Influence of synthesis conditions on structural,optical and magnetic properties of iron oxide nanoparticles prepared by hydrothermal method

The iron oxide nanoparticles were synthesized by a simple hydrothermal method at different heating temperatures and pH conditions. The synthesized materials were characterized by X-ray diffractometer, Fourier transform infrared spectroscopy, field emission scanning electron microscopy, transmission electron microscopy, UV–visible spectrometer and vibrating sample magnetometer. With increment in pH of the synthesized materials were resulted in orthorhombic (goethite) and cubic (magnetite) structures at pH 6 and 12, respectively. The banding nature of synthesized materials was analyzed by infrared spectra. The synthesized powders at 130?°C showed higher percent of nanorods (length = 90–120 nm) in addition to lower percentage of nanoparticles. The material at pH 12 consisted of maximum nanoparticles with size = 10–60 nm with small agglomerations. Band gap energy of synthesized materials was 2.2–2.8 eV. Herein, the reaction conditions tuned the saturation magnetization (M_S). The maximum M_S (59.38 emu/g) was obtained at pH 12 and lower M_S (0.65 emu/g) was observed at pH 6 due to intrinsic property of goethite phase.     

Controlled synthesis of Sb<Subscript>2</Subscript>O<Subscript>3</Subscript> nanoparticles by chemical reducing method in ethylene glycol

Antimony trioxide (Sb₂O₃) nanoparticles with particle size range from 2 to 12 nm were successfully synthesized by chemical reducing method. Antimony trichloride was reduced by hydrazine with the presence of sodium hydroxide (NaOH) as catalyst in ethylene glycol at 120 °C for 1 h. Effects of hydrazine concentration ([N₂H₅OH]/[Sb³⁺] = 0.75, 5, 10, 20, and 30, when concentration of NaOH was fixed [NaOH]/[Sb³⁺] = 3) and NaOH concentration ([NaOH]/[Sb³⁺] = 0, 1, 3, and 5, when concentration of hydrazine was fixed [N₂H₅OH]/[Sb³⁺] = 10) on the particle size and shape of the Sb₂O₃ nanoparticles were investigated. Transmission electron microscope, selected area electron diffraction pattern, and high resolution electron microscope were employed to study the morphology and crystallinity of the nanoparticles. It was observed that the particle size decreased and remained constant when [N₂H₅OH]/[Sb³⁺]) ≥ 10 and [NaOH]/[Sb³⁺] = 3. Further study on the crystallinity and phase of the nanoparticles was assisted by X-ray diffractometer (XRD). XRD revealed a cubic phase of Sb₂O₃ (ICDD file no. 00-043-1071) with preferred plane of (622) and lattice spacing of 1.68 Å. Correlation between UV–visible absorption wavelengths of the nanoparticles and their sizes was established.     

Chemical synthesis and magnetic properties of HCP and FCC nickel nanoparticles

In this study, we successfully synthesized single-phase hexagonal closed packed (HCP) and face-centered cubic (FCC) nickel nanoparticles via reduction of nickel nitrate hexahydrate and nickel acetate tetrahydrate, respectively, in polyethylene glycol-200. Structural information of the as-synthesized nickel nanoparticles are studied by X-ray diffraction (XRD) as a function of the molar concentration of the nickel precursor. XRD results reveal that low concentrations of nickel precursor (0.005?M and below) favor the HCP, while high concentrations favor the mixture of HCP and FCC crystal structures. Particle size of HCP structure is found in the range of ～15?nm via transmission electron microscope analysis. Vibratory sample magnetometer is employed to study its magnetic behavior and the results reveal that FCC crystalline phase shows ferromagnetic nature with high saturation magnetization (M _s?～?39.6?emu?gm^?1) as compared to metastable HCP crystalline structure (M _s?～?2?emu?gm^?1). The surfactants bonding on the surface of nickel nanoparticles are studied.     

