Perpendicular magnetic anisotropy in 70 nm CoFe2O4 thin films fabricated on SiO2/Si(1 0 0) by the sol-gel method

Cobalt ferrite CoFe₂O₄ films were fabricated on SiO₂/Si(1 0 0) by the sol-gel method. Films crystallized at/above 600 °C are stoichiometric as expected. With increase of the annealing temperature from 600 °C to 750 °C, the columnar grain size of CoFe₂O₄ film increases from 13 nm to 50 nm, resulting in surface roughness increasing from 0.46 nm to 2.55 nm. Magnetic hysteresis loops in both in-plane and out-of-plane directions, at different annealing temperatures, indicate that the films annealed at 750 °C exhibit obvious perpendicular magnetic anisotropy. Simultaneously, with the annealing temperature increasing from 600 °C to 750 °C, the out of plane coercivity increases from 1 kOe to 2.4 kOe and the corresponding saturation magnetization increases from 200 emu/cm³ to 283 emu/cm³. In addition, all crystallized films exhibit cluster-like structured magnetic domains.     

Magnetic and FTIR studies of BixY3−xFe5O12 (x = 0, 1, 2) powders prepared by the metal organic decomposition method

The crystallization process of bismuth substituted yttrium iron garnet (Bi_xY_3−xFe₅O₁₂; x = 0, 1, 2) powder prepared by the metal-organic decomposition method has been studied with various sintering temperatures. The pure garnet phase was observed for the x = 1 powder at 900 °C sintering temperature, whereas the x = 0, 2 powder showed secondary phases. The x = 0 powder showed a similar crystallization process to that of the solid state reaction method. For the x =1, 2 powders, it is proposed that the lowering of the crystallization temperature is due to the lowered stability of the intermediate phase. The infrared spectroscopy and magnetic properties were also investigated. The pure garnet phase showed three absorption bands located at 563, 598, 655 cm⁻¹ that shifted to 555, 588, 639 cm⁻¹ along with an increase of bismuth concentration. The maximum values of saturation and remanence magnetization and the minimum value of coercivity were observed for the x = 1 powder sintered at 900 °C, which were 20.8 emu/g, 2.67 emu/g, and 31.9 Oe, respectively.     

Facile synthesis, magnetic and microwave absorption properties of Fe3O4/polypyrrole core/shell nanocomposite

Fe₃O₄/polypyrrole (PPy) core/shell nanocomposite, with Fe₃O₄ nanoparticle as core and PPy as shell, could be facilely synthesized via in situ chemical oxidative polymerization of pyrrole monomers on the surface of Fe₃O₄ nanoparticles. The results indicate that core/shell nanocomposite consists of Fe₃O₄ core with the mean diameter of 100 nm and adjacent PPy shell with a thickness of about 70 nm. The as-prepared Fe₃O₄/PPy core/shell nanocomposite exhibits a saturated magnetization of 20.1 emu/g and coercivity value of 368.3 Oe, respectively. The electromagnetic characteristics of Fe₃O₄/PPy core/shell nanocomposite were also investigated with a vector network analyzer in the 2-18 GHz range. The absorbing peak position moves to lower frequency with increasing the thicknesses of samples. The value of the minimum reflection loss is −22.4 dB at 12.9 GHz for Fe₃O₄/PPy core/shell nanocomposite with a thickness of 2.3 mm, and a broad peak with a bandwidth lower than −10 dB is about 5 GHz. Such strong absorption is attributed to better electromagnetic matching due to the existence of PPy and the special core/shell structure.     

