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1.
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 (MS). The maximum MS (59.38 emu/g) was obtained at pH 12 and lower MS (0.65 emu/g) was observed at pH 6 due to intrinsic property of goethite phase.  相似文献   

2.
A new method to produce elaborate nanostructure with magnetic and fluorescent properties in one entity is reported in this article. Magnetite (Fe3O4) coated with fluorescent silica (SiO2) shell was produced through the one-pot reaction, in which one reactor was utilized to realize the synthesis of superparamagnetic core of Fe3O4, the formation of SiO2 coating through the condensation and polymerization of tetraethylorthosilicate (TEOS), and the encapsulation of tetramethyl rhodamine isothiocyanate-dextran (TRITC-dextran) within silica shell. Transmission electron microscopy (TEM), energy dispersive X-ray (EDX) analysis, and X-ray diffraction (XRD) were carried out to investigate the core–shell structure. The magnetic core of the core–shell nanoparticles is 60 ± 10 nm in diameter. The thickness of the fluorescent SiO2 shell is estimated at 15 ± 5 nm. In addition, the fluorescent signal of the SiO2 shell has been detected by the laser confocal scanning microscopy (LCSM) with emission wavelength (λem) at 566 nm. In addition, the magnetic properties of TRITC-dextran loaded silica-coating iron oxide nanoparticles (Fe3O4@SiO2 NPs) were studied. The hysteresis loop of the core–shell NPs measured at room temperature shows that the saturation magnetization (M s) is not reached even at the field of 70 kOe (7T). Meanwhile, the very low coercivity (H c) and remanent magnetization (M r) are 0.375 kOe and 6.6 emu/g, respectively, at room temperature. It indicates that the core–shell particles have the superparamagnetic properties. The measured blocking temperature (T B) of the TRITC-dextran loaded Fe3O4@SiO2 NPs is about 122.5 K. It is expected that the multifunctional core–shell nanoparticles can be used in bio-imaging.  相似文献   

3.
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 (Ms) values of the Fe/Cu core–shell particles are varied owing to the different thickness of copper layer. Though the Ms value of the Fe/Cu nanocomposite is lower than that of pure iron nanoparticles, the higher Ms 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.  相似文献   

4.
A novel method is described for the preparation of superparamagnetic mesoporous maghemite (γ-Fe2O3)/silica (SiO2) composite microspheres to allow rapid magnetic separation of DNA from biological samples. With magnetite (Fe3O4) and silica nanoparticles as starting materials, such microspheres were synthesized by the following two consecutive steps: (1) formation of monodispersed organic/inorganic hybrid microspheres through urea-formaldedyde (UF) polymerization and (2) removal of the organic template and phase transformation of Fe3O4 to γ-Fe2O3 by calcination at elevated temperatures. The as-synthesized particles obtained by heating at temperature 300 °C feature spherical shape and uniform particle size (dparticle=1.72 μm), high saturation magnetization (Ms=17.22 emu/g), superparamagnetism (Mr/Ms=0.023), high surface area (SBET=240 m2/g), and mesoporosity (dpore=6.62 nm). The composite microsphere consists of interlocked amorphous SiO2 nanoparticles, in which cubic γ-Fe2O3 nanocrystals are homogeneously dispersed and thermally stable against γ- to α-phase transformation at temperatures up to 600 °C. With the exposed iron oxide nanoparticles coated with a thin layer of silica shell, the magnetic microspheres were used as a solid-phase adsorbent for rapid extraction of genomic DNA from plant samples. The results show that the DNA templates isolated from pea and green pepper displayed single bands with molecular weights greater than 8 kb and A260/A280 values of 1.60-1.72. The PCR amplification of a fragment encoding the endogenous chloroplast ndhB gene confirmed that the DNA templates obtained were inhibitor-free and amenable to sensitive amplification-based DNA technologies.  相似文献   