Effect of reaction condition on microstructure and properties of (NiCuZn)Fe2O4 nanoparticles synthesized via co-precipitation with ultrasonic irradiation

Nano-spinel ferrites synthesized via chemical co-precipitation method are small in size and have serious agglomeration phenomenon, which makes separation difficult in the subsequent process. Ni_0.4Cu_0.2Zn_0.4Fe₂O₄ ferrites nanoparticles were synthesized via co-precipitation assisted with ultrasonic irradiation produced by ultrasonic cleaner with 20 kHz frequency using chlorinated salts and KOH as initial materials. The effects of ultrasonic power (0, 40 W, 60 W, 80 W) and reaction temperature on the microstructure and magnetic properties of ferrite nanoparticles were investigated. The structure analyses via XRD revealed the successful formation of pure (NiCuZn)Fe₂O₄ ferrites nanospinel without any impurity. The crystallites sizes were less than 40 nm and the lattice constant was near 8.39 Å. The TEM showed ferrite particle polygonal. M−H analyses performed the saturation magnetization and coercivity of ferrite nanoparticles obtained at the reaction temperature of 25℃ were higher than at 50℃ with same power. The samples exhibited the highest values of Ms 55.67 emu/g at 25℃ and 47.77 emu/g at 50℃ for 60 W and the lowest values of Hc 71.23 Oe at 25℃ for 40 W and 52.85 Oe at 50℃ for 60 W. The squareness ratio (SQR) were found to be lower than 0.5, which revealed the single magnetic domain nature (NiCuZn)Fe₂O₄ nanoparticles. All the outcomes show the ultrasonic irradiation has positive effects on improving the microstructure and increasing magnetic properties.     

Fabrication of magnetic gold nanorod particles for immunomagnetic separation and SERS application

The preparation and application of rod-shaped core–shell structured Fe₃O₄–Au nanoparticles for immunomagnetic separation and sensing were described for the first time with this study. To synthesize magnetic gold nanorod particles, the seed-mediated synthetic method was carried out and the resulting nanoparticles were characterized with transmission electron microscopy (TEM), ultraviolet visible spectroscopy (UV–Vis), energy-dispersive X-ray (EDX), and X-ray diffraction (XRD). Magnetic properties of the nanoparticles were also examined. Characterization of the magnetic gold nanorod particles has proven that the resulting nanoparticles were composed of Fe₃O₄ core and the gold shell. The rod-shaped gold-coated iron nanoparticles have an average diameter of 16 ± 2 nm and an average length of about 50 ± 5 nm (corresponding aspect ratio of 3). The saturation magnetization value for the magnetic gold nanorod particles was found to be 37 emu/g at 300 K. Rapid and room temperature reaction synthesis of magnetic gold nanorod particles and subsequent surface modification with E. coli antibodies provide immunomagnetic separation and SERS application. The analytical performance of the SERS-based homogenous sandwich immunoassay system with respect to linear range, detection limit, and response time is also presented.     

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 characterization of superparamagnetic iron oxide nanoparticles for biomedical applications

Monodisperse iron oxide nanoparticles (NPs) of 4 nm were obtained through high-temperature solution phase reaction of iron (III) acetylacetonate with 1, 2-hexadecanediol in the presence of oleic acid and oleylamine. The as-synthesized iron oxide nanoparticles have been characterized by X-ray diffraction, transmission electron microscopy, Mössbauer spectroscopy and magnetic measurements. The species obtained were Fe₃O₄ and/or $\upgamma$ -Fe₂O₃. These NPs are superparamagnetic at room temperature and even though the reduced particle size they show a high saturation magnetization (MS ≈ 90 emu/g).     

