Synthesis and magnetic characterization of Zn0.7Ni0.3Fe2O4 nanoparticles via microwave-assisted combustion route

We report on the synthesis of Zn_0.7Ni_0.3Fe₂O₄ nanoparticles via microwave assisted combustion route by using urea as fuel. XRD and FT-IR analyses confirm the composition and structure as spinel ferrite. The crystallite size estimated from XRD (16.4 nm) and the magnetic core size (15.04 nm) estimated from VSM agree well, while a slightly smaller magnetic diameter reflects a very thin magnetically dead layer on the surface of the nanoparticles. Morphological investigation of the products was done by TEM which revealed the existence of irregular shapes such spherical, spherodial and polygon. Magnetization measurements performed on Zn_0.7Ni_0.3Fe₂O₄ nanoparticles showed that saturation was not attained at even in the high magnetic field. The sample shows superparamagnetic behavior at around the room temperature and ferromagnetic behavior below the blocking temperature which is measured as 284 K.     

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.     

High heat generation ability in AC magnetic field for nano-sized magnetic Y3Fe5O12 powder prepared by bead milling

Nano-sized magnetic Y₃Fe₅O₁₂ ferrite having a high heat generation ability in an AC magnetic field was prepared by bead milling. A commercial powder sample (non-milled sample) of ca. 2.9 μm in particle size did not show any temperature enhancement in the AC magnetic field. The heat generation ability in the AC magnetic field improved with a decrease in the average crystallite size for the bead-milled Y₃Fe₅O₁₂ ferrites. The highest heat ability in the AC magnetic field was for the fine Y₃Fe₅O₁₂ powder with a 15-nm crystallite size (the samples were milled for 4 h using 0.1 mm? beads). The heat generation ability of the excessively milled Y₃Fe₅O₁₂ samples decreased. The main reason for the high heat generation property of the milled samples was ascribed to an increase in the Néel relaxation of the superparamagnetic material. The heat generation ability was not influenced by the concentration of the ferrite powder. For the samples milled for 4 h using 0.1 mm? beads, the heat generation ability (W g⁻¹) was estimated using a 3.58×10⁻⁴ fH² frequency (f/kHz) and the magnetic field (H/kA m⁻¹), which is the highest reported value of superparamagnetic materials.     

Structure and magnetic properties of nanocrystalline cobalt ferrite powders synthesized using organic acid precursor method

Nanocrystalline octahedra of cobalt ferrite CoFe₂O₄ powders were synthesized using the organic acid precursor route. The effect of the calcination temperature, Fe³⁺/Co²⁺ molar ratio, calcination time and type of organic acid (oxalic, benzoic and tartaric acids) on the formation, crystallite size, microstructure and magnetic properties was studied systematically. The Fe³⁺/Co²⁺ molar ratio was varied from 2 to 1.739 while the annealing temperature was controlled from 400 to 1000 °C for various periods from 0.5 to 2 h. The resulting powders were investigated using X-ray diffraction (XRD) analysis, Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). XRD results indicate that a well crystallized, single spinel cobalt ferrite phase was formed for the precursors annealed at 600-800 °C for 2 h, using oxalic and tartaric acids as precursors for Fe³⁺/Co²⁺ molar ratio 1.818. The crystallite size of as-formed powders was in the range of 38.0-92.6 nm at different operating conditions. The calcination temperature and Fe³⁺/Co²⁺ molar ratio have a significant effect on the microstructure of the produced cobalt ferrite. The microstructure of the produced powders was found to be octahedra-shaped. The crystalline, pure cobalt ferrite powders with magnetic properties having a maximum saturation magnetization (76.1 emu/g) was achieved for the single phase at Fe³⁺/Co²⁺ molar ratio 1.818 and annealing temperature of 600 °C for 2 h using tartaric acid precursor.     

