Synthesis of α-Fe2O3 nanobelts and nanoflakes by thermal oxidation and study to their magnetic properties

α-Fe₂O₃ nanobelts and nanoflakes have been successfully synthesized by oxidation of iron-coated ITO glass in air. The X-ray diffraction, Raman spectrum and scanning electron microscopy are carried out to characterize the nanobelts and nanoflakes. The formation mechanism has been presented. Significantly, the magnetic investigations show that the magnetic properties are strongly shape-dependent. The magnetization measurements of belt-like and flake-like α-Fe₂O₃ in perpendicular exhibit ferromagnetic feature with the coercivity (H_c) and saturation magnetization (M_s) of 334.5 Oe and 1.35 emu/g, 239.5 Oe and 0.12 emu/g, respectively. For the parallel, belt-like and flake-like α-Fe₂O₃ also exhibit ferromagnetic feature with the H_c and M_s of 205.5 Oe and 1.44 emu/g, 159.6 Oe and 0.15 emu/g, respectively.     

Magnetic properties of bio-synthesized zinc ferrite nanoparticles

The magnetic properties of zinc ferrite (Zn-substituted magnetite, Zn_yFe_1-yFe₂O₄) formed by a microbial process compared favorably with chemically synthesized materials. A metal reducing bacterium, Thermoanaerobacter, strain TOR-39 was incubated with Zn_xFe_1−xOOH (x=0.01, 0.1, and 0.15) precursors and produced nanoparticulate zinc ferrites. Composition and crystalline structure of the resulting zinc ferrites were verified using X-ray fluorescence, X-ray diffraction, transmission electron microscopy, and neutron diffraction. The average composition from triplicates gave a value for y of 0.02, 0.23, and 0.30 with the greatest standard deviation of 0.02. Average crystallite sizes were determined to be 67, 49, and 25 nm, respectively. While crystallite size decreased with more Zn substitution, the lattice parameter and the unit cell volume showed a gradual increase in agreement with previous literature values. The magnetic properties were characterized using a superconducting quantum interference device magnetometer and were compared with values for the saturation magnetization (M_s) reported in the literature. The averaged M_s values for the triplicates with the largest amount of zinc (y=0.30) gave values of 100.1, 96.5, and 69.7 emu/g at temperatures of 5, 80, and 300 K, respectively indicating increased magnetic properties of the bacterially synthesized zinc ferrites.     

Synthesis and magnetic properties of barium–calcium hexaferrite particles prepared by sol–gel and microemulsion techniques

The preparation of W-type hexaferrite particles with the composition BaCa₂Fe₁₆O₂₇ by microemulsion and a stearic acid sol–gel method with and without surfactant has been investigated at various sintering temperatures. The structural and magnetic characteristics have been studied by X-ray diffraction (XRD), a vibrating sample magnetometer (VSM), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), differential scanning calorimetric (DSC) and Fourier transform infrared (FTIR) techniques. The effect of sintering temperature on the properties of BaCa₂Fe₁₆O₂₇ hexaferrites has been studied. The value of saturation magnetization (M_s) depends on types of surfactant used. The sample prepared in the presence of polyoxyethylene (20) sorbitan monooleat (Tween 80) shows low saturation magnetization (M_s=15.10 emu/g), whereas the other sample prepared in the presence of a surfactant cetyltrimethylammonium bromide (CTAB) exhibits high saturation magnetization (M_s=24.60 emu/g) compared to the normal sample.     

Synthesis and characterization of Sr(ZnZr)x Fe12−2xO19-PANI composites

Strontium zinc zirconium hexaferrites/polyaniline (Sr(ZnZr)_xFe_12−2xO₁₉-PANI, x=0, 0.5, 1.0) composites were synthesized by oxidative chemical polymerization of aniline in the presence of ammonium peroxydisulfate (APS). The structure and morphology of the product was characterized by FTIR, TGA and SEM. The particle size of the core material was found to be about 250-500 nm. After coating with polyaniline, the particle size of Sr(ZnZr)_0.5Fe₁₁O₁₉-PANI composites grew upto 0.5-1.0 μm. XRD of the ferrites indicated that the structure of the core materials is hexagonal, with lattice constants around 5.886-5.885 Å. It was found that the saturation magnetization (M_S) and coercivity (H_C) for Sr(ZnZr)_xFe_12−2xO₁₉-PANI composites decreased after polyaniline coating. The composite under applied magnetic field, exhibited ferromagnetic hysteretic loops with high saturation magnetization (M_S=18.9-3.8 emu/g) and coercivity (H_C=3850.0-583.91 Oe).     