Controlling magnetic properties of iron oxide nanoparticles using post-synthesis thermal treatment

Changes in morphological and magnetic properties of Fe₃O₄ nanoparticles before and after annealing are investigated in the present work. The nanoparticles are synthesized in a standard capacitively coupled plasma enhanced chemical vapour deposition system with two electrodes using ferrocene as the source compound. Post annealing, due to the sintering process, the particles fuse along with recrystallization. This results in increased size of the nanoparticles and the interparticle interaction, which play a major role in deciding the magnetic properties. X-ray diffraction patterns of the samples before and after annealing indicate a phase change from Fe₃O₄ to Fe₂O₃. Annealing at 200 ^°C causes the apparent saturation magnetization to increase from 6 emu?g^?1 to 15 emu?g^?1. When annealed at 500 ^°C, the magnetic properties of the nanoparticles resemble those of the bulk material. The evidence for the transition from a superparamagnetic state to a collective state is also observed when annealed at 500 ^°C. Variation of the magnetic relaxation data with annealing also reflects the change in the magnetic state brought about by the annealing. The correlation between annealing temperature and the magnetic properties can be used to obtain nanocrystallites of iron oxide with different sizes and magnetic properties.     

Microstructure and mechanical properties of a large-dimensional bulk nanocrystalline-based Fe–Al–Cr alloy prepared by an aluminothermic reaction casting and followed annealing at 1000 °C

A large-dimensional bulk nanocrystalline phase-based Fe–Al–Cr alloy with 10?wt.% Cr, which was about 200?mm in diameter and 10?mm in thickness, was prepared by an aluminothermic reaction casting and followed annealing at 1000?°C. Microstructures of the alloy were investigated by optical microscope, electron probe microscope, scanning electron microscope attached with electron backscattered diffraction, X-ray diffraction and transmission electron microscope. The magnetization curves of the alloy were tested by Lake Shore 7410 vibrating sample magnetometer. Compressive properties of the alloy were tested. The results show the alloy was consisted of a Fe–Al–Cr nanocrystalline matrix, Cr₇C₃ phase and contaminants in micrometre. Average grain size of the nanocrystalline matrix was 19?nm. Volume fraction of the Cr₇C₃ phase in the alloy was about 4.5%. After annealing, the saturated intensity of magnetization and the specific magnetic susceptibility of the alloy increased slightly from 99 emu/g and 0.083 emu/g?Oe to 104 emu/g and 0.113 emu/g?Oe, respectively. Compressive strength of the alloy was 1200?MPa and much higher than that of the small-scale nanocrystalline alloy and alloy with grains in micrometre.     

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.     

Synthesis and magnetic properties of single-crystalline BaFe12O19 nanoparticles

Rod-like and platelet-like nanoparticles of simple-crystalline barium hexaferrite (BaFe₁₂O₁₉) have been synthesized by the molten salt method. Both particle size and morphology change with the reaction temperature and time. The easy magnetization direction (0 0 l) of the BaFe₁₂O₁₉ nanoparticles has been observed directly by performing X-ray diffraction on powders aligned at 0.5 T magnetic field. The magnetic properties of the BaFe₁₂O₁₉ magnet were investigated with various sintering temperatures. The maximum values of saturation magnetization (σ_s=65.8 emu/g), remanent magnetization (σ_r=56 emu/g) and coercivity field (H_ic=5251 Oe) of the aligned samples occurred at the sintering temperatures of 1100 °C. These results indicate that BaFe₁₂O₁₉ nanoparticles synthesized by the molten salt method should enable detailed investigation of the size-dependent evolution of magnetism, microwave absorption, and realization of a nanodevice of magnetic media.     

Synthesis and characterization of manganese ferrite nanoparticles by thermal treatment method

Cubic structured manganese ferrite nanoparticles were synthesized by a thermal treatment method followed by calcination at various temperatures from 723 to 873 K. In this investigation, we used polyvinyl pyrrolidon (PVP) as a capping agent to control the agglomeration of the nanoparticles. The characterization studies were conducted by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The average particle sizes of manganese ferrite nanoparticles were determined by TEM, which increased with the calcination temperature from 12 to 22 nm and they had good agreement with XRD results. Fourier transform infrared spectroscopy confirmed the presence of metal oxide bands at all temperatures and the absence of organic bands at 873 K. Magnetic properties were demonstrated by a vibrating sample magnetometer, which showed a super-paramagnetic behavior for all samples and also saturation magnetization (M_s) increases from 3.06 to 15.78 emu/g by increasing the calcination temperature. The magnetic properties were also confirmed by the use of electron paramagnetic resonance spectroscopy, which revealed the existence of unpaired electrons and also measured peak-to-peak line width, resonant magnetic field and the g-factor.     

