Structural analysis of nickel doped cobalt ferrite nanoparticles prepared by coprecipitation route

Magnetic nanoparticles of nickel substituted cobalt ferrite (Ni_xCo_1−xFe₂O₄:0≤x≤1) have been synthesized by co-precipitation route. Particles size as estimated by the full width half maximum (FWHM) of the strongest X-ray diffraction (XRD) peak and transmission electron microscopy (TEM) techniques was found in the range 18–28±4 nm. Energy dispersive X-ray (EDX) analysis confirms the presence of Co, Ni, Fe and oxygen as well as the desired phases in the prepared nanoparticles. The selective area electron diffraction (SAED) analysis confirms the crystalline nature of the prepared nanoparticles. Data collected from the magnetization hysteresis loops of the samples show that the prepared nanoparticles are highly magnetic at room temperature. Both coercivity and saturation magnetization of the samples were found to decrease linearly with increasing Ni-concentration in cobalt ferrite. Superparamagnetic blocking temperature as determined from the zero field cooled (ZFC) magnetization curve shows a decreasing trend with increasing Ni-concentration in cobalt ferrite nanoparticles.     

Structural and magnetic characterization of soft-magnetic FeCo alloy nanoparticles

Soft-magnetic FeCo alloy nanoparticles with diameters less than 100 nm are prepared by ball milling. X-ray photoemission spectroscopy (XPS) and X-ray magnetic circular dichroism (XMCD) are used to characterize these particles. While the XPS spectrum from the as-prepared sample clearly shows Co photoemission peaks, no sign of Fe is observed in the same spectrum. However, Fe photoemission peaks appear after 1 h of Ar ion sputtering. A quantitative analysis of the XPS spectra shows an increase of Fe concentration versus sputtering time until the Fe:Co ratio of the bulk alloy is reached. In addition, the narrow scan Fe and Co 2p XPS spectra show that Co is more oxidized than Fe. All these measurements indicate that the nanoparticles have a Co shell and an Fe-rich core. They further demonstrate the usefulness of XPS combined with depth-profiling via sputtering to obtain element- and chemically-sensitive structural information on nanoparticles. XMCD as an element-specific magnetic analysis tool further reveals that Fe and Co are ferromagnetically coupled in these particles. The information obtained is useful for establishing a structure–property relation for the studied material that is expected to have applications as a soft magnetic material at high temperatures.     

Structural characterization and magnetic properties of superparamagnetic zinc ferrite nanoparticles synthesized by the coprecipitation method

Single phase zinc ferrite (ZnFe₂O₄) nanoparticles have been prepared by the coprecipitation method without any subsequent calcination. The effects of precipitation temperature in the range 20–80 °C on the structural and the magnetic properties of zinc ferrite nanoparticles were investigated. The crystallite size, microstructure and magnetic properties of the prepared nanoparticles were studied using X-ray diffraction (XRD), Fourier transmission infrared spectrum, transmission electron microscope (TEM), energy dispersive X-ray spectrometer and vibrating sample magnetometer. The XRD results showed that the coprecipitated nanoparticles were single phase zinc ferrite with mixture of normal and inverse spinel structures. Furthermore, ZnFe₂O₄ nanoparticles have the crystallite size in the range 5–10 nm, as confirmed by TEM. The magnetic measurements exhibited that the zinc ferrite nanoparticles synthesized at 40 °C were superparamagnetic with the maximum magnetization of 7.3 emu/g at 10 kOe.     

Morphologies and magnetic properties of FeCo nanoparticles modulated by changing the types of ligands of Co

A new way of preparing FeCo nanoparticles has been developed using the co-precipitation technique based on the appropriate Co precursors of different types of ligands. These new precursors have been prepared by the reaction of cobalt acetate with three various coordination compositions for forming cobalt complex types. This technique provides proper control on nanoparticle size distribution after annealing to 500 °C. The variation of the magnetic properties with the type of ligands of Co can arise from the changes of the microstructures and crystalline anisotropies. Maximum coercivity values of 480 Oe were obtained. It is found that the precursors with special structures can prevent from agglomeration without presence of any surfactants.     

Ferromagnetic FeCo nanoparticles for biotechnology

Calculated magnetophoretic mobility of a variety of magnetic compounds has identified FeCo to be an alternative for magnetite in in vitro biological cell separations. The synthesis of FeCo nanoparticles and the resulting microstructure is discussed as a function of the particle size. Their synthesis kinetics is modeled using a consecutive decomposition and growth model and is compared to experimental data.     