5.
Synthesis of magnetite (Fe3O4) nanoparticles under oxidizing environment by precipitation from aqueous media is not straightforward because Fe2+ gets oxidized to Fe3+ and thus the ratio of Fe3+:Fe2+=2:1 is not maintained during the precipitation. A molar ratio of Fe3+:Fe2+ smaller than 2:1 has been used by many to compensate for the oxidation of Fe2+ during the preparation. In this work, we have prepared iron oxide nanoparticles in air environment by the precipitation technique using initial molar ratios Fe3+:Fe2+?2:1. The phases of the resulting powders have been determined by several techniques. It is found that the particles consist mainly of maghemite with little or no magnetite phase. The particles have been suspended in non-aqueous and aqueous media by coating the particles with a single layer and a bilayer of oleic acid, respectively. The particle sizes, morphology and the magnetic properties of the particles and the ferrofulids prepared from these particles are reported. The average particle sizes obtained from the TEM micrographs are 14, 10 and 9 nm for the water, kerosene and dodecane-based ferrofluids, respectively, indicating a better dispersion in the non-aqueous media. The specific saturation magnetization (σs) value of the oleic-acid-coated particles (∼53 emu/g) is found to be lower than that for the uncoated particles (∼63 emu/g). Magnetization σs of the dodecane-based ferrofluid is found to be 10.1 emu/g for a volume fraction of particles ?=0.019. Zero coercivity and zero remanance on the magnetization curves indicate that the particles are superparamagnetic (SPM) in nature.  相似文献   

6.
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.  相似文献   

7.
Superparamagnetic iron oxide nanoparticles are used in diverse applications, including optical magnetic recording, catalysts, gas sensors, targeted drug delivery, magnetic resonance imaging, and hyperthermic malignant cell therapy. Combustion synthesis of nanoparticles has significant advantages, including improved nanoparticle property control and commercial production rate capability with minimal post-processing. In the current study, superparamagnetic iron oxide nanoparticles were produced by flame synthesis using a coflow flame. The effect of flame configuration (diffusion and inverse diffusion), flame temperature, and additive loading on the final iron oxide nanoparticle morphology, elemental composition, and particle size were analyzed by transmission electron microscopy (TEM), high-resolution TEM (HR-TEM), energy dispersive spectroscopy (EDS), and Raman spectroscopy. The synthesized nanoparticles were primarily composed of two well known forms of iron oxide, namely hematite αFe2O3 and magnetite Fe3O4. We found that the synthesized nanoparticles were smaller (6–12 nm) for an inverse diffusion flame as compared to a diffusion flame configuration (50–60 nm) when CH4, O2, Ar, and N2 gas flow rates were kept constant. In order to investigate the effect of flame temperature, CH4, O2, Ar gas flow rates were kept constant, and N2 gas was added as a coolant to the system. TEM analysis of iron oxide nanoparticles synthesized using an inverse diffusion flame configuration with N2 cooling demonstrated that particles no larger than 50–60 nm in diameter can be grown, indicating that nanoparticles did not coalesce in the cooler flame. Raman spectroscopy showed that these nanoparticles were primarily magnetite, as opposed to the primarily hematite nanoparticles produced in the hot flame configuration. In order to understand the effect of additive loading on iron oxide nanoparticle morphology, an Ar stream carrying titanium-tetra-isopropoxide (TTIP) was flowed through the outer annulus along with the CH4 in the inverse diffusion flame configuration. When particles were synthesized in the presence of the TTIP additive, larger monodispersed individual particles (50–90 nm) were synthesized as observed by TEM. In this article, we show that iron oxide nanoparticles of varied morphology, composition, and size can be synthesized and controlled by varying flame configuration, flame temperature, and additive loading.  相似文献   

8.
We have synthesized the iron oxide nanoparticles using the newly developed mechanical ultrasonication method with the FeSO4 · 7H2O. We have also investigated the crystallographic structural properties, morphology, and magnetic properties of the nanopowders. According to the high resolution X-ray diffraction result, the as-synthesized iron oxide nanoparticles were magnetite (Fe3O4). The particle size of the magnetite nanoparticles was about 6 nm confirmed by transmission electron microscopy image. The particle shape was almost a sphere confirmed by scanning electron microscopy image. The coercivity and saturation magnetization of the as-synthesized iron oxide nanopowders were 114 Oe, and 3.7 emu/g, respectively.  相似文献   

