Microwave-induced combustion synthesis of Ni–Zn ferrite powder and its characterization

Ni–Zn ferrite powders were successfully synthesized by microwave-induced combustion process. The process takes only a few minutes to obtain calcined Ni–Zn ferrite powders. The resultant powders were investigated by XRD, SEM, VSM, TG/DTA and surface area measurements. The as-received product shows the formation of cubic ferrite with saturation magnetization (M_s)≈23 emu/g, whereas upon annealing at 850°C for 4 h, the saturation magnetization (M_s) increased to ≈52 emu/g.     

Effects of calcining temperature on structural and magnetic properties of nanosized Fe-doped NiO prepared by diol-based sol−gel process

Iron-doped nickel oxide (Fe_0.01Ni_0.99O, abbreviated as FNO) nanoparticles were prepared by sol–gel process using 1,3-propanediol as a solvent and also as a chelating agent, and calcined at the various temperatures (400–1000 °C) for 2 h. The phase composition and the microstructure of the calcined products were investigated by X-ray diffraction and scanning electron microscopy techniques, respectively. Magnetic properties were measured at room temperature using a vibrating sample magnetometer. All calcined samples showed the single phase of FNO cubic rock-salt structure without the presence of any impurity phases. The crystallite size from XRD and particle size from SEM increased as calcining temperature increased. The FNO powders calcined at 400?600 °C revealed the uniform and dense spherical particles in nanosize. The room-temperature ferromagnetism was observed for all samples. When the calcining temperature was increased, the saturation magnetization decreased whereas the coercivity increased, corresponding to the less dense and larger particles. The calcined sample at 400 °C had the best magnetic properties with the highest M_s of 5.34 emu/g (at 10 kOe) and the lowest H_c of 372 Oe.     

Magnetic fluid thermochemotherapy of murine tumors

Four series of water-based dextran-ferrite (DF) magnetic fluids (MFs) containing Melphalan (MP) were prepared. Their saturation magnetization (M_s) was from 0.8 to 7.8 kA/m; specific power absorption rates were 240 W/g Fe. After nine courses of magnetic fluid thermochemotherapy with MP containing DF MF (M_s 7.5 kA/m, pH 6.6, ζ+15 mV) at 44–46 °C for 30 min in an AC magnetic field (0.88 MHz, 9.3 kA/m, 0.3 kW), complete P388 tumor regression was seen in 30% of BDF₁ mice. Furthermore, a life span increase of 180% was achieved.     

Magnetic properties and formation of Sr ferrite nanoparticle and Zn,Ti/Ir substituted phases

Strontium hexaferrite nanoparticles are prepared by the chemical sol–gel route. Specific saturation magnetization σ_s and coercive field strength H_c are determined depending on the heat treatment of the gel and iron/strontium ratio in the starting solution. These ultrafine powders with single-domain behavior have specific saturation magnetization σ_s=74 emu/g and coercive field strength H_c=6.4 kOe. Experimental results show that it is necessary to preheat the gel between 400 and 500°C for several hours . It can prevent the formation of intermediate γ-Fe₂O₃ and help to obtain ultrafine strontium ferrite single phase with narrow size distribution at a low annealing temperature. Additionally, the magnetic properties of sol–gel derived strontium ferrite with iron substituted by Zn²⁺, Ti⁴⁺ and Ir⁴⁺ are discussed. For an amount of substitution 0<x⩽0.6, the (Zn, Ti)_x substituted strontium ferrite shows higher values of both coercive field strength and saturation magnetization than the (Zn, Ir)_x substituted phase.     

Electrochemical supercapacitor studies of hierarchical structured Co2+-substituted SnO2 nanoparticles by a hydrothermal method

Hierarchical structured Co-doped SnO₂ nanoparticles are prepared by a low temperature hydrothermal process. The structural and surface morphologies of the SnO₂ and Sn_1?xCo_xO₂ nanoparticles are studied by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The Sn_1?xCo_xO₂ nanoparticles form with a tetragonal rutile structure during the hydrothermal process without further calcination. The pseudocapacitance behavior of the Sn_1?xCo_xO₂ nanoparticles is characterized by cyclic voltammetry (CV) in 1.0 M H₂SO₄ electrolyte. The specific capacitance (SC) is found to increase with an increase in cobalt content. A maximum SC of 840 F g^?1 is obtained for a Sn_0.96Co_0.04O₂ composite at a 10 mV s^?1 scan rate.     