Preparation of Ni0.5Zn0.5Fe2O4/SiO2 nanocomposites and their adsorption of bovine serum albumin

The magnetic nanocomposites of (1 − x)Ni_0.5Zn_0.5Fe₂O₄/xSiO₂ (x = 0-0.2) were synthesized by the citrate-gel process and their absorption behavior of bovine serum albumin (BSA) was investigated by UV spectroscopy at room temperature. The gel precursor and resultant nanocomposites were characterized by FTIR, XRD, TEM and BET techniques. The results show that the single ferrite phase of Ni_0.5Zn_0.5Fe₂O₄ is formed at 400 °C, with high saturation magnetization and small coercivity. A porous, amorphous silica layer is located at the ferrite nanograin boundaries, with the silica content increasing from 0 to 0.20, the average grain size of Ni_0.5Zn_0.5Fe₂O₄ calcined at 400 °C reduced from about 18-8 nm. Consequently, the specific surface area of the nanocomposites ascends clearly with the increase of silica content, which is largely contributed by the increase in the thickness of the porous silica layer. The Ni_0.5Zn_0.5Fe₂O₄/SiO₂ nanocomposites demonstrate a better adsorption capability than the bare Ni_0.5Zn_0.5Fe₂O₄ nanoparticles for BSA. With the increase of the silica content from 0 to 0.05 and the specific surface area from about 49-57 m²/g, the BSA adsorption capability of the Ni_0.5Zn_0.5Fe₂O₄/SiO₂ nanocomposites calcined at 400 °C improve dramatically from 22 to 49 mg/g. However, with a further increase of the silica content from 0.05 to 0.2, the specific surface area increase from about 57-120 m²/g, the BSA adsorption for the nanocomposites remains around 49 mg/g, owing to the pores in the porous silica layer which are too small to let the BSA protein molecules in.     

Direct synthesis and characterization of mesoporous Fe3O4 through pyrolysis of ferric nitrate-ethylene glycol gel

Mesoporous magnetite (Fe₃O₄) was successfully synthesized on a large scale by direct pyrolysis of ferric nitrate-EG (EG = ethylene glycol) gel in a one-end closed horizontal tube furnace in the air without using any template, additions, and carrier gas. The as-synthesized mesoporous Fe₃O₄ were characterized by powder X-ray diffraction (XRD), infrared spectra (IR), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), Brunauer-Emmett-Teller (BET), Barrett-Joyner-Halenda (BJH), and thermal gravimetric analysis (TGA). Results from TEM showed that the as-obtained Fe₃O₄ has mesoporous structure formed by the loose agglomeration of nanoparticles with diameter of about 6 nm, which was also confirmed by small-angle XRD and nitrogen adsorption analysis. Furthermore, vibrating sample magnetometer (VSM) measurements indicated that the saturated magnetization of the as-obtained mesoporous Fe₃O₄ was ferromagnetic with the saturation magnetization (Ms) and coercivity (Hc) of 46 emu/g and 136 Oe, respectively. In addition, a possible growth mechanism of mesoporous Fe₃O₄ was also discussed.     

Direct synthesis of Fe3O4 nanopowder by thermal decomposition of Fe-urea complex and its properties

An easy synthesis route of magnetite (Fe₃O₄) nanopowder is developed by using thermal decomposition of Fe-urea complex ([Fe(CON₂H₄)₆](NO₃)₃). The formation of Fe₃O₄ is confirmed from X-ray powder diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) measurements. The morphological properties and magnetic properties of the Fe₃O₄ are characterized by transmission electron microscopy (TEM) and magnetic measurements, respectively. By an increase in reaction temperature from 200 to 300 °C, the average crystallite size of the Fe₃O₄ nanopowder increases from 37 to 50 nm. Room temperature magnetization hysteresis curves show that the Fe₃O₄ nanopowder possesses ferrimagnetic characteristics. The saturation magnetization of the Fe₃O₄ nanopowder increases from 70.7 to 89.1 emu/g when the reaction temperature increases from 200 to 300 °C.     

Influence of MnO2 on the sintering behavior and magnetic properties of NiFe2O4 ferrite ceramics