9.
For the first time nanocrystalline magnetic particles of Mg x Fe(3−x)O4 with x ranging from 0.5 to 1.5 have been synthesized by a combustion reaction method using iron nitrate Fe(NO3)3.9H2O, magnesium nitrate Mg(NO3)2.6H2O, and urea CO(NH2)2 as fuel without intermediate decomposition and/or calcining steps. X-ray diffraction patterns of all systems showed broad peaks consistent with cubic inverse spinel structure of MgFe2O4. The absence of extra reflections in the diffraction patterns of as-prepared materials ensures the phase purity. The mean crystallite sizes determined from the prominent (311) peak of the diffraction using Scherrer’s equation and transmission electron microscopy micrographs were c.a. 40 nm with spherical morphology. Fourier transform infrared spectra of the as-prepared material showed traces of organic and metallic salt by-products; however, these could be removed by washing with deionized water. Typical hysteresis curves were obtained for all specimens in magnetic field up to 14 T between 4 and 340 K. The saturation magnetization was 48.3 emu/g and 31.3 emu/g, 44.8 emu/g, and 28.4 emu/g for x=1.0 and 0.8 at 4 K and 340 K, respectively. The saturation magnetization, M s , of nanoparticles of the MgFe2O4 specimen is about 50% higher when compared to the bulk. The enhanced magnetization measured in our nanoparticles MgFe2O4 specimens may be attributed to the uncompensated magnetic moment of iron ions between the A- and B-sites, i.e., changes in the inversion factor. Our magnetization results of MgFe2O4 specimens are comparable to the existing data for the same compound but with different particle size and prepared by different synthesis methods.  相似文献   

10.
《Current Applied Physics》2019,19(4):548-555
Magnetic powders of nickel ferrite (NiFe2O4) were successfully synthesized by combustion synthesis in air using iron (Fe), iron oxide (Fe2O3), and nickel oxide (NiO) as reactants and sodium perchlorate (NaClO4) as fuel (or oxidizing agent). The thermal behaviors were characterized using thermogravimetric analysis (TG) and differential thermal analysis (DSC). The as-combusted and final nickel ferrite powders were characterized in terms of chemical composition and morphology by X-Ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), and scanning electron microscopy (SEM) coupled with energy dispersive X-Ray spectroscopy (EDX). In addition, magnetic properties were examined by vibrating sample magnetometer (VSM). The results of TG/DSC analysis indicated that increasing the content of NaClO4 increased the exothermicity of combustion reaction. XRD indicated that the final nickel ferrite powders formed a single spinel NiFe2O4 phase when the amount of NaClO4 used was 0.08 or 0.10 mol. SEM revealed roughly octahedron particles with sizes in a sub-micrometer range (∼500 nm). All final products exhibited soft magnetism and, synthesis that included 0.1 mol of NaClO4 produced pure NiFe2O4 powders that had a saturation magnetization (Ms) of 58.93 emu/g, which is higher than the reported value (55 emu/g) for the bulk product.  相似文献   

11.
Obtaining small (<50 nm), monodispersed, well-separated, single iron oxide core–silica (SiO2) shell nanoparticles for biomedical applications is still a challenge. Preferably, they are synthesised by inverse microemulsion method. However, substantial amount of aggregated and multicore core–shell nanoparticles is the undesired outcome of the method. In this study, we report on the production of less than 50 nm overall size, monodispersed, free of necking, single core iron oxide–SiO2 shell nanoparticles with tuneable shell thickness by a carefully optimized inverse microemulsion method. The high degree of control over the process is achieved by understanding the mechanism of core–shell nanoparticles formation. By varying the reaction time and precursor concentration, the thickness of silica layer on the core nanoparticles can be finely adjusted from 5 to 13 nm. Residual reactions during the workup were inhibited by a combination of pH control with shock freezing and ultracentrifuging. These high-quality tuneable core–shell nanocomposite particles exhibit superparamagnetic character and sufficiently high magnetization with great potential for biomedical applications (e.g. MRI, cell separation and magnetically driven drug delivery systems) either as-prepared or by additional surface modification for improved biocompatibility.  相似文献   