Magnetic characterization of dual phase FeZrB soft magnetic alloy

The magnetic properties and the annealing process of Fe₇₈Zr₇B₁₅ amorphous ribbons are investigated by X-ray diffraction (XRD), differential scanning calorimetry, and vibrating sample magnetometer. The fully amorphous structure of the as-quenched ribbons is confirmed by the XRD pattern. The Curie temperature and the saturation magnetization M_s of the ribbons are 305 °C and 124.3 emu/g, respectively. Annealing at 550 °C can result in an increase in M_s with annealing time due to the increasing crystallized volume fraction of α-Fe phase. The optimized annealing process is established at 550 °C for 20-30 min with maximum M_s of 146.6 emu/g. The morphology of the ribbons annealed at 550 °C is observed by scanning electron microscopy, showing that nanocrystalline α-Fe grains are dispersed in an amorphous matrix.     

Synthesis of magnetite nanorods and porous hematite nanorods

Fe₃O₄ nanorods with average diameters of 40-50 nm and lengths of up to 1 μm were synthesized through hydrolysis of FeCl₃ and FeSO₄ solutions containing urea in the temperature range from 90 to 95 °C in reflux condition for 12 h, following an aging time of 12 h. The porous hematite nanorods were prepared by calcination of the precursor which was obtained from hydrolysis of FeCl₃ and FeSO₄ solutions containing urea at a temperature of 90 °C for 10 h in hydrothermal condition. The formation of the porosity of hematite was due to the decomposition of FeCO₃ and FeOOH. Urea played a key role in the formation of the iron oxide nanorods. Transmission electron microscopy (TEM) images showed that the morphology of magnetite particles is homogeneous in the shape of rods and hematite rods are full of porosity. The values of saturation magnetization (M) and coercivity (H) of magnetite nanorods are 67.55 emu/g and 114 Oe, respectively. The samples were also characterized by X-ray powder diffraction (XRD) and electron diffraction (ED). At last, the forming mechanism of both the magnetite and porous hematite nanorods was discussed.     

Novel hybrid nanostructured materials of magnetite nanoparticles and pectin

A novel hybrid nanostructured material comprising superparamagnetic magnetite nanoparticles (MNPs) and pectin was synthesized by crosslinking with Ca²⁺ ions to form spherical calcium pectinate nanostructures, referred as MCPs, which were typically found to be 100-150 nm in size in dried condition, confirmed from transmission electron microscopy and scanning electron microscopy. The uniform size distribution was revealed from dynamic light scattering measurement. In aqueous medium the MCPs showed swelling behavior with an average size of 400 nm. A mechanism of formation of spherical MCPs is outlined constituting a MNP-pectin interface encapsulated by calcium pectinate at the periphery, by using an array of characterization techniques like zeta potential, thermogravimetry, Fourier transformed infrared and X-ray photoelectron spectroscopy. The MCPs were stable in simulated gastrointestinal fluid and ensured minimal loss of magnetic material. They exhibited superparamagnetic behavior, confirmed from zero field cooled and field cooled profiles and showed high saturation magnetization (M_s) of 46.21 emu/g at 2.5 T and 300 K. M_s decreased with increasing precursor pectin concentrations, attributed to quenching of magnetic moments by formation of a magnetic dead layer on the MNPs.     