Preparation of barium hexaferrite nanopowders by the sol-gel method, using goethite

A series of barium hexaferrite nanoparticles (BaO·nFe₂O₃) with different n values were prepared by the sol-gel method, using goethite and Ba carbonate as raw materials. Phase identification of the samples was investigated by X-ray diffraction (XRD). XRD investigations show that the samples with n=5 and calcined at temperatures higher than 875 °C are single-phase Ba ferrite. An average crystallite size of 22 nm was obtained for the single-phase sample with minimum calcining temperature of 875 °C, using the Scherrer's formula. The morphology of the samples was checked by transmission electron microscope (TEM) and magnetic properties were measured by a sensitive permeameter. The results show that the samples have nonzero coercivities, which shows the particle size are not less than the critical size of Ba ferrite and then are not superparamagnet.     

Microwave synthesis of magnetic Fe3O4 nanoparticles used as a precursor of nanocomposites and ferrofluids

Methods to synthesize magnetic Fe₃O₄ nanoparticles and to modify the surface of particles are presented in the present investigation. Fe₃O₄ magnetic nanoparticles were prepared by the co-precipitation of Fe³⁺ and Fe²⁺, NH₃·H₂O was used as the precipitating agent to adjust the pH value, and the aging of Fe₃O₄ magnetic nanoparticles was accelerated by microwave (MW) irradiation. The obtained Fe₃O₄ magnetic nanoparticles were characterized by Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), X-ray powder diffraction (XRD) and vibrating sample magnetometer (VSM). The average size of Fe₃O₄ crystallites was found to be around 8–9 nm. Thereafter, the surface of Fe₃O₄ magnetic nanoparticles was modified by stearic acid. The resultant sample was characterized by FT-IR, scanning electron microscopy (SEM), XRD, lipophilic degree (LD) and sedimentation test. The FT-IR results indicated that a covalent bond was formed by chemical reaction between the hydroxyl groups on the surface of Fe₃O₄ nanoparticles and carboxyl groups of stearic acid, which changed the polarity of Fe₃O₄ nanoparticles. The dispersion of Fe₃O₄ in organic solvent was greatly improved. Effects of reaction time, reaction temperature and concentration of stearic acid on particle surface modification were investigated. In addition, Fe₃O₄/polystyrene (PS) nanocomposite was synthesized by adding surface modified Fe₃O₄ magnetic nanoparticles into styrene monomer, followed by the radical polymerization. The obtained nanocomposite was tested by thermogravimetry (TG), differential scanning calorimetry (DSC) and XRD. Results revealed that the thermal stability of PS was not significantly changed after adding Fe₃O₄ nanoparticles. The Fe₃O₄ magnetic fluid was characterized using UV–vis spectrophotometer, Gouy magnetic balance and laser particle-size analyzer. The testing results showed that the magnetic fluid had excellent stability, and had susceptibility of 4.46×10⁻⁸ and saturated magnetization of 6.56 emu/g. In addition, the mean size d (0.99) of magnetic Fe₃O₄ nanoparticles in the fluid was 36.19 nm.     

Synthesis of Fe3O4/CNTs magnetic nanocomposites at the liquid-liquid interface using oleate as surfactant and reactant

Carbon nanotubes (CNTs)-based magnetic nanocomposites have attracted significant research interest owing to their great potentialities in various technological fields. In this investigation, a kind of novel Fe₃O₄/CNTs magnetic nanocomposites were prepared by in situ chemical precipitation using oleate as reactant and surfactant at the liquid-liquid interface of cyclohexane/ethanol/water mixture solvent. The as-prepared samples were characterized via transmission electron microscopy (TEM), X-ray diffractometry (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FTIR) and vibration sample magnetometry (VSM). Results indicated that the Fe₃O₄/CNTs magnetic nanocomposites dispersed well in organic medium were prepared organic medium, were prepared. The magnetic nanocomposites were proved to be superparamagnetic with coercive force of 3.69 Oe. A mechanism scheme was proposed to illustrate the formation process of the magnetic nanocomposites.     