Preparation and characterization of complex ferrite nanoparticles by a polymer-pyrolysis route

The polymer-pyrolysis route used in this work was to synthesize the copolymeric precursor of the mixed metallic ions and then to pyrolyze the precursor into complex spinel ferrite nanoparticles. Thermogravimetric analysis (TGA) showed that the complex ferrite nanoparticles could be obtained by calcination of their precursors at 500°C. The structures, elemental analyses and particle morphology of the as-calcined products were characterized by powder X-ray diffraction (XRD), ICP-AES, transmission electron microscope (TEM) and electron diffraction (ED) pattern. The results revealed that the as-calcined powders were complex spinel ferrites and the size of those nanoparticles ranged from 10 to 20 nm. Magnetic measurements were carried out at room temperature using a vibrating sample magnetometer (VSM). The saturation magnetization of the Mn–Zn ferrites was related to the molar ratio of Mn to Zn and increased with the increase of Mn. The complex Co–Mn–Zn ferrite nanoparticles showed a high magnetization of 58 emu/g at the applied field of 10 kOe and a low coercivity of 30 Oe, which indicated that this materials exhibited characteristics of soft ferromagnetism.     

Synthesis and magnetic characterization of nickel ferrite nanoparticles prepared by co-precipitation route

Magnetic nanoparticles of nickel ferrite (NiFe₂O₄) have been synthesized by co-precipitation route using stable ferric and nickel salts with sodium hydroxide as the precipitating agent and oleic acid as the surfactant. X-ray diffraction (XRD) and transmission electron microscope (TEM) analyses confirmed the formation of single-phase nickel ferrite nanoparticles in the range 8-28 nm depending upon the annealing temperature of the samples during the synthesis. The size of the particles (d) was observed to be increasing linearly with annealing temperature of the sample while the coercivity with particle size goes through a maximum, peaking at ∼11 nm and then decreases for larger particles. Typical blocking effects were observed below ∼225 K for all the prepared samples. The superparamagnetic blocking temperature (T_B) was found to be increasing with increasing particle size that has been attributed to the increased effective anisotropy energy of the nanoparticles. The saturation moment of all the samples was found much below the bulk value of nickel ferrite that has been attributed to the disordered surface spins or dead/inert layer in these nanoparticles.     

Preparation of magnetic nanoparticles by pulsed plasma chemical vapor synthesis

FePt nanoparticle is expected as a candidate for the magnetic material of the high density recording media. We attempted to synthesize FePt alloy nanoparticles using 13.56 MHz glow discharge plasma with the pulse operation of a square-wave on/off cycle of plasma discharge to control the size of nanoparticles. Vapors of metal organics, Biscyclopentadienyl iron (ferrocene) for Fe and (Methylcyclopentadienyl) trimethyl platinum for Pt, were introduced into the capacitively coupled flow-through plasma chamber, which consisted of shower head RF electrode and grounded mesh electrode. Synthesis experiments were conducted at room temperature under the conditions of pressure 0.27 Pa, source gas concentration 0.005 Pa, gas residence time 0.5 s and plasma powers 60 watts. Pulse width for plasma duration was chosen from 0.5 to 30 s and plasma off period was 4 s to each pulse operation. Visual observations during the particle growth showed plasma emission in the bulk region was increased with the particle growth. These were theoretically explained by using the model for both transient particle charging in the plasma and single particle behavior in the stationary plasma as well as assuming the similarity between the negative charged particle and negative gas containing plasma. Synthesized nanoparticles were directly collected onto TEM grid, which was placed just below the grounded mesh electrode in the plasma reactor downstream. TEM pictures showed two kinds of particles in size, one of which was nanometer size and isolated with crystal structures and the other appeared agglomerate of nanometer size particles. The size of agglomerated particle was controlled in the 10–120 nm range by varying the plasma-on time from 0.5 to 30 s, although the nanometer size particles did not change. The composition of FePt alloy particles could be altered by adjusting the source gas feed ratio. Also magnetization of FePt nanoparticles was measured by use of SQUID (superconducting quantum interference device) magnetometry measurements. As-synthesized FePt nanoparticles did not exhibit loop-shape characteristic, which indicated superpamagnetic property. Annealed nanoparticles with the composition of Fe₅₈Pt₄₂ at 650°C in atmospheric hydrogen showed clear hysterisis loop with the coercivity as large as 10 KOe.     