The samples with small amounts of MnO₂ (0, 0.5, 1.0, 1.5, 2.0, and 2.5 wt%, respectively) were prepared via ball-milling process and two-step sintering process from commercial powders (i.e. Fe₂O₃, NiO and MnO₂). Microstructural features, phase transformation, sintering behavior and magnetic properties of Mn-doped NiFe₂O₄ composite ceramics have been investigated by means of scanning electron microscopy (SEM), differential thermal analyzer, X-ray diffraction (XRD), thermal dilatometer and vibrating sample magnetometer (VSM) respectively. The XRD analysis and the result of differential thermal analysis indicate that the reduction of MnO₂ into Mn₂O₃ and the following reduction of Mn₂O₃ into MnO existed in sintering process. No new phases are detected in the ceramic matrix, the crystalline structure of the ceramic matrix is still NiFe₂O₄ spinel structure. Morphology and the detecting result of thermal dilatometer show that MnO₂ can promote the sintering process, the temperature for 1 wt% MnO₂-doped samples to reach the maximum shrinkage rate is 59 °C lower than that of un-doped samples. For 1 wt% MnO₂-doped samples, the value of the saturation magnetization (M_s) and coercivity (H_c) is 15.673 emu/g and 48.316 Oe respectively.     

Part II. Large scale applications of NixMn0.8−xMg0.2Fe2O4; 0.1 ≤ x ≤ 0.35 using laser irradiation

Ni_xMn_0.8−xMg_0.2Fe₂O₄; 0.1 ≤ x ≤ 0.35 was prepared by standard ceramic technique at sintering temperature 1200 °C using heating / cooling rate 4 °C/min. The samples were irradiated by Nd YAG pulsed laser with energy of the pulse 250 mJ. X-ray diffractograms reveal cubic spinel structure for all the samples before and after laser irradiation. After laser irradiation, better crystallinity was obtained in a form of an increase in the calculated crystal size. This increase was discussed as due to the change in the valence of some ions like Fe³⁺, Ni²⁺ and Mn²⁺. The conductivity of all the investigated samples decreases after laser irradiation and becomes temperature independent for a wider range than that before irradiation. This was ascribed to electron rearrangement after laser irradiation. Accordingly, these ferrites are recommended to be useful in electronic devices.     

Luminescent and magnetic properties of YVO4:Ln@Fe3O4 (Ln = Eu or Dy) nanocomposites

A series of core-shell bifunctional magnetic-optical YVO₄:Ln³⁺@Fe₃O₄ (Ln³⁺ = Eu³⁺ or Dy³⁺) nanocomposites have been successfully synthesized via two-step method. The nanocomposites have the advantage of high magnetic responsive and unique luminescence properties. The structure, luminescent and magnetic properties of the nanocomposites were investigated by XRD, TEM, PL and VSM. The maximum emission peaks of the nanocomposites are at 618 nm (doping Eu³⁺), 574 nm (doping Dy³⁺). The special saturation magnetization of the nanocomposites is 54 emu/g. The diameter of the nanocomposites is 400-900 nm.     

Enhanced magnetization and magnetoelectric coupling in hydrogen treated hexagonal YMnO3

The single phase hexagonal YMnO₃ has been synthesized via sol-gel route by adopting two different sintering conditions. In one case, sintering has been done at ∼700 °C in Ar/H₂ atmosphere and in other case it has been done at ∼1250 °C in air. Magnetic measurements of the samples, synthesized by sintering at relatively lower temperature in Ar/H₂ atmosphere, show the enhanced ferromagnetic behaviour at 10 K. M-H curve shows that the value of saturation magnetization (M_s) at 10 K is 8.04 emu/g for Ar/H₂ sintered sample while it is 2.93 emu/g for the air sintered sample. Moreover, a weak ferromagnetic signal at room temperature has been observed in YMnO₃ compound. Magnetization versus magnetic field (M-H) curves of hydrogen treated samples, measured at room temperature, show small kink in the linear variation near origin, possibly due to presence of weak ferromagnetic interactions in the samples at room temperature. However, the polarization-electric field (P-E) curve shows weak ferroelectric characteristics for the Ar/H₂ sintered samples. It is suggested that the enhanced ferromagnetism in Ar/H₂ sintered sample originates from the presence of oxygen vacancies in the Ar/H₂ sintered samples. Moreover, the magnetoelectric coupling coefficient at room temperature is improved to 106 mV/cm Oe for Ar/H₂ sintered sample as compared to 96 mV/cm Oe for air sintered sample at 40 kHz ac magnetic field frequency.     