Biosynthesis and magnetic properties of mesoporous Fe3O4 composites

Magnetic Fe₃O₄ materials with mesoporous structure are synthesized by co-precipitation method using yeast cells as a template. The X-ray diffraction (XRD) pattern indicates that the as-synthesized mesoporous hybrid Fe₃O₄ is well crystallized. The Barrett-Joyner-Halenda (BJH) models reveal the existence of mesostructure in the dried sample which has a specific surface area of 96.31 m²/g and a pore size distribution of 8-14 nm. Transmission electron microscopy (TEM) measurements confirm the wormhole-like structure of the resulting samples. The composition and chemical bonds of the Fe₃O₄/cells composites are studied by Fourier transform infrared (FT-IR) spectroscopy. Preliminary magnetic properties of the mesoporous hybrid Fe₃O₄ are characterized by a vibrating sample magnetometer (VSM). The magnetic Fe₃O₄/cells composites with mesoporous structure have potential applications in biomedical areas, such as drug delivery.     

Preparation and characterization of silica-coated Fe3O4 nanoparticles used as precursor of ferrofluids

Fe₃O₄ magnetic nanoparticles (MNPs) were synthesized by the co-precipitation of Fe³⁺ and Fe²⁺ with ammonium hydroxide. The sodium citrate-modified Fe₃O₄ MNPs were prepared under Ar protection and were characterized by Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), X-ray powder diffraction (XRD) and vibrating sample magnetometer (VSM). To improve the oxidation resistance of Fe₃O₄ MNPs, a silica layer was coated onto the modified and unmodified MNPs by the hydrolysis of tetraethoxysilane (TEOS) at 50 °C and pH 9. Afterwards, the silica-coated Fe₃O₄ core/shell MNPs were modified by oleic acid (OA) and were tested by IR and VSM. IR results revealed that the OA was successfully grafted onto the silica shell. The Fe₃O₄/SiO₂ core/shell MNPs modified by OA were used to prepare water-based ferrofluids (FFs) using PEG as the second layer of surfactants. The properties of FFs were characterized using a UV-vis spectrophotometer, a Gouy magnetic balance, a laser particle size analyzer and a Brookfield LVDV-III+ rheometer.     

Study of polydiethylsiloxane-based ferrofluid with excellent frost resistance property

The polydiethylsiloxane-based ferrofluid was prepared by dispersing finely divided magnetic Fe₃O₄ particles which are modified with oleoyl sarcosine and lauroyl sarcosine. The optimized experiment parameters including molar ratio of surfactant to Fe₃O₄ (1:5), temperature (80 °C), stirring rate (300 RPM), the surfactant content of lauroyl sarcosine (0 to 33 mol%) and the modification time (25 min) were obtained by the orthogonal test. The magnetic liquid was characterized by a transmission electron microscope (TEM), infrared (IR) spectrometer, X-ray diffractometer (XRD), thermogravimetry (TG), vibrating sample magnetometer (VSM) and differential scanning calorimetry (DSC). It is indicated that the surfactant is mainly bonded to the surface of Fe₃O₄ nanoparticles through covalent bond between carboxylate (COO⁻) and Fe atom. The modified magnetic particles are equally dispersed into the carrier and remain stable below −12 °C over 4 months. The ferrofluids exhibit excellent frost resistance property and distinctly reduced temperature coefficient of viscosity compared with polydimethylsiloxane-based ferrofluids and hydrocarbon-based ferrofluids, respectively. The saturation magnetization could reach up to 27.7 emu/g.     