Structure and magnetic properties of FeCo nanoparticles encapsulated in carbon nanotubes grown by microwave plasma enhanced chemical vapor deposition

Plasma enhanced chemical vapor deposition is a simple technique for preparing magnetic nanoparticles encapsulated in carbon nanotubes. We employed alloy catalysts when growing carbon nanotubes to control the composition and magnetic properties of encapsulated nanoparticles. Single-crystal nanoparticles were successfully encapsulated in carbon nanotubes, and their crystal structure varied depending on the composition of the alloy catalysts. The coercive force of nanoparticles also varied according to the composition of the catalysts.     

Perovskite nanoparticles: Preparation by reactive milling and magnetic characteristics

La_0.7Sr_0.3MnO₃ and La_0.7Ca_0.3MnO₃ nanoparticles were synthesized by reactive milling method. Grain size determined from XRD, TEM, and magnetization measurements show an average diameter ?18 nm and decreasing with increasing milling time. DC and AC magnetic measurements evidenced an interacting superparamagnetism due to clustering of perovskite nanoferromagnets with spin dynamic time in range of 10⁻⁹–10⁻¹⁰ s.     

Physical and magnetic properties of highly aluminum doped strontium ferrite nanoparticles prepared by auto-combustion route

Highly Al³⁺ ion doped nanocrystalline SrFe_12−xAl_xO₁₉ (0≤x≤12), were prepared by the auto-combustion method and heat treated in air at 1100 °C for 12 h. The phase identification of the powders performed using x-ray diffraction show presence of high-purity hexaferrite phase and absence of any secondary phases. With Al³⁺ doping, the lattice parameters decrease due to smaller Al³⁺ ion replacing Fe³⁺ ions. Morphological analysis performed using transmission electron microscope show growth of needle shaped ferrites with high aspect ratio at Al³⁺ ion content exceeding x≥2. Al³⁺ substitution modifies saturation magnetization (M_S) and coercivity (H_C). The room temperature M_S values continuously reduced while H_C value increased to a maximum value of 18,100 Oe at x=4, which is an unprecedented increase (∼321%) in the coercivity as compared to pure Sr-Ferrite. However, at higher Al³⁺ content x>4, a decline in magnetization and coercivity has been observed. The magnetic results indicate that the best results for applications of this ferrite will be obtained with an iron deficiency in the stoichiometric formulation.     

Synthesis of FeCo nanoparticles by pulsed laser deposition in a diffusion cloud chamber

Magnetic FeCo nanoparticles were successfully synthesized in a diffusion cloud chamber setup within pulsed laser deposition (PLD) equipment. The variation of morphology and size of FeCo nanoparticles with the number of laser pulses, ambient gas pressure and temperature gradient was studied. It was observed that the morphology of the nanoparticles changes from “cloud-like” fractal clusters to particle chains; average particle size increased at higher argon gas pressure. Increasing the temperature gradient considerably reduced the agglomeration of the nanoparticles. Nanoparticles deposited using the diffusion cloud chamber are found to be crystalline.     

Preparation and magnetic properties of magnetite nanoparticles by sol–gel method

 Magnetite (Fe₃O₄) nanoparticles have been successfully synthesized by sol–gel method combined with annealing under vacuum. The phase structures, morphologies, particle sizes, chemical composition, and magnetic properties of Fe₃O₄ nanoparticles have been characterized by X-ray diffraction, field emission scanning electron microscopy, energy-dispersive X-ray spectrometer and vibrating sample magnetometer (VSM). The results indicate that the size, the corresponding saturation magnetization value and coercivity value of Fe₃O₄ nanoparticles increase with the increase of synthesized temperature. And the phase transformation of Fe₃O₄ nanoparticles has been studied under different atmospheres and temperatures.     

Giant magnetic anisotropy in tetragonal FeCo alloys

In order to further increase the recording density in hard disk drives, new media materials are required. Two essential parameters of future recording media are a large uniaxial magnetic anisotropy energy (MAE) K(u) and a large saturation magnetization M(s). Based on first-principles theory, we predict that very specific structural distortions of FeCo alloys possess these desired properties. The discovered alloy has a saturation magnetization that is about 50% larger than that of FePt--a compound that has received considerable attention lately-with a uniaxial MAE that can easily be tailored reaching a maximum value that is 50% larger than that of FePt.     