Synthesis and magnetic properties of Cu-coated Fe composite nanoparticles

The Fe/Cu nanocomposites with iron as core and copper as shell have been successfully synthesized by a two-step reduction method. A spherical nanoparticle of γ-Fe was first fabricated by the reduction of ferrous chloride, and then the Fe particle was coated by nanocrystalline Cu through the reduction of copper sulfate. The thickness of copper shell has been tuned by varying the initial concentration of copper sulfate. The morphology, crystalline structure, chemical composition and magnetic properties of the products were investigated by using transmission electron microscopy (TEM), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS) and vibrating sample magnetometer (VSM). It was found that the saturation magnetization (M_s) values of the Fe/Cu core–shell particles are varied owing to the different thickness of copper layer. Though the M_s value of the Fe/Cu nanocomposite is lower than that of pure iron nanoparticles, the higher M_s value (22.411 emu/g) of the Fe/Cu composites is also investigated. The result of the thermogravimetric analysis (TGA) showed the enhanced antioxidation capacity of the Fe/Cu nanocomposites. This kind of nanocomposites combined the excellent magnetism of iron and the electronic, thermal conductivity of copper, suggesting potential application as a novel electromagnetic material.     

Dielectric and magnetic properties of Bi1−xYxFeO3 ceramics

Y doped BiFeO₃ polycrystalline ceramics were prepared by sol–gel method. Crystal structure examined by X-ray diffraction indicates that the samples were single-phase and crystallize in rhombohedral structure. An anomaly in the dielectric constant and dielectric loss in the vicinity of the antiferromagnetic Neel temperature (T_N) was observed. Saturated magnetization loops were observed for all sample with saturated magnetization M_s=0.678 emu/g and remnant magnetization M_r=0.084 emu/g for x=0.3.     

Synthesis,characterization and magnetic properties of lightly doped La2−xSrxCuO4 (x = 0.04) nanoparticles

Lightly doped La_2−xSr_xCuO₄ (x = 0.04) nanoparticles with different particle sizes have been successfully prepared by a sol–gel method and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared transmission (IR) spectra and superconducting quantum interference device (SQUID) magnetometer. All samples are single phase and have an orthorhombic unit cell. As the particle size reduces, it is found that the IR band at around 685 cm⁻¹ corresponding to the in-plane Cu–O asymmetrical stretching mode shifts to higher frequency and the magnetization exhibits a large enhancement at low temperature. The magnetic susceptibility of all samples follows a modulated Curie law between ∼20 K and ∼100 K and the Curie constant displays a strong dependence on the particle size. It is suggested that as the particle size decreases surface effects should play an important role in the magnetic properties of the nanoparticles.     

Sonochemical synthesis of cobalt aluminate nanoparticles under various preparation parameters

Cobalt aluminate (CoAl₂O₄) nanoparticles were synthesized using a precursor method with the aid of ultrasound irradiation under various preparation parameters. The effects of the preparation parameters, such as the sonochemical reaction time and temperature, precipitation agents, calcination temperature and time on the formation of CoAl₂O₄ were investigated. The precursor on heating yields nanosized CoAl₂O₄ particles and both these nanoparticles and the precursor were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and atomic force microscopy (AFM). The use of ultrasound irradiation during the homogeneous precipitation of the precursor reduces the duration of the precipitation reaction. The mechanism of the formation of cobalt aluminate was investigated by means of Fourier transformation infrared spectroscopy (FT-IR) and EDX (energy dispersive X-ray). The thermal decomposition process and kinetics of the precursor of nanosized CoAl₂O₄ were investigated by means of differential scanning calorimetry (DSC) and thermogravimetry (TG). The apparent activation energy (E) and the pre-exponential constant (A) were 304.26 kJ/mol and 6.441 × 10¹⁴ s^?1, respectively. Specific surface area was investigated by means of Brunauer Emmett Teller (BET) surface area measurements.     