Templated synthesis of monodisperse mesoporous maghemite/silica microspheres for magnetic separation of genomic DNA

A novel method is described for the preparation of superparamagnetic mesoporous maghemite (γ-Fe₂O₃)/silica (SiO₂) composite microspheres to allow rapid magnetic separation of DNA from biological samples. With magnetite (Fe₃O₄) and silica nanoparticles as starting materials, such microspheres were synthesized by the following two consecutive steps: (1) formation of monodispersed organic/inorganic hybrid microspheres through urea-formaldedyde (UF) polymerization and (2) removal of the organic template and phase transformation of Fe₃O₄ to γ-Fe₂O₃ by calcination at elevated temperatures. The as-synthesized particles obtained by heating at temperature 300 °C feature spherical shape and uniform particle size (d_particle=1.72 μm), high saturation magnetization (M_s=17.22 emu/g), superparamagnetism (M_r/M_s=0.023), high surface area (S_BET=240 m²/g), and mesoporosity (d_pore=6.62 nm). The composite microsphere consists of interlocked amorphous SiO₂ nanoparticles, in which cubic γ-Fe₂O₃ nanocrystals are homogeneously dispersed and thermally stable against γ- to α-phase transformation at temperatures up to 600 °C. With the exposed iron oxide nanoparticles coated with a thin layer of silica shell, the magnetic microspheres were used as a solid-phase adsorbent for rapid extraction of genomic DNA from plant samples. The results show that the DNA templates isolated from pea and green pepper displayed single bands with molecular weights greater than 8 kb and A₂₆₀/A₂₈₀ values of 1.60-1.72. The PCR amplification of a fragment encoding the endogenous chloroplast ndhB gene confirmed that the DNA templates obtained were inhibitor-free and amenable to sensitive amplification-based DNA technologies.     

Simultaneous variations of microstructure and magnetic properties of Ni58Fe12Zr20B10 nanostructure/amorphous alloy prepared by mechanical alloying

This study aims to evaluate magnetic and micro-structural properties of amorphous/nanocrystalline mechanically alloyed Ni₅₈Fe₁₂Zr₂₀B₁₀ powders with ball-milling time up to 190 h. Structural, micro-structural and thermal evaluations of the milled powders were carried out by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM) and differential scanning calorimetry (DSC) methods. Magnetic properties were also measured by a vibrating sample magnetometer (VSM) instrument. Results showed that the amorphous phase reached maximum value of 95% and the crystallite size was about 3 nm at the end of the milling. Magnetization saturation (M_s) decreased slightly and coercivity (H_c) reached to the highest value at 72 h of the milling time. At the 190 h of milling, the coercivity and saturation magnetization reached 18 Oe and 20 emu/g, respectively. While, after an appropriate amount of heat treatment, these two variables became approximately 2 Oe and 32 emu/g.     

Microstructure and magnetic properties of Ni-rich Ni54Mn25.7Ga20.3 ferromagnetic shape memory alloy thin film

A Ni₅₄Mn_25.7Ga_20.3 ferromagnetic shape memory alloy thin film has been fabricated by using the RF magnetron-sputtering technique. The structure and magnetic properties of the film were systematically investigated. The results show that the film is in ferromagnetic martensite state at room temperature with the Curie temperature (T_c) of about 370 K. The saturation magnetization (M_s) of the film reaches 45 emu/g at 300 K, which is about 80% as large as that of Ni–Mn–Ga bulk material. The magnetization hysteresis loops significantly depend on temperatures. The residual magnetization (M_r) and the coercive force (H_c) increase with decreasing temperatures. The grains homogeneously distribute in the film. The microstructure of the film consists of martensite plates. The interface between the martensite variants is clear and straight, indicating a good mobility.     

Synthesis of aqueous ferrofluids of ZnxFe3−xO4 nanoparticles by citric acid assisted hydrothermal-reduction route for magnetic hyperthermia applications