One-step solvothermal approach for preparing soft magnetic hydrophilic PFR coated Fe3O4 nanocrystals

The hydrophilic phenol formaldehyde resin coated Fe₃O₄ nanocrystals are prepared via a novel one-step solvothermal approach at 160 °C for 6-9 h without inert gas protection. Water-glycol mixture is used as solvent in common air surrounding. FeSO₄·7H₂O, hexamethylenetetramine and phenol are used as resource materials without any others additives or surfactants. The transmission electronic microscope images show the samples are composed of sphere-like particles with sizes about 10-20 nm. The X-ray diffraction data indicate cube-phase Fe₃O₄ nanocrystals are obtained at given conditions. Fourier transform infrared spectra further reveal the samples are consisted of Fe₃O₄ and PFR. Without modified pH and added surfactants, the solubility of the obtained sample is over 1% in water, which is far more than its solubility in toluene. Room-temperature hysteresis loop indicate that the as-obtained nano-crystals possess soft magnetic properties with high saturated mass magnetization (50.6 emu/g) and negligible coercivity.     

Role of Cr ions on the microstructure development, and magnetic phase evolution of Ni0.7Zn0.3Fe2O4 ferrite nanoparticles

A series of ferrite samples with the chemical formula Ni_0.7Zn_0.3Cr_xFe_2−xO₄ (x = 0.0-0.5) were prepared by a sol-gel auto-combustion method and annealed at 600 °C for 4 h. The resultant powders were investigated by various techniques, including X-ray diffractometry (XRD), vibrating sample magnetometry (VSM), and permeability studies. The prepared samples have a cubic spinel structure with no impurity phase. As the Cr³⁺ content x increases, bulk density and crystallite size decrease, whereas porosity increases. The saturation magnetization decreases linearly from 58.31 to 42.90 emu/g with increasing Cr³⁺ content. However, coercivity increases with increasing Cr³⁺ substitution. The magnetic moments calculated from Neel's molecular-field model are in agreement in the experiment results. The initial permeability (μ_i) decreases with increasing Cr³⁺ substitution. The decrease in initial permeability (μ_i) is attributed to decrease in magnetization on addition of Cr³⁺. The real part of the permeability decreases gradually with increasing frequency in accordance with Snoek's law. The Curie temperature decreases linearly with increasing Cr³⁺ content.     

Synthesis, characterization, magnetic and electrical properties of the novel conductive and magnetic Polyaniline/MgFe2O4 nanocomposite having the core-shell structure

Conductive and magnetic Polyaniline/MgFe₂O₄ nanocomposite was successfully synthesized in the form of core-shell via in situ chemical polymerization of aniline in the presence of MgFe₂O₄ nano-particles. X-ray powder diffraction of ferrites indicated that the structure of the core material is having the spinel structure, and demonstrated the formation of PAni/MgFe₂O₄ nanocomposite. XRD and TEM photographs showed that the particle's size of the MgFe₂O₄ core-material were around 30-35 nm before coating with Polyaniline, and grown up to 45 nm in the core-shell nanocomposite after coating. Although PAni has a relatively smaller electrical field coefficient than the core-shell nanocomposite, the resistivity of the core-shell material decreased, and hence its conductivity increased after a certain threshold voltage of 0.98 V equivalent to threshold electric field value equals 5.5 V cm⁻¹. The magnetic hysteresis loops investigated with VSM indicated that coating MgFe₂O₄ with Polyaniline has an healing effect which covers the ferrite surface defects, thus decreasing the magnetic surface anisotropy of ferrite particles leading to a decrease of the saturated magnetization (Ms) from 21.33 emu/g to 5.905 emu/g and a decrease of the coercivity (Hc) from 88.66 Oe to 81.6 Oe for MgFe₂O₄ and the core-shell nanocomposite respectively due to the amount of Polyaniline added. TGA and DTA revealed improved thermal stability of the core-shell nanocomposite with respect to that of Polyaniline due to the incorporation of ferrites. Raman spectroscopy confirmed TGA, DTA and XRD studies, and revealed that pure PAni is less stable than the corresponding core-shell nanocomposite with respect to molecular changes which might occur during heating at elevated temperatures. Moreover, Raman study confirmed the interfacial interaction between the core and the shell materials, and lead to an assumption about the presence of different conjugation chain lengths and types, such as the presence of the semi-quinones aside the quinone rings in the polymer chain, which showed different response upon heating the sample.     