Synthesis and characterization of lithium ferrite by oxalate precursor route

Nanocrystalline lithium ferrite (LiFe₅O₈) powders have been synthesized by oxalate precursor route. The effects of Fe³⁺/Li⁺ mole ratio, and annealing temperature on the formation, crystalline size, morphology and magnetic properties were systematically studied. The Fe³⁺/Li⁺ mole ratio was controlled from 5 to 3.33 while the annealing temperature was controlled from 600 to 1100 °C. The resultant powders were investigated by differential thermal analyzer (DTA), X-ray diffractometer (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). DTA results showed that LiFe₅O₈ phase started to form at around 520 °C. XRD indicated that LiFe₅O₈ phase always contained α-Fe₂O₃ impurity and the hematite phase formation increased by increasing the annealing temperature ?850 °C for different Fe³⁺/Li⁺ mole ratios 5, 4.55 and 3.85. Moreover, lithium ferrite phase was formed with high conversion percentage at critical annealing temperature 750–800 °C. Single well crystalline LiFe₅O₈ phase was obtained at Fe³⁺/Li⁺ mole ratio 3.33 and annealing temperatures from 800 to 1000 °C. Maximum saturation magnetization (68.7 emu/g) was achieved for the formed lithium ferrite phase at Fe³⁺/Li⁺ mole ratio 3.33 and annealing temperature 1000 °C.     

Effect of zinc substitution on magnetic and electrical properties of nanocrystalline nickel ferrite synthesized by refluxing method

Nanocrystalline Nickel ferrite (NiFe₂O₄) and Zn substituted nickel ferrite (NiZnFe₂O₄) have been synthesized by the refluxing method. These ferrites were characterized by XRD, TEM, Mossbauer spectroscopy and VSM in order to study the effect of zinc substitution in nickel ferrite. XRD diffraction results confirm the spinel structure for the prepared nanocrystalline ferrites with an average crystallite size of 14-16 nm. Lattice parameter was found to increase with the substitution of Zn²⁺ ions from 8.40 Å to 8.42 Å. TEM images confirmed average particle size of about 20 nm and indicates nanocrystalline nature of the compounds. A shift in isomeric deviation with the doublet was observed due to the influence of Zn substitution in the nickel ferrite. The Zn content has a significant influence on the magnetic behavior and electrical conductivity of NiFe₂O₄. Saturation magnetization drastically increased whereas room temperature electrical conductivity decreased due to the addition of Zn content in NiFe₂O₄, indicating super magnetic material with lesser coercivity.     

Magnetic and bioactivity evaluation of ferrimagnetic ZnFe2O4 containing glass ceramics for the hyperthermia treatment of cancer

Glass ceramics of the composition xZnO·25Fe₂O₃·(40−x)SiO₂·25CaO·7P₂O₅·3Na₂O were prepared by the melt-quench method using oxy-acetylene flame. Glass-powder compacts were sintered at 1100 °C for 3 h and then rapidly cooled at −10 °C. X-ray diffraction (XRD) revealed 3 prominent crystalline phases: ZnFe₂O₄, CaSiO₃ and Ca₁₀(PO₄)₆(OH)₂. Vibrating sample magnetometer (VSM) data at 10 KOe and 500 Oe showed that saturation magnetization, coercivity and hence hysteresis area increased with the increase in ZnO content. Nano-sized ZnFe₂O₄ crystallites were of pseudo-single domain structure and thus coercivity increased with the increase in crystallite size. ZnFe₂O₄ exhibited ferrimagnetism due to the random distribution of Zn²⁺ and Fe³⁺ cations at tetrahedral A sites and octahedral B sites. This inversion/random distribution of cations was probably due to the surface effects of nano-ZnFe₂O₄ and rapid cooling of the material from 1100 °C (thus preserving the high temperature state of the random distribution of cations). Calorimetric measurements were carried out using magnetic induction furnace at 500 Oe magnetic field and 400 KHz frequency. The data showed that maximum specific power loss and temperature increase after 2 min were 26 W/g and 37 °C, respectively for the sample containing 10% ZnO. The samples were immersed in simulated body fluid (SBF) for 3 weeks. Scanning electron microscope (SEM), energy dispersive spectroscopy (EDX) and XRD results confirmed the growth of precipitated hydroxyapatite phase after immersion in SBF, suggesting that the ferrimagnetic glass ceramics were bioactive and could bond to the living tissues in physiological environment.     