Superparamagnetic and monodispersed aqueous ferrofluids of Zn substituted magnetite nanoparticles (Zn_xFe_3−xO₄, x=0, 0.25, 0.3, 0.37 and 0.4) were synthesized via hydrothermal-reduction route in the presence of citric acid, which is a facile, low energy and environmental friendly method. The synthesized nanoparticles were characterized by X ray diffraction (XRD) analysis, Fourier transform infrared (FTIR) spectroscopy, scanning and transmission electron microscopy (SEM and TEM) and the dynamic light scattering (DLS) method. The results showed that a certain amount of citric acid was required to obtain single phase Zn substituted magnetite nanoparticles. Citric acid acted as a modulator and reducing agent in the formation of spinel structure and controlled nanoparticle size and crystallinity. Mean particle sizes of the prepared nanoparticles were around 10 nm. The results that are obtained from XRD, magnetic and power loss measurements showed that the crystallinity, saturation magnetization (M_S) and loss power of the synthesized ferrofluids were all influenced by the substitution of Zn in the structure of magnetite. The Zn substituted magnetite nanoparticles obtained by this route showed a good stability in aqueous medium (pH 7) and hydrodynamic sizes below 100 nm and polydispersity indexes below 0.2. The calculated intrinsic loss power (ILP) for the sample x=0.3 (e.g. 2.36 nH m²/kg) was comparable to ILP of commercial ferrofluids with similar hydrodynamic sizes.     

Structural, microstructural and magnetic properties of NiFe2O4, CoFe2O4 and MnFe2O4 nanoferrite thin films

The structural, microstructural and magnetic properties of nanoferrite NiFe₂O₄ (NF), CoFe₂O₄ (CF) and MnFe₂O₄ (MF) thin films have been studied. The coating solution of these ferrite films was prepared by a chemical synthesis route called sol-gel combined metallo-organic decomposition method. The solution was coated on Si substrate by spin coating and annealed at 700 °C for 3 h. X-ray diffraction pattern has been used to analyze the phase structure and lattice parameters. The scanning electron microscopy (SEM) and atomic force microscopy (AFM) have been used to show the nanostructural behavior of these ferrites. The values of average grain's size from SEM are 44, 60 and 74 nm, and from AFM are 46, 61 and 75 nm, respectively, measured for NF, CF and MF ferrites. At room temperature, the values of saturation magnetization, M_s∼50.60, 33.52 and 5.40 emu/cc, and remanent magnetization, M_r∼14.33, 15.50 and 1.10 emu/cc, respectively, are observed for NF, CF and MF. At low temperature measurements of 10 K, the anisotropy of ferromagnetism is observed in these ferrite films. The superparamagnetic/paramagnetic behavior is also confirmed by χ′(T) curves of AC susceptibility by applying DC magnetizing field of 3 Oe. The temperature dependent magnetization measurements show the magnetic phase transition temperature.     

Study of the magnetic and structural properties of Mn-, Fe-, and Co-doped ZnO powder

A study of the magnetic and structural properties of Zn_1−xM_xO powder (where x=0 or 0.01, and M=Mn, Fe or Co) produced by the proteic sol–gel process was undertaken. The sample crystal structure was analyzed by XRD and magnetic measurements were carried out in a SQUID magnetometer. Of the XRD analysis, all samples had hexagonal wurtzite crystal structure with P63mc space group, and no secondary phase was observed. It is observed of the M(H) measures at 2 K, that the Co- and Mn-doped ZnO displayed saturation magnetizations (M_s) of approximately 2 and 3.2 emu/g, respectively, and no remanence (M_r) was observed, indicating a superparamagnetic behavior in these samples. However, the Fe-doped sample showed a ferromagnetic behavior with M_s∼0.34 emu/g, M_r∼0.05 emu/g, and coercivity (H_c)∼1090 Oe. Already at room temperature, the M(H) measurements reveal a purely paramagnetic behavior for Mn- and Fe-doped ZnO, indicating that the Curie temperature (T_c) is below 300 K. However, a weak superparamagnetic behavior was observed in the Co-doped sample, indicating that T_c>300 K.     

Synthesis and surface modified hard magnetic properties in Co0.5Pt0.5 nanocrystallites from a rheological liquid precursor

