–4 torr at 573 K for 3 h, results in a powder formed by nanoparticles of -Fe₂O₃ as stated from XRD, XAS and MS. This material is stable during several years and behaves almost totally like superparamagnetic at room temperature.     

Modification of γ-(Fe,Cr)3C pseudo-binary eutectic

The -(Fe, Cr)₃C pseudo-binary eutectic alloy with K, Ce, Sb additives was unidirectionally solidified in a Brigdman-type unit. The quasi-regular, lamellar eutectic carbide was changed into rods and bent blades by the modifiers under well-controlled conditions. At very slow growth, partial modification was common. At growth rates corresponding to a slightly cellular interface, a fully modified structure could be obtained. The modification behaviour as a function of the modifying element, its concentration and the growth rate is described and discussed.     

The surface chemical properties of cobalt-modified γ-Fe2-O3 magnetic particles

The surface chemical properties of cobalt-modified -Fe₂O₃ (Co--Fe₂O₃) magnetic particles were studied by adsorption isotherms, FT-i.r. spectroscopy and microcalorimetry. The monolayer-adsorption amount of water on Co--Fe₂O₃ surfaces is 4.8 molecules per square nanometre, and the surface is considered to be covered with a thin water film in its normal environment. The surface hydrophilicity of Co--Fe₂O₃ is comparable to that of TiO₂. The acidic carboxyl group shows the strongest interaction with Co--Fe₂O₃, and a portion of this group chemically interacts. The basic amino group indicates stronger interaction with Co--Fe₂O₃ than the neutral hydroxyl group. It is concluded that the Co--Fe₂O₃ surface possesses a basic rather than an acidic character. This is interpreted in terms of the inherent nature of the adsorption site of Co--Fe₂O₃. Furthermore, the Co--Fe₂O₃ adsorption site appears to be energetically heterogeneous.     

Some magnetic properties of γ-Fe2O3 synthesized from ferrous fumarate half-hydrate

-Fe₂O₃ synthesized from ferrous fumarate half-hydrate was studied by measurements of D.c. electrical conductivity, Seebeck coefficient, initial magnetization and magnetic hysteresis, and by Mössbauer spectroscopy and scanning electron microscopy. The phase transformation observed by electrical conductivity measurements matched well with the phase transformation observed by the variation with temperature of initial magnetization measurements of -Fe₂O₃; this magnetic study also established the single-domain character of -Fe₂O₃. The magnetic hysteresis values of the -Fe₂O₃ synthesized indicated improved values over that of a -Fe₂O₃ sample synthesized by established procedures. The scanning electron micrographs showed that the -Fe₂O₃ particles were acicular in shape and the Mössbauer spectrum showed a well-resolved six-band spectrum. The presence of a hydrogen ferrite phase was also confirmed by the electrical and magnetic measurements.Deceased, 10 October, 1985.     

Behaviour of α-Fe2O3 (hematite), prepared by oxidation precipitation of ferrous sulphate,on heating

The effects of heating-Fe₂O₃ (hematite) prepared by oxidation precipitation of ferrous sulphate, at temperatures up to 700° C were studied. It was found that, in the course of heating, losses of structurally-bound water occured, accompanied by the formation and removal of pores, the lattice constants changed and the optical properties were modified, an effect which is important from the standpoint of the use of hematite as ferric pigment. With increasing annealing temperature, the complementary wavelength was shifted to higher values and the spectral purity of the pigment colour was decreased.     

Synthesis of maghemite (γ-Fe2O3) nanoparticles by thermal-decomposition of magnetite (Fe3O4) nanoparticles

In this research work, we prepared γ-Fe₂O₃ nanoparticles by thermal-decomposition of Fe₃O₄. The Fe₃O₄ nanoparticles were synthesized via co-precipitation method at room temperature. This simple, soft and cheap method is suitable for preparation of iron oxide nanoparticles (γ-Fe₂O₃; Fe₃O₄). The samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), vibrating sample magnetometer and differential scanning calorimeter (DSC). The XRD and FT-IR results indicated the formation of γ-Fe₂O₃ and Fe₃O₄ nanoparticles. The TEM images showed that the γ-Fe₂O₃ and Fe₃O₄ were spherical, and their size was 18 and 22 nm respectively. Magnetic properties have been measured by VSM at room temperature. Hysteresis loops showed that the γ-Fe₂O₃ and Fe₃O₄ nanoparticles were super-paramagnetic.     