Nano-sized Y2O3:Eu hollow spheres with enhanced photoluminescence properties

Nano-sized Y₂O₃:Eu³⁺ hollow spheres were fabricated via a facile strategy including preparation of the hollow precursor and a later calcination. Moreover, the growth process of these hollow spheres was monitored by time-dependent experiments and their luminescence properties were also intensively studied. The products exhibit strong red emitting at 613 nm under ultraviolet excitation and control experiments were carried out to optimize the synthetic conditions. It was found 850 °C calcination with 9 mol% doping level could give out the best photoluminescence performance. Moreover, a possible mechanism for the enhanced PL performance was also proposed based on the FT-IR investigation.     

Effect of Ni substitution on the structural and transport properties of NixMn0.8−xMg0.2Fe2O4; 0.0 ≤ x ≤ 0.40 ferrite

Ni_xMn_0.8−xMg_0.2Fe₂O₄; 0.0≤ x ≤0.40 was prepared by standard ceramic technique, presintering was carried out at 900 °C and final sintering at 1200 °C with heating/cooling rate 4 °C/min. X-ray diffraction analyses assured the formation of the samples in a single phase spinel cubic structure. The calculated crystal size was obtained in the range of 75-130 nm. A slight increase in the theoretical density and decrease in the porosity was obtained with increasing the nickel content. This result was discussed based on the difference in the atomic masses between Ni (58.71) and Mn (54.938). IR spectral analyses show four bands of the spinel ferrite for all the samples. The conductivity and dielectric loss factor give nearly continuous decrease with increasing Ni-content. This was discussed as the result of the significant role of the multivalent cations, such as iron, nickel, manganese, in the conduction mechanism. Anomalous behavior was obtained for the sample with x = 0.20 as highest dielectric constant, highest dielectric loss and highest conductivity. This anomalous behavior was explained due to the existence of two divalent cations on B-sites with the same ratio, namely, Mg²⁺ and Ni²⁺.     

Ultrasonic-assisted in situ synthesis and characterization of superparamagnetic Fe3O4 nanoparticles

Superparamagnetic Fe₃O₄ nanoparticles were synthesized via a modified coprecipitation method, and were characterized with X-ray diffraction (XRD), vibrating sample magnetometer (VSM), Zeta potential and FT-IR, respectively. The influences of different kinds of surfactants (sodium dodecyl benzene sulfonate, polyethyleneglycol, oleic acid and dextran), temperatures and pH values on the grain size and properties were also investigated. In this method, Fe³⁺ was used as the only Fe source and partially reduced to Fe²⁺ by the reducing agent with precise content. The following reaction between Fe³⁺, Fe²⁺ and hydroxide radical brought pure Fe₃O₄ nanoparticles. The tiny fresh nanoparticles were coated in situ with surfactant under the action of sonication. Comparing with uncoated sample, the mean grain size and saturation magnetization of coated Fe₃O₄ nanoparticles decrease from 18.4 nm to 5.9-9.0 nm, and from 63.89 emu g⁻¹ to 52-58 emu g⁻¹ respectively. When oleic was used as the surfactant, the mean grain size of Fe₃O₄ nanoparticles firstly decreases with the increase of reaction temperature, but when the temperature is exceed to 80 °C, the continuous increase of temperature resulted in larger nanoparticles. the grain size decreases gradually with the increasing of pH values, and it remains unchanged when the PH value is up to 11. The saturation magnetization of as-prepared Fe₃O₄ nanoparticles always decreases with the fall of grain size.     