Small crystallites of a metastable phase Co_0.5Pt_0.5 are precipitated by heating a rheological liquid precursor of cobalt–hydrazine complex and platinum chloride H₂PtCl₆·xH₂O in polymer molecules of poly(vinylpyrrolidone) (PVP) in ethylene glycol. The hydrazine co-reduces nascent atoms from the Co²⁺ and Pt⁴⁺ that recombine and grow as Co_0.5Pt_0.5. The PVP molecules cap a growing Co_0.5Pt_0.5 as it achieves a critical size so that it stops growing further in given conditions. X-ray diffraction pattern of a recovered powder reveals a crystalline Co_0.5Pt_0.5 phase (average crystallite size D∼8 nm) of a well-known Fm3m-fcc crystal structure with the lattice parameter a=0.3916 nm (density ρ=14.09 g/cm³). A more ordered L1₀ phase (ρ=15.91 g/cm³) transforms (D≥25 nm) upon annealing the powder at temperature lesser than 700 °C (in vacuum). At room temperature, the virgin crystallites bear only a small saturation magnetization M_s=5.54 emu/g (D=8 nm) of a soft magnet and it hardly grows on bigger sizes (D≤31 nm) in a canted ferromagnetic structure. A rectangular hysteresis loop is markedly expanded on an optimally annealed L1₀ phase at 800 °C for 60 min, showing a surface modified coercivity H_c=7.781 kOe with remnant ratio M_r/M_s=0.5564, and M_s=39.75 emu/g. Crystallites self-assembled in an acicular shape tailor large H_c from ideal single domains and high magnetocrystalline anisotropy of a hard magnet L1₀ phase.     

Structural and magnetic properties of self-assembled Sm-Co spherical aggregates

Self-assembled Sm-Co nanoparticles in the form of spherical aggregates (referred as nanospheres) with diameter ranging from 50 to 180 nm were achieved by means of polyol technique. The size distribution of the Sm-Co nanospheres can be regulated close to ∼100 nm by controlling the molar ratio of Sm:Co precursor. The spherical aggregates exhibited Sm₂Co₇ phase as a major constituent; while the aggregates obtained at higher Co concentration showed co-existence of Co-phase with Sm₂Co₇ phase. Upon annealing, the biphasic nature of nanospheres (Sm₂Co₇/Co) transformed into Sm₂Co₁₇ structure. By varying the Sm:Co precursor ratio from 1:5 to 1:9, the coercivity (H_c) and magnetization (M_s) values of the as-synthesized nanospheres can be tuned from 336 to 140 Oe and from 63.7 to 108 emu/g, respectively, and these values significantly improved after annealing. Maximum values of H_c (1050 Oe) at the Sm:Co molar ratio of 1:5 and M_s of 184.6 emu/g at the Sm:Co molar ratio of 1:9 were achieved in the annealed samples.     

Preparation and properties of cobalt oxides coated carbon fibers as microwave-absorbing materials

Cobalt oxides/carbon fibers (CoO_x/CFs) composites were synthesized by thermal oxidation of cobalt coated carbon fibers (Co/CFs). The scanning electron microscopy images and X-ray diffraction pattern indicate that the layers are about 0.7 μm and composed of Co₃O₄ and CoO (CoO_x), the preferred condition for preparation of CoO_x/CFs composites is to anneal Co/CFs precursors at 350 °C for 3 h in air. The coercivity, saturation magnetization and residual magnetization of the CoO_x/CFs composites are 464.8 Oe, 10.62 emu/g and 2.21 emu/g, respectively. The reflectivity of cobalt oxides coated carbon fibers (1.11-5.12 mm in thickness) is less than −10 dB over the working frequency range of 4.04-18.00 GHz and less than −20 dB over 11.54-14.77 GHz. The lowest reflectivity is −45.16 dB at 13.41 GHz when the thickness is 1.50 mm.     

Synthesis of (Mg0.476Mn0.448Zn0.007)(Fe1.997Ti0.002)O4 powder and sintered ferrites by high energy ball-milling process

(Mg_0.476Mn_0.448Zn_0.007)(Fe_1.997Ti_0.002)O₄ nanocrystalline powder prepared by high energy ball-milling process were consolidated by microwave and conventional sintering processes. Phases, microstructure and magnetic properties of the ferrites prepared by different processes were investigated. The (Mg_0.476Mn_0.448Zn_0.007)(Fe_1.997Ti_0.002)O₄ nanocrystalline powder could be prepared by high energy ball-milling process of raw Fe₃O₄, MnO₂, ZnO, TiO₂ and MgO powders. Prefired and microwave sintered ferrites could achieve the maximum density (4.86 g/cm⁻³), the average grain size (15 μm) was larger than that (10 μm) prepared by prefired and conventionally sintered ferrites with pure ferrite phase, and the saturation magnetization (66.77 emu/g) was lower than that of prefired and conventionally sintered ferrites (88.25 emu/g), the remanent magnetization (0.7367 emu/g) was higher than that of prefired and conventionally sintered ferrites (0.0731 emu/g). Although the microwave sintering process could increase the density of ferrites, the saturation magnetization of ferrites was decreased and the remanent magnetization of ferrites was also increased.     