Effect of the particle size on the electrochemical performance of nano-Li2FeSiO4/C composites

Nano-Li₂FeSiO₄/C composites were prepared from three kinds of nano-SiO₂ (their particle sizes are 15?±?5, 30?±?5, and 50?±?5 nm, respectively) by a traditional solid-state reaction method. The as-prepared materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), elementary analyzer, Brunauer–Emmett–Teller (BET) analysis, galvanostatic charge–discharge test, and electrochemical impedance spectroscopy. XRD results reveal that nano-Li₂FeSiO₄ composites fabricated from nano-SiO₂ (smaller than 30 nm) have less impurity. SEM results indicate that the particle size of nano-Li₂FeSiO₄ composites is nearly accord with the particle size of nano-SiO₂. BET analysis indicates that the specific surface areas of LFS15, LFS30, and LFS50 are 35.10, 35.27, and 26.68 m² g, respectively, and the main pore size distribution of LFS15, LFS30, and LFS50 are 1.5, 5.5, and 10 nm, respectively. Electrochemical measurements indicate that nano-Li₂FeSiO₄ composites prepared from nano-SiO₂ of 30?±?5 nm have the best electrochemical performance among the three samples.     

Magnetic properties of prussian blue modified Fe3O4 nanocubes

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

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.     

Ni80Fe20 permalloy nanoparticles: Wet chemical preparation, size control and their dynamic permeability characteristics when composited with Fe micron particles

Ni₈₀Fe₂₀ permalloy nanoparticles (NPs) have been prepared by the polyol processing at 180 °C for 2 h and their particle sizes can be precisely controlled in the size range of 20-440 nm by proper addition of K₂PtCl₄ agent. X-ray diffraction results show that the Ni-Fe NPs are of FCC structure, and a homogeneous composition and a narrow size distribution of these NPs have been confirmed by scanning electron microscopy assisted with energy dispersion spectroscopy of X-ray (SEM-EDX). The saturation magnetization of ~440nm NPs is 80.8 emu/g that is comparable to that of bulk Ni₈₀Fe₂₀ alloys, but it decreases to 28.7 emu/g for ~20 nm NPs. The coercive force decreases from 90 to 3 Oe with decreasing NP size. The wide range of particle size is exploited to seek for high permeability composite particles. The planar type samples composed of the NiFe NPs exhibit low initial permeability due to the deteriorated magnetic softness and low packing density. However, when they are mixed with Fe micron particles, the initial permeability significantly increases depending on the mixing ratio and the NiFe NP size. A maximum initial permeability is achieved to be ~9.1 at 1 GHz for the Fe-10 vol%NiFe (~20 nmΦ), which is about three times that of pure Fe micron particles. The effects of Ni-Fe particle size, volume percentage and solvent on the static and dynamic permeability are discussed.     

Sol-gel derived nanoparticles of Zn substituted lithium ferrite (Li0.32Zn0.36Fe2.32O4): magnetic and Mössbauer effect measurements and their theoretical analysis