12.
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.  相似文献   

13.
This study reports the new and simple synthesis of magnetic La0.7Sr0.3MnO3 (LSMO) nanoparticles by thermal decomposition method using acetate salts of La, Sr and Mn as starting materials. To obtain the LSMO nanoparticles, thermal decomposition of the precursor is carried out at the temperatures of 600, 700, 800, 900, and 1000°C for 6 hours. The synthesized LSMO nanoparticles were characterized by XRD, FT-IR, TEM and SEM. Structural characterization shows that the prepared particles consisted of two phases of LaMnO3 (LMO) and LSMO with crystallite sizes ranging from 18 to 55 nm. All the prepared samples have a perovskite structure which changes from cubic to rhombohedral with the increase in the thermal decomposition temperature. Basic magnetic characteristics such as saturation magnetization (M S) and coercive field (H C) are evaluated by sample vibrating magnetometry at room temperature (20°C). The samples show soft ferromagnetic behavior with M S values of ∼9–55 emu/g and H C values of ∼8–37 Oe, depending on the crystallite size and thermal decomposition temperature. The relationship between the crystallite size and the magnetic properties is presented and discussed. The cytotoxicity of synthesized LSMO nanoparticles was also evaluated with NIH 3T3 cells and the result showed that the synthesized nanoparticles were not toxic to the cells as determined from cell viability in response to the liquid extraction of LSMO nanoparticles.  相似文献   

14.
Vidyadhar Singh  S. Ram 《哲学杂志》2013,93(11):1401-1414
Ni nanoparticles (Ni-NPs), with diameter (D) ranging 5–30 nm, were synthesized by reducing nickel chloride with NaBH4 in the presence of polymer molecules of poly-vinyl alcohol (PVA) in cold water. Nickel chloride was dispersed in the PVA molecules which stabilized the resulting Ni-NPs. Experiments were carried out with and without PVA to elucidate the effect of PVA molecules on the structural and magnetic properties of Ni-NPs. It was found that both uncoated (uc) and PVA-coated (pc) Ni-NPs exhibit a tetragonal (t) crystal structure, i.e. different from the cubic (fcc) structure of bulk nickel. pc Ni-NPs (paramagnetic in nature) converted to fcc Ni (spherical shape, D ~ 12 nm) on annealing at 573 K in air, exhibiting a saturation magnetization M s = 20.5 emu/g, squareness ratio M r /M s = 0.48 and coercivity H c = 248 Oe, which is higher than the bulk Ni (0.7 Oe). uc Ni-NPs showed little improvement in M s and H c on air annealing. The core–shell structure resulted in a high H c value in stable pc Ni-NPs in air. Electron magnetic resonance revealed exchange interaction between the core and shell, which changes on annealing in air.  相似文献   

15.
In this paper, we report a new route to synthesize novel magnetic hollow silica nanospheres (MHSNs) using polystyrene particles as sacrificial templates, and TEOS and Fe3O4 as precursors. TEM, EDS, XRD, and SQUID were applied to characterize MHSNs. TEM and EDS results show that the MHSNs consist of about 200 nm of hollow cores and ∼35 nm shells with ∼10 nm of Fe3O4 nanoparticles embedded. The polystyrene beads were successfully removed by immersing the as-prepared silica nanocomposite in a toluene solution. XRD results demonstrate that the Fe3O4 magnetic nanoparticles still keep spinel structure even heated at low temperature. The surface status of the polystyrene beads and Fe3O4 nanoparticles has an important effect on the formation of the MHSNs. The MHSNs present a superparamagnetism at room temperature by SQUID measurement. The MHSNs have potential applications in biosystem and nanomedicine.  相似文献   