Magnetic properties of CoFeP films prepared by electroless deposition

Structure and magnetization of CoFeP films prepared by the electroless deposition were systematically investigated by varying the bath composition and deposition parameters to optimize soft magnetic properties. The cobalt content in the CoFeP films varies from 40.4 to 94.9 wt% by controlling the bath composition. Increase of the metallic ratio FeSO₄·7H₂O/(CoSO₄·7H₂O+FeSO₄·7H₂O) affects the films’ microstructure, which switches from amorphous to crystalline structure. The magnetic properties of CoFeP films reveal that the coercivity (H_c) values range from 80 up to 185 A/m and the saturation magnetization (M_s) from 82 to 580 eum/g depending on the bath composition, deposition parameters and heat-treatment conditions. Increase of M_s and remanent magnetization (M_r) as well as decrease of H_c are observed for the CoFeP films with bath pH, temperature and the metallic molar ratio increasing. It is also found that the H_c is enhanced with the increase of NaH₂PO₂·H₂O concentration. CoFeP films showing good soft magnetic properties with coercivities less than 140 A/m and M_s close to 600 emu/g can be obtained in high pH bath and thereafter heat treatment. The deposit is found to be suitable as soft magnetic materials for core materials.     

Magnetic properties of prussian blue modified Fe3O4 nanocubes

Size controlled cubic Fe₃O₄ nanoparticles in the size range 90–10 nm were synthesized by varying the ferric ion concentration using the oxidation method. A bimodal size distribution was found without ferric ion concentration and the monodispersity increased with higher concentration. The saturation magnetization decreased from 90 to 62 emu/g when the particle size is reduced to 10 nm. The Fe₃O₄ nanoparticles with average particle sizes 10 and 90 nm were surface modified with prussian blue. The attachment of prussian blue with Fe₃O₄ was found to depend on the concentration of HCl and the particle size. The saturation magnetization of prussian blue modified Fe₃O₄ varied from 10 to 80 emu/g depending on the particle size. The increased tendency for the attachment of prussian blue with smaller particle size was explained based on the surface charge. The prussian blue modified magnetite nanoparticles could be used as a radiotoxin remover in detoxification applications.     

Influence of Nb substitution for Fe on the magnetic and magneto-impedance properties of amorphous and annealed Fe76.5−xSi13.5B9Cu1Nbx (x=0–7) ribbons

We report a systematic study of the influence of Nb substitution for Fe on the magnetic properties and magneto-impedance (MI) effect in amorphous and annealed Fe_76.5−xSi_13.5B₉Cu₁Nb_x (x=0, 1, 2, 3, 4, 5, 6, and 7) ribbons. The amorphous ribbons were annealed at different temperatures ranging from 530 to 560 °C in vacuum for different annealing times between 5 and 20 min. We have found that for the as-quenched amorphous ribbons, the substitution of Nb for Fe first increases the saturation magnetization (M_s) and decreases the coercivity (H_c) until x=3, for which the largest M_s∼152 emu/g and the smallest H_c∼1.3 Oe are obtained, then an opposite trend is found for x>3. The largest MI ratio (ΔZ/Z∼38% at f=6 MHz) is achieved in the amorphous ribbon with x=3. A similar trend has been observed for the annealed ribbons. The most desirable magnetic properties (M_s∼156 emu/g and H_c∼1.8 Oe) and the largest MI ratio (ΔZ/Z∼221% at f=6 MHz) are achieved for the x=3 sample annealed at 540 °C for 15 min. A correlation between the microstructure, magnetic properties, and MI effect in the annealed ribbons has been established.