Magnetic properties of iron nanoparticles in a polymer film

We systematically synthesized self-aggregated iron nanoparticles in the perfluorinated sulfo-cation membrane (MF-4SK) by ion-exchange method. Our experimental results show that iron nanoparticles in MF-4SK exhibit superparamagnetic properties above the blocking temperature. Field-cooled and zero-field-cooled magnetization data show the blocking temperature, T_B≅120 K for the iron concentration of 5×10¹⁹ atoms per 1 g of polymer film at 500 Oe applied field. This result is well matched with the calculation based on the temperature dependence of the coercivity, which shows T_B≅110 K, with the zero temperature coercivity (H_C0) ≅ 420 Oe. The radius of the typical iron particle is determined to be ∼2 nm from transmission electron microscopy (TEM), showing good agreement with the value acquired by Langevin function fit. These experimental evidences suggest that iron nanoparticles in the polymer film obey a single-domain theory.     

Preparation of monodisperse magnetite nanoparticles under mild conditions

In this paper, we reported a method to prepare monodisperse magnetite nanoparticles at mild temperature using cheap and non-toxic precursors. It overcomes the shortages of chemical co-precipitation method and thermal decomposition method and combines the advantages of facile, cheap, large-scale, monodisperse, nanosize, and low synthesis temperature and low toxic. In this method, FeCl₃ · 6H₂O, FeCl₂ · 4H₂O and sodium oleate were mixed in toluene/ethanol/water mixture solvent and refluxed at 74 °C to prepare magnetite nanoparticles directly. The nanoparticles were characterized by transmission electron microscopy, dynamic light scattering, X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectrometer and thermogravimetric analysis. The magnetic properties of nanoparticles were measured by superconducting quantum interference device. The results showed that the nanoparticles are well-monodisperse with about 4–5 nm of average diameter. The nanoparticles were proved to be superparamagnetic with saturated magnetization 23.6 emu/g and blocking temperature 24.4 K. A possible formation mechanism of monodisperse magnetite nanoparticles was presented at the same time.     

Synthesis of Co nanocapsules coated with BN layers by annealing of KBH4 and [Co(NH3)6]Cl3

Cobalt (Co) nanocapsules coated with boron nitride (BN) layers were synthesized by annealing of ammine complex. KBH₄ and [Co(NH₃)₆]Cl₃ were used as starting materials, and annealed these powders at 500–1000 °C with flowing nitrogen gas. Formation of fcc-Co nanocapsules coated with BN layers was observed from X-ray diffraction patterns and high-resolution electron microscopy. Particle size of fcc-Co prepared at 1000 °C with flowing 100 sccm N₂ gas was approximately 40 nm, and the values of saturation magnetization and coercivity were 74.5 emu/g and 88 Oe, respectively. Good oxidation- and wear-resistances were obtained by encapsulating Co nanoparticles with BN layers.     

Biosynthesis of gold nanoparticles by Aspergillum sp. WL-Au for degradation of aromatic pollutants

A simple method for synthesis of gold nanoparticles (AuNPs) using Aspergillum sp. WL-Au was presented in this study. According to UV–vis spectra and transmission electron microscopy images, the shape and size of AuNPs were affected by different parameters, including buffer solution, pH, biomass and HAuCl₄ concentrations. Phosphate sodium buffer was more suitable for extracellular synthesis of AuNPs, and the optimal conditions for AuNPs synthesis were pH 7.0, biomass 100 mg/mL and HAuCl₄ 3 mM, leading to the production of spherical and pseudo-spherical nanoparticles. The biosynthesized AuNPs possessed excellent catalytic activities for the reduction of 2-nitrophenol, 3-nitrophenol, 4-nitrophenol, o-nitroaniline and m-nitroaniline in the presence of NaBH₄, and the catalytic rate constants were calculated to be 6.3×10⁻³ s⁻¹, 5.5×10⁻³ s⁻¹, 10.6×10⁻³ s⁻¹, 8.4×10⁻³ s⁻¹ and 13.8×10⁻³ s⁻¹, respectively. The AuNPs were also able to catalyze the decolorization of various azo dyes (e.g. Cationic Red X-GRL, Acid Orange II and Acid scarlet GR) using NaBH₄ as the reductant, and the decolorization rates reached 91.0–96.4% within 7 min. The present study should provide a potential candidate for green synthesis of AuNPs, which could serve as efficient catalysts for aromatic pollutants degradation.     