Influence of Ni(II), Cu(II) and Cr(III) on the formation,morphology and molecular adsorption properties of α-FeOOH rust particles prepared by aerial oxidation of neutral Fe(II) solutions

To elucidate the role of alloying metals such as Ni, Cu and Cr in weathering steels on the formation of α-FeOOH rust by atmospheric corrosion of the steels in industrial and urban districts, influence of alloying metal ions on the formation, morphology and adsorption properties of α-FeOOH particles synthesized by aerial oxidation of neutral FeSO₄ solution was examined. The addition of Cu(II) and Cr(III) dramatically suppresses the crystal growth of α-FeOOH and turns the rod-shaped α-FeOOH particles into nano-sized irregular ones. Besides, increase of amount of added Cr(III) forms the iron oxyhydroxysulfate named as Schwertmannite (Fe₈O₈(SO₄)(OH)₆). Whereas, the Ni(II) addition shows no noticeable influence on the growth of α-FeOOH crystal and particles. These results imply that the inhibitory effect of crystal and particle growth of α-FeOOH is in order of Cr(III)?>?Cu(II)?>>?Ni(II). The adsorption of CO₂ gas on the α-FeOOH particles is impeded by adding Cu(II) and Cr(III). Whereas, the formation of Schwertmannite by adding Cr(III) enhances the CO₂ and SO₂ adsorption. These results suggest that alloying Cu and Cr in weathering steels inhibit the crystal and particle growth of α-FeOOH to accelerate the formation of protective rust layer composed of fine α-FeOOH and/or Schwertmannite rust particles on the steels in urban and industrial atmosphere.     

The morphology of α-Fe crystals which grow in the amorphous Fe80(C1−xBx)20 alloys

Crystallization behaviour of amorphous Fe₈₀(C_1–x B _x )₂₀ alloys, obtained by splat-cooling technique, for x values ranging from zero to unity has been investigated mainly by transmission electron microscopy. The crystalline phase which first appeared in the amorphous matrix was -Fe for all alloys studied. However, the morphology of -Fe phase changed from a spherical shape for low x values to a watch-glass shape for intermediate x values and to dendritic for large x values. The nucleation of -Fe crystals was homogeneous for low x samples while preferred nucleation on edges and surfaces was noted for samples with higher x values. The final volume fraction of -Fe phase before the appearance of the second crystalline phase increased with the increase in x.     

Effect of zinc on the magnetic properties of acicular cobalt-modified γ-Fe2O3 particles

Acicular -FeOOH particles with a particle length of about 0.35 m and an axial ratio of about 7 were synthesized by the coprecipitation method using the reaction of FeCl₂-NaOH. The (Co, Zn)-modified -F₂O₃ particles were produced by absorbing Co²⁺ and Zn²⁺ ions on the surfaces of -FeOOH particles followed by dehydration, reduction and oxidation. The saturation magnetization and thermal stability of the coercivity of (Co, Zn)--Fe₂O₃ particles were all higher than those of Co--F₂O₃ particles. For the same (Co+Zn) content, the saturation magnetization of (Co, Zn)--Fe₂O₃ particles increased with increasing zinc content but the coercivity decreased.     

Synthesis and gas sensing properties of α-Fe(2)O(3)@ZnO core-shell nanospindles

α-Fe(2)O(3)@ZnO core-shell nanospindles were synthesized via a two-step hydrothermal approach, and characterized by means of SEM/TEM/XRD/XPS. The ZnO shell coated on the nanospindles has a thickness of 10-15 nm. Considering that both α-Fe(2)O(3) and ZnO are good sensing materials, we have investigated the gas sensing performances of the core-shell nanocomposite using ethanol as the main probe gas. It is interesting to find that the gas sensor properties of the core-shell nanospindles are significantly enhanced compared with pristine α-Fe(2)O(3). The enhanced sensor properties are attributed to the unique core-shell nanostructure. The detailed sensing mechanism is discussed with respect to the energy band structure and the electron depletion theory. The core-shell nanostructure reported in this work provides a new path to fabricate highly sensitive materials for gas sensing applications.     

Fabrication, growth mechanism, and characterization of α-Fe(2)O(3) nanorods

This work reports the facile synthesis of α-Fe(2)O(3) nanorods and nano-hexagons and its application as sunlight-driven photocatalysis. The obtained products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), scanning electron microscopy (SEM), diffused reflectance spectroscopy (DRUV-vis), Fourier transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS). The phase and crystallinity were confirmed from the XRD study. Electron microscopy study clearly indicates the formation of different morphologies of nanocrystals. These hematite nanostructures were used as a model system for studying the shape-dependent photocatalytic degradation of phenol, methylene blue, and congo red. Amongst all the nanostructured semiconductors, Pt-doped hematite nanorod showed 55% efficiency towards the decolonization of methylene blue and 63% toward congo red under sun light illumination. The difference in photocatalytic activity is discussed in terms of their crystallize size and morphological ordering.