The effect of La-substitution on magnetic properties of nanosized Sr1−xLaxTi0.05Zn0.2(Fe)11.75−δ(Fe)δO19 powders

A series of La-substituted M-type Sr hexaferrite powders Sr_1−xLa_xTi_0.05Zn_0.2Fe³⁺_11.75O₁₉, wherein x ranges from 0.1 to 0.5 with a step of 0.1, have been prepared by the conventional ceramic method and were then milled in a high energy mill to prepare nanosized powders. XRD investigation of the calcined and the milled powders shows that single phase hexaferrite structure has been formed after calcining and has not changed after milling. The lattice parameters and the mean crystallite sizes of the samples have been determined from the XRD data and Scherrer's formula. The results show that the lattice parameters (“а” and “c”) decrease with increase in La-substitution and the mean crystallite size of the milled powders is about 17 nm. Coercivities and magnetizations of the samples in a magnetic field of 16 kOe have been determined from the room temperature hysteresis loops. It was found that both parameters increase with La substitutions up to 0.3 and then decrease for higher substitutions. These variations were attributed to the enhancement of hyperfine field and spin-canting magnetic structure when La content increases. In addition, the magnetizations were smaller for the nanosized samples in comparison with those of bulk ones, which were discussed according to the core-shell model. Also the results show that annealing of the nanosized samples up to 500 °C can enhance coercivity and magnetization of the samples, which is discussed based on crystallite size growth.     

Effect of high magnetic field annealing on the microstructure and magnetic properties of Co-Fe layered double hydroxide

The effects of high magnetic field (10 T) on the products obtained by calcination of Co-Fe LDH precursors at different temperatures were investigated. The XRD results indicated that Fe^III substituted for Co^III in Co₃O₄ to yield Co^IICo^IIIFe^IIIO₄ under the calcination of Co-Fe LDH precursors at 400 °C. The products obtained by magnetic field annealing at 400 °C had a porous plate-like morphology, whereas the products without magnetic field annealing were composed of nanoparticles. It was seen that CoFe₂O₄ phase could be formed at low temperature (about 500 °C) under the magnetic field annealing. The grain size of products obtained by magnetic field annealing at 800 °C was larger than that of zero magnetic field. It was found that the saturation magnetization was significantly enhanced after magnetic field annealing, especially at lower temperature (≤600 °C). The possible reason for the effects on the microstructure and magnetic properties of products obtained by magnetic field annealing was discussed.     

Application of citrate-stabilized gold-coated ferric oxide composite nanoparticles for biological separations

Gold-coated magnetic nanoparticles were synthesized with size ranging from 15 to 40 nm using sodium citrates as the reducing agent. Oxidized magnetites (Fe₃O₄) fabricated by co-precipitation of Fe²⁺ and Fe³⁺ in strong alkaline solution were used as magnetic cores. The structures of gold (Au) shell and magnetic core (Au–Fe) were studied by transmission electron microscopy (TEM) image and energy dispersive spectroscopy (EDS) spectrum. Results from high-resolution X-ray diffraction (HR XRD) show that the Au–Fe oxide nanoparticles have a face-centered cubic shape with the crystalline faces of {1 1 1}. The Au-coated magnetic nanoparticles exhibited a surface plasmon resonance peak at 528 nm. The nanoparticles are well dispersed in distilled water. A 3000 G permanent magnet was successfully used for the separation of the functionalized nanoparticles. Magnetic properties of the nanoparticles were determined by magnetic force microscope (MFM) in nanometric resolution and vibrating sample magnetometer (VSM). Magnetic separation of biological molecules using Au-coated magnetic oxide composite nanoparticles was examined after attachment of protein immunoglobulin G (IgG) through electrostatic interactions. Using this method, separation was achieved with a maximum yield of 35% at an IgG concentration of 400 ng/ml.     