Preparation and magnetic studies of nickel ferrite nanoparticles substituted by Sn and Cu

The mixed ferrite systems, namely NiFe_2−2xSn_xCu_xO₄ (x=0, 0.1, 0.2, and 0.3) nanoparticles have been studied to understand their structural and magnetic parameters. The NiFe_2−2xSn_xCu_xO₄ nanoparticles were prepared by high energy ball milling (HEBM). The samples were characterized by the X-ray diffraction technique. All samples exhibited spinel structures. The crystalline size and internal strain were evaluated by XRD patterns using Williamson-Hall and Scherrer methods. Magnetic properties of the nanoparticles ferrite were studied by means of alternating gradient force magnetometry (AGFM) and Faraday balance.     

Preparation and characterization of magnetic nanoparticles with controlled magnetization

The effect of molar ratio of two hydrated iron salts used as precursors into a (co)precipitation-based synthesis method, on the composition, size and specific saturation magnetization of mixed iron oxides and oxyhydroxides magnetic nanoparticles as reaction products, was studied. The preparation procedure is based on a salt-assisted solid-state chemical reaction. The obtained products are magnetic multiphase components with the mean size ranging from 3 to 10 nm and specific saturation magnetization between 25 and 95.5 emu/g. The specific saturation magnetization modifies in a non-linear manner as the molar ratio of the iron salts varies. Excepting one sample, for which Fe²⁺/Fe³⁺ molar ratio was zero, all magnetic nanoparticles show a ferrofluid-like behaviour in the colloidal form. The small size, ferrofluid-like behaviour, and controlled specific saturation magnetization allow the use of new synthesized nanoparticles in specific biomedical or industrial applications.     

Soft magnetic properties of FeCo films with Co underlayer

Bilayered Fe₆₅Co₃₅ (=FeCo)/Co films were prepared by facing targets sputtering with 4πM_s∼24 kg. The soft magnetic properties of FeCo films were induced by a Co underlayer. H_c decreased rapidly when the Co underlayer was 2 nm or more. The films showed well-defined in-plane uniaxial anisotropy with the typical values of H_ce=10 Oe and H_ch=3 Oe, respectively. High frequency characteristics of the films show the films can work at 0.8 GHz with real permeability as high as 250.     

Surface characterisation of dextran-coated iron oxide nanoparticles prepared by laser pyrolysis and coprecipitation

The favoured mechanism of adsorption of dextran on the surface of maghemite nanoparticles (5 nm) prepared by laser pyrolysis seems to be the collective hydrogen bonding between dextran hydroxyl groups and iron oxide particle surface. After heating, the formation of a surface complex between the polysaccharide oxygen atoms and the surface iron atoms gave rise to a stronger bonding.     

Morphology and magnetic properties of FeCo nanocrystalline powder produced by modified mechanochemical procedure

Properties of FeCo nanocrystalline intermetallic powders prepared by salt-matrix hydrogen reduction of a milled Fe₂O₃-Co₃O₄ mixture were investigated. The product of 72 ks ball-milling at 350 rpm was CoFe₂O₄ nanopowder. Reduction of this powder for 3.6 ks by hydrogen at 750 °C resulted in the formation of Fe_0.67Co_0.33 stoichiometric compound. Scanning electron microscopy, electron dispersive spectrometry, X-ray diffraction and vibrating sample magnetometry were used to characterize the nanopowder. Using a salt-matrix (NaCl as a dispersion medium) resulted in the decrease of the reduction temperature and improvement of the morphology and magnetic properties of the nanopowder. Dispersion of the ball-milled product in Hexan resulted in further improvements of the magnetic properties.     

Spin-polarized electron tunneling in bcc FeCo/MgO/FeCo(001) magnetic tunnel junctions

In combining spin- and symmetry-resolved photoemission, magnetotransport measurements and ab initio calculations we detangled the electronic states involved in the electronic transport in Fe(1-x)Co(x)(001)/MgO/Fe(1-x)Co(x)(001) magnetic tunnel junctions. Contrary to previous theoretical predictions, we observe a large reduction in TMR (from 530 to 200% at 20 K) for Co content above 25 atomic% as well as anomalies in the conductance curves. We demonstrate that these unexpected behaviors originate from a minority spin state with Δ(1) symmetry that exists below the Fermi level for high Co concentration. Using angle-resolved photoemission, this state is shown to be a two-dimensional state that occurs at both Fe(1-x)Co(x)(001) free surface, and more importantly at the interface with MgO. The combination of this interface state with the peculiar density of empty states due to chemical disorder allows us to describe in details the complex conduction behavior in this system.