16.
Mn-Zn ferrite nanoparticles with various amounts of cobalt doping have been synthesized by the co-precipitation method. The structure and morphology of the nanoparticles have been characterized by X-ray diffraction and transmission electron microscopy. The effects of cobalt ions on the crystallization behavior, lattice parameters and magnetic properties of Mn-Zn ferrites have been investigated. All the Co-doped ferrite nanoparticles calcined at 1150 °C possess a simple spinel structure and have an approximately spherical shape. The lattice parameters increase almost linearly with increasing Co content. The studies of magnetic properties show that the saturation magnetization Ms strongly depends on the Co content, having a maximum Ms value of 73 emu/g at a Co content of 1.0 at%, and all the Co-doped ferrites, with the average crystallite sizes ranging from 24.5 to 27.0 nm, exhibit superparamagnetism at room temperature.  相似文献   

17.
Magnetic FeCo nanoparticles with high saturation magnetization (Ms = 148 emu/g) at 15 kOe were prepared by a coprecipitation route. The value of Ms for FeCo nanoparticles depends on the ratio of Fe to Co components. The size of the nanoparticles was confirmed by transmission electron microscopy (TEM) images, and morphology of the nanoparticles was obtained by field emission scanning electron microscopy (FE-SEM) images. The crystal structure of the nanoparticles dependent on annealing was characterized by X-ray diffraction data. The magnetic properties were characterized by saturation magnetization from a hysteresis loop by VSM.  相似文献   

18.
We use the Fourier transform based Warren–Averbach (WA) analysis to separate the contributions of X-ray diffraction (XRD) profile broadening due to crystallite size and microstrain for magnetic iron oxide nanoparticles. The profile shape of the column length distribution, obtained from WA analysis, is used to analyze the shape of the magnetic iron oxide nanoparticles. From the column length distribution, the crystallite size and its distribution are estimated for these nanoparticles which are compared with size distribution obtained from dynamic light scattering measurements. The crystallite size and size distribution of crystallites obtained from WA analysis are explained based on the experimental parameters employed in preparation of these magnetic iron oxide nanoparticles. The variation of volume weighted diameter (Dv, from WA analysis) with saturation magnetization (Ms) fits well to a core shell model wherein it is known that Ms=Mbulk(1?6g/Dv) with Mbulk as bulk magnetization of iron oxide and g as magnetic shell disorder thickness.  相似文献   

19.
Superparamagnetic silica-coated magnetite (Fe3O4) nanoparticles with immobilized metal affinity ligands were prepared for protein adsorption. First, magnetite nanoparticles were synthesized by co-precipitating Fe2+ and Fe3+ in an ammonia solution. Then silica was coated on the Fe3O4 nanoparticles using a sol–gel method to obtain magnetic silica nanoparticles. The condensation product of 3-Glycidoxypropyltrimethoxysilane (GLYMO) and iminodiacetic acid (IDA) was immobilized on them and after charged with Cu2+, the magnetic silica nanoparticles with immobilized Cu2+ were applied for the adsorption of bovine serum albumin (BSA). Scanning electron micrograph showed that the magnetic silica nanoparticles with an average size of 190 nm were well dispersed without aggregation. X-ray diffraction showed the spinel structure for the magnetite particles coated with silica. Magnetic measurement revealed the magnetic silica nanoparticles were superparamagnetic and the saturation magnetization was about 15.0 emu/g. Protein adsorption results showed that the nanoparticles had high adsorption capacity for BSA (73 mg/g) and low nonspecific adsorption. The regeneration of these nanoparticles was also studied.  相似文献   

20.
The formation of γ-Fe2O3 nanoparticles embedded in a silica matrix has been studied in low-pressure premixed flames of hydrogen and oxygen. The organometallic precursors iron-pentacarbonyl (Fe(CO)5) and tetramethylsilane (Si(CH3)4) were used as starting materials for the core particles and matrix material, respectively. Fe2O3 particles with a diameter of about 3–7nm were successfully embedded in a surrounding silica matrix of about 9–13nm in diameter. The iron oxide particle kernels are superparamagnetic at room temperature.  相似文献   

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