Growth of Sr2CrReO6 epitaxial thin films by pulsed laser deposition

We report the growth, structural, magnetic, and electrical transport properties of epitaxial Sr₂CrReO₆ thin films. We have succeeded in depositing films with a high crystallinity and a relatively large cationic order in a narrow window of growth parameters. The epitaxy relationship is Sr₂CrReO₆ (SCRO) (0 0 1) [1 0 0]∥SrTiO₃ (STO) (0 0 1) [1 1 0] as determined by high-resolution X-ray diffraction and scanning transmission electron microscopy (STEM). Typical values of saturation magnetization of M_S (300 K)=1 μ_B/f.u. and ρ (300 K)=2.8 mΩ cm have been obtained in good agreement with previous published results in sputtered epitaxial thin films. We estimate that the antisite defects concentration in our thin films is of the order of 14%, and the measured Curie temperature is T_C=481(2) K. We believe these materials be of interest as electrodes in spintronic devices.     

Control synthesis of magnetic Fe3O4–chitosan nanoparticles under UV irradiation in aqueous system

Novel magnetic Fe₃O₄–chitosan nanoparticles were synthesized via photochemical method in an emulsifier-free aqueous system at room temperature for the first time. The scanning electron microscopy (SEM) and transmission electron microscopy (TEM) results showed that the Fe₃O₄–chitosan nanoparticles were in regular shape with a mean diameter of 41 nm, whereas the average size in aqueous solution measured by photocorrelation spectroscopy (PCS) was 64 nm, which indicated that the nanoparticles had water-swelling properties. X-ray diffraction (XRD) patterns indicated that the Fe₃O₄ nanoparticles were pure Fe₃O₄ with a spinel structure, and the irradiation under UV light did not result in a phase change. The Fe₃O₄–chitosan nanoparticles were also characterized by Fourier transform infrared (FTIR) spectra, thermogravimetric analysis (TGA) and vibrating sample magnetometer (VSM). Magnetic measurement revealed that the saturated magnetization (Ms) of the Fe₃O₄–chitosan nanoparticles reached 48.6 emu/g and the nanoparticles showed the characteristics of superparamagnetism. The stability test showed these novel nanoparticles had high magnetic stability. The PCS and TGA results indicated that the size and chitosan content of Fe₃O₄–chitosan nanoparticles formed was pH- and chitosan/Fe₃O₄ ratio-dependent, which could be used to synthesize magnetic Fe₃O₄–chitosan nanoparticles with different size to meet the requirements of different applications.     

Fe3O4/hydroxyapatite/graphene quantum dots as a novel nano-sorbent for preconcentration of copper residue in Thai food ingredients: Optimization of ultrasound-assisted magnetic solid phase extraction

Fe₃O₄/hydroxyapatite/graphene quantum dots (Fe₃O₄/HAP/GQDs) nanocomposite was synthesized and used as a novel magnetic adsorbent. This nanocomposite was characterized using scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, and magnetization property. The Fe₃O₄/HAP/GQDs was applied to pre-concentrate copper residues in Thai food ingredients (so-called “Tom Yum Kung”) prior to determination by inductively coupled plasma-atomic emission spectrometry. Based on ultrasound-assisted extraction optimization, various parameters affecting the magnetic solid-phase extraction, such as solution pH, amount of magnetic nanoparticles, adsorption and desorption time, and type of elution solvent and its concentration were evaluated. Under optimal conditions, the linear range was 0.05–1500 ng mL⁻¹ (R² > 0.999), limit of detection was 0.58 ng mL⁻¹, and limit of quantification was 1.94 ng mL⁻¹. The precision, expressed as the relative standard deviation of the calibration curve slope (n = 5), for intra-day and inter-day analyses was 0.87% and 4.47%, respectively. The recovery study of Cu for real samples was ranged between 83.5% and 104.8%. This approach gave the enrichment factor of 39.2, which guarantees trace analysis of Cu residues. Therefore, Fe₃O₄/HAP/GQDs can be a potential and suitable candidate for the pre-concentration and separation of Cu from food samples. It can easily be reused after treatment with deionized water.     