Nanoparticles of Zn substituted lithium ferrite (Li_0.32Zn_0.36Fe_2.32O₄) have been prepared by a sol-gel method where the ultra-sonication technique has been adopted to reduce the agglomeration effect among the nanoparticles. The samples were heat-treated at three different temperatures and the formation of the nanocrystalline phase was confirmed by X-ray diffractograms (XRD). The average particle size of each sample has been estimated from the (311) peak of the XRD pattern using the Debye-Scherrer formula and the average sizes are in the range of 10-21 nm. The average particle size, crystallographic phase, etc. of some selected samples obtained from the high-resolution transmission electron microscopy are in agreement with those estimated from the XRD patterns. Static magnetic measurements viz., hysteresis loops, field cooled and zero field cooled magnetization versus temperature curves of some samples carried out by SQUID in the temperature range of 300 to 5 K clearly indicate the presence of superparamagnetic (SPM) relaxation of the nanoparticles in the samples. The maximum magnetization of the SPM sample annealed at 500 °C is quite high (68 Am²/Kg) and the hysteresis loops are almost square shaped with very low value of coercive field at room temperature (827.8 A/m). The particle size, magneto-crystalline anisotropy, etc. have been estimated from the detailed theoretical analysis of the static magnetic data. The dynamic magnetic behavior of the samples was also investigated by observing the ac hysteresis loops and magnetization versus field curves with different time windows at room temperatures. The different soft magnetic quantities viz., coercive field, magnetization, remanance, hysteresis losses, etc. were extracted from dynamic measurements. Dynamic measurements confirmed that the samples are in their mixed state of SPM and ordered ferrimagnetic particles, which is in good agreement with the results of static magnetic measurements. Mössbauer spectra of the samples recorded at room temperature (300 K) and at different temperatures down to 20 K confirmed the presence of the SPM relaxation of the nanoparticles of the samples.     

Nanostructured Materials with Conducting and Magnetic Properties: Preparation of Magnetite/Conducting Copolymer Hybrid Nanocomposites by Ultrasonic Irradiation

Conducting copolymer poly(aniline-co-p-phenylenediamine) [poly(Ani-co-pPD)] and surface-modified magnetite (Fe₃O₄) composites were synthesized by ultrasonically-assisted chemical oxidative polymerization. Fe₃O₄ nanoparticles were surface-modified with silane coupling agent methacryloxypropyltrimethoxysilane (MPTMS) in order that they would be well dispersed for the reaction process. It was also found that the aggregation of Fe₃O₄ nanoparticles could be reduced under ultrasonic irradiation. TEM analysis confirmed that the resulting poly(Ani-co-pPD)/Fe₃O₄ nanocomposite showed core–shell morphology, in which Fe₃O₄ nanoparticles were well dispersed. The incorporation of Fe₃O₄ in the nanocomposites was endorsed by FT-IR. The nanocomposites were also confirmed by UV-visible, TGA and XRD. Conductivity of the nanocomposites was found to be in the range of 7.02 × 10^?4–6.54 × 10^?6 S/cm. Higher saturated magnetization of 12 emu/g was observed for composite with 20% Fe₃O₄.     

Magnetic nanoparticles based on iron coated carbon produced from the reaction of Fe2O3 with CH4: a Mössbauer study

In this work, it was investigated the production of magnetic nanoparticles encapsulated with carbon by the reaction of hematite and methane by Temperature Programmed Reaction up to 950°C. XRD and Mössbauer analyses showed that the materials prepared at 600°C and 700°C are mainly composed of magnetite and small amounts of hematite α -Fe₂O₃ with particle size of 30–40 nm. At higher temperatures, the spectra also display two central doublets corresponding to wüstite phase (Fe_1???x O). The materials were also characterized by magnetization measurements, BET surface area, thermal analysis (TG) and SEM. These materials can be prepared by a simple and low cost process and show great potential to be used as adsorbents and catalyst support.     

Evidence of a core–shell structure in the antiferromagnetic La0.2Ce0.8CrO3 nanoparticles by neutron scattering

We report the evidence of a core?Cshell structure in the antiferromagnetic La_0.2Ce_0.8CrO₃ nanoparticles by using a combination of neutron diffraction, polarized neutron small angle scattering (SANSPOL), and dc magnetization techniques. The neutron diffraction study establishes that the present nanoparticles are antiferromagnetic in nature. The magnetic scattering in the SANSPOL study arises from the shell part of the nanoparticles due to the disordered surface spins. The analysis of the SANSPOL data shows that these nanoparticles have a mean core diameter of 12.3±1.1?nm, and a shell thickness of 2.8±0.4?nm, giving a core?Cshell structure with an antiferromagnetic core, and a shell with a net magnetic moment under an applied magnetic field.