Magnetic properties of Sn-Mg substituted strontium hexaferrite nanoparticles synthesized via coprecipitation method

Nanoparticles of Sn-Mg substituted strontium hexaferrite with the composition of SrFe_12−x(Sn_0.5 Mg_0.5)_xO₁₉ (x = 0.0-1.0) were synthesized by chemical coprecipitation method. Deionized water/ethanol (50/50) was used as the solvent. The single phase strontium hexaferrites were obtained at pH 13 and Fe³⁺/Sr²⁺ molar ratio of 9 after calcination at 800 °C. The mean particle size of samples was decreased from 82 to 56 nm with increasing the Sn-Mg content from x = 0.0 to x = 0.8. The effect of Sn-Mg substitution on magnetic properties of hexaferrites was studied using vibrating-sample magnetometer. It was found that increasing the Sn-Mg from x = 0.0 to x = 0.8 reduced the coercivity from 4728.9 to 1455.5 Oe and increased the saturation magnetization from 51.34 to 65.49 emu/g. A vector network analyzer was used to investigate the microwave absorption properties. According to microwave measurements, doped strontium hexaferrite composites had much more effective electromagnetic absorption properties than undoped strontium hexaferrite composite.     

Synthesis, structure, and properties of Li2Pb2CuB4O10 with isolated [CuB4O10] units

The copper borate Li₂Pb₂CuB₄O₁₀ has been synthesized in air by the standard solid-state reaction at temperature in the range 550-650 °C and the structure of Li₂Pb₂CuB₄O₁₀ was determined by single-crystal X-ray diffraction. Li₂Pb₂CuB₄O₁₀ crystallizes in the monoclinic space group C2/c (no. 15) with a = 16.8419(12), b = 4.7895(4), c = 13.8976(10) Å, and β = 125.3620(10)°, V = 914.22(12) Å³, and Z = 4, as determined by single-crystal X-ray diffraction. The Li₂Pb₂CuB₄O₁₀ structure exhibits isolated units of stoichiometry [CuB₄O₁₀]⁶⁻ that are built from CuO₄ distorted square planes and triangular BO₃ groups. The IR spectroscopy and thermal analysis investigations of Li₂Pb₂CuB₄O₁₀ are also presented.     

Synthesis and characterization of cobalt-free Ba0.5Sr0.5Fe0.8Cu0.2O3−δ perovskite oxide cathode nanofibers

The cobalt-free perovskite-oxide, Ba_0.5Sr_0.5Fe_0.8Cu_0.2O_3−δ (BSFC) is a very important cathode material for intermediate-temperature proton-conducting solid oxide fuel cells. Ba_0.5Sr_0.5Fe_0.8Cu_0.2O_3−δ nanofibers were synthesized for the first time by a sol-gel electrospinning. Process wherein a combination of polyvinylpyrrolidone and acetic acid was used as the spinning aid and barium, strontium, iron and copper nitrates were used as precursors for the synthesis of BSFC nanofibers. X-ray diffraction studies on products prepared at different calcination temperatures revealed a cubic perovskite structure at 900 °C. The temperature of calcination has a direct effect on the crystallization and surface morphology of the nanofibers. High porosity, and surface area, in addition to an electrical conductivity of 69.54 S cm⁻¹ at 600 °C demonstrate the capability of BSFC nanofibers to serve as effective cathode materials for intermediate-temperature solid oxide fuel cells.     

Synthesis of nanocrystalline nickel-zinc ferrite (Ni0.8Zn0.2Fe2O4) thin films by chemical bath deposition method

The nickel-zinc ferrite (Ni_0.8Zn_0.2Fe₂O₄) thin films have been successfully deposited on stainless steel substrates using a chemical bath deposition method from alkaline bath. The films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), static water contact angle and cyclic voltammetry measurements. The X-ray diffraction pattern shows that deposited Ni_0.8Zn_0.2Fe₂O₄ thin films were oriented along (3 1 1) plane. The FTIR spectra showed strong absorption peaks around 600 cm⁻¹ which are typical for cubic spinel crystal structure. SEM study revealed compact flakes like morphology having thickness ∼1.8 μm after air annealing. The annealed films were super hydrophilic in nature having a static water contact angle (θ) of 5°.The electrochemical supercapacitor study of Ni_0.8Zn_0.2Fe₂O₄ thin films has been carried out in 6 M KOH electrolyte.The values of interfacial and specific capacitances obtained were 0.0285 F cm⁻² and 19 F g⁻¹, respectively.