Synthesis and magnetic characterization of Zn0.6Ni0.4Fe2O4 nanoparticles via a polyethylene glycol-assisted hydrothermal route

Zn-doped nickel ferrite nanoparticles (Zn_0.6Ni_0.4Fe₂O₄) have been prepared via a surfactant, polyethylene glycol assisted hydrothermal route. X-ray powder diffractometry (XRD), Fourier transform infrared spectroscopy, transmission electron microscopy (TEM), and vibrating scanning magnetometry (VSM) were used for the structural, morphological, and magnetic characterizations of the product, respectively. TEM analysis revealed that the nanoparticles have a narrow size distribution, with average particle size of 15±1 nm, which agrees well with the XRD based estimate of 14±2 nm. The absence of saturation and remanent magnetization, and coercivity in the high temperature region of the M-H curve and non-zero magnetic moments indicate superparamagnetism of the nanoparticles with a canted spin structure. The appearance of a peak on the temperature-dependent zero-field cooling magnetization curve at ∼190 K indicates the blocking temperature of the sample.     

Green synthesis and characterization of superparamagnetic Fe3O4 nanoparticles

In this paper, we have first demonstrated a facile and green synthetic approach for preparing superparamagnetic Fe₃O₄ nanoparticles using α-d-glucose as the reducing agent and gluconic acid (the oxidative product of glucose) as stabilizer and dispersant. The X-ray powder diffraction (XRD), X-ray photoelectron spectrometry (XPS), and selected area electron diffraction (SAED) results showed that the inverse spinel structure pure phase polycrystalline Fe₃O₄ was obtained. The scanning electron microscopy (SEM) and transmission electron microscopy (TEM) results exhibited that Fe₃O₄ nanoparticles were roughly spherical shape and its average size was about 12.5 nm. The high-resolution TEM (HRTEM) result proved that the nanoparticles were structurally uniform with a lattice fringe spacing about 0.25 nm, which corresponded well with the values of 0.253 nm of the (3 1 1) lattice plane of the inverse spinel Fe₃O₄ obtained from the JCPDS database. The superconducting quantum interference device (SQUID) results revealed that the blocking temperature (T_b) was 190 K, and that the magnetic hysteresis loop at 300 K showed a saturation magnetization of 60.5 emu/g, and the absence of coercivity and remanence indicated that the as-synthesized Fe₃O₄ nanoparticles had superparamagnetic properties. Fourier transform infrared spectroscopy (FT-IR) spectrum displayed that the characteristic band of Fe-O at 569 cm⁻¹ was indicative of Fe₃O₄. This method might provide a new, mild, green, and economical concept for the synthesis of other nanomaterials.     

The effect of aging time and calcination temperature on the magnetic properties of α-Fe/Fe3O4 composite

Composites of α-Fe/Fe₃O₄ having dimensions in the range of 100–150 nm have been prepared by disproportion method. The structure and morphology are investigated by XRD and TEM. XRD shows that the metal has got the BCC structure. TEM shows balls of metallic iron about 100-nm-wide stuck to magnetite grains. Magnetic measurement shows that the sample aged for 3 h and calcined at 200 °C has the maximal saturation magnetization corresponding to the highest concentration of α-Fe in the final sample.     

The effect of solution temperature on crystallite size and magnetic properties of Zn substituted Co ferrite nanoparticles

In this work zinc substituted cobalt ferrite nanoparticles (Co_0.5Zn_0.5Fe₂O₄) have been synthesized by the coprecipitation method, using stable ferric, zinc and cobalt salts with sodium hydroxide, at different solution temperatures, from room temperature to 363 K. The cobalt-zinc ferrite crystalline phase, the particle size and the morphology of the resulting nanoparticles were studied by X-ray diffraction and transmission electron microscopy. The average crystallite size of each sample was calculated from the broadening of the most intense peak (3 1 1), using Scherrer's formula and the results show crystallite sizes increased from 6 to 8 nm by increasing the solution temperature from room temperature to 363 K respectively. Room temperature VSM measurements show that the prepared nanoparticles have superparamagnetic behavior and did not saturate at maximum field of 800 kA/m. The variation of AC-susceptibility of the samples with respect to temperature was measured and it was found that the blocking temperature increased from 198 to 270 K by increasing the solution temperature from room temperature to 363 K respectively. FTIR spectra of the samples have been analyzed in the frequency range 400-4000 cm⁻¹, which also confirms the results of XRD.