Structure,magnetic and microwave properties of FeNi invar nanoparticles obtained by electrical explosion of wire in different preparation conditions

Magnetic nanoparticles (MNPs) of close to invar (Fe_0.635Ni_0.365) composition were prepared by the electrical explosion of wire using different conditions to insure different values of overheating rates. X-ray diffraction, transmission electron microscopy, low temperature nitrogen adsorption, magnetic and microwave measurements were used for the characterization of MNPs. Increase of the energy injected into the wire led to increase of the specific surface (S_sp) of the produced MNPs from 4.6 to 13.5 m²/g. The fabricated MNPs were spherical and weakly aggregated with the average weighted diameter in the range of 54–160 nm depending on the S_sp. The phase composition of FeNi MNPs consists of two solid solutions of Ni in α-phase and γ-phase lattices. The increase of the energy injected into the wire leads to increase of the α-phase from 5 to 10 wt% as the injected energy raised from 0.8 to 2.5 times the sublimation energies of the wire material. Comparative analysis of structure magnetic and microwave properties showed that the obtained MNPs are important magnetic materials with high saturation magnetization and significant zero field microwave absorption which can be expected to lead to important technological applications.     

Sonochemical synthesis of Dy2(CO3)3 nanoparticles,Dy(OH)3 nanotubes and their conversion to Dy2O3 nanoparticles

Dysprosium carbonates nanoparticles were synthesized by the reaction of dysprosium acetate and NaHCO₃ by a sonochemical method. Dysprosium oxide nanoparticles with average size about 17 nm were prepared from calcination of Dy₂(CO₃)₃·1.7H₂O nanoparticles. Dy(OH)₃ nanotubes were synthesized by sonication of Dy(OAC)₃·6H₂O and N₂H₄. The as-synthesized nanostructures were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and Fourier transform infrared spectroscopy (FT-IR). Photoluminescence measurement shows that the nanoparticles have two emission peaks around 17,540 cm^?1 and 20,700 cm^?1, which should come from the electron transition from ⁴F_9/2 → ⁶H_15/2 levels and ⁴F_9/2 → ⁶H_13/2 levels, respectively. The effect of calcination temperature and sonication time was investigated on the morphology and particle size of the products. The sizes could be controlled by the feeding rate of the precipitating agent (NaHCO₃ and N₂H₄) and slower feeding rate lead to smaller nanoparticles.     

Study of structural and magnetic properties of superparamagnetic Fe3O4/SiO2 core–shell nanocomposites synthesized with hydrophilic citrate-modified Fe3O4 seeds via a sol–gel approach

This paper describes a simple way for the coating of magnetite nanoparticles (MNPs) with amorphous silica. First, MNPs were synthesized by controlled co-precipitation technique under N₂ gas and then their surface was modified with trisodium citrate in order to achieve particles with improved dispersibility. Afterward, magnetite-silica core/shell nanocomposites were prepared by a sol–gel approach, using magnetic fluid including electrostatically stabilized MNPs as seeds. The prepared samples were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, zeta potential analysis and vibrating sample magnetometer (VSM) in order to study their structural and magnetic properties. FT-IR and XRD results imply that resultant nanocomposites are consisted of two compounds; Fe₃O₄ and SiO₂ and TEM images confirm formation of their core/shell structure. TEM images also show increase in silica shell thickness from ∼5 to ∼24 nm with increase in amount of tetraethyl orthosilicate (TEOS) used during the coating process from 0.1 to 0.3 mL. Magnetic studies indicate that Fe₃O₄ nanoparticles remain superparamagnetic after coating with silica although their M_s values are significantly less than pristine MNPs. These core/shell nanocomposites offer a high potential for different biomedical applications due to having superparamagnetic property of magnetite and unique properties of silica.     

Structure and magnetic properties of co-sputtered Co–C thin films

We studied the structure and magnetic properties of co-sputtered Co_1−xC_x thin films using a transmission electron microscope (TEM) and a SQUID magnetometer. These properties were found to depend critically on deposition temperature, T_S, and composition, x. Generally, phase separation into metallic Co and graphite-like carbon phases proceeds with increasing T_S and decreasing x. Plan view and cross-sectional TEM images of the films prepared showed that Co grains about 10–20 nm in diameter and 30–50 nm in height are three-dimensionally separated by graphite-like carbon layers 1–2 nm thick. Optimum magnetic properties with saturation magnetization of 380 emu/cc and coercivity of 400 Oe were obtained for a film with x=0.5 and T_S=350°C.