Particle size effect on the magnetic properties of NiO nanoparticles prepared by a precipitation method

Nickel oxide (NiO) nanoparticles of nominal size range 16 nm and 25 nm were obtained by controlling the calcination temperature. These particles were prepared by the precipitation method. Structural, optical and morphological characterizations were done by X-ray powder diffraction, UV-vis diffuse reflectance spectroscopy and scanning electron microscopy. Studies of magnetic measurements (up to 60 kOe) and temperature variations from 2 K to 300 K of the NiO nanoparticles were investigated. Particles of 16 nm exhibited a weak ferromagnetic component and hysteresis loop. There is a increase in coercivity H_c and the remanence M_r at 8 K accompanied by an exchange bias H_E. H_E monotonically tends to zero as the particles size varied from 16 nm to 25 nm. The hysteresis loop and the size dependent χ are interpreted with the uncompensated surface spins, whereas the transition at 30 K is suggested to be Néel temperature T_N of the spins in the core of the 16 nm particles. In addition, the increasing temperature cannot showed an approach to saturation in the magnetization curve, it indicates the possibility of an asperomagnetism and/or spin glass behavior of the NiO nanoparticles.     

Direct transformation from goethite to magnetite nanoparticles by mechanochemical reduction

We present a novel method for synthesizing highly crystalline superparamagnetic magnetite (Fe₃O₄) nanoparticles (particle size about 15 nm) with relatively high saturation magnetization by direct transformation via ball-milling treatment from an amorphous goethite precipitate in a water system at room temperature. The obtained product was characterized by transmission electron microscopy, X-ray diffraction, and energy-dispersive X-ray spectroscopy; the particle size was measured by dynamic light scattering particle size analysis, and magnetic properties were measured by superconducting quantum interference device magnetometer. The mechanochemical effect induced by ball-milling treatment generates hydrogen gas, which contributes in reduction of part of the goethite, without addition of reducing agents, to give ferrous hydroxide. The mechanochemical effect also promotes solid-phase reaction between ferrous hydroxide and goethite to give magnetite, simultaneously crystallizing the formed magnetite nanoparticles while inhibiting particle growth with addition of neither heat nor additives such as surfactants and organic solvents. Thus, mechanochemical reduction provides an easy route for the synthesis of crystalline magnetite nanoparticles from ferric ion solution.     

Synthesis and characterization of the core–shell Au covered LSMO manganite magnetic nanoparticles

In this work we report the synthesis and characterization of the nanomagnetic perovskite Sr manganites covered with Au shells having different thickness. La_2/3Sr_1/3MnO₃ (LSMO) manganite nanoparticles were first prepared by a sol–gel procedure. The LSMO manganite nanoparticles were chemically covered with gold to produce the core–shell samples. TEM, HRTEM and atomic emission spectroscopy techniques were used to determine the morphology and structure of the LSMO@Au nanoparticles. The bare LSMO nanoparticles have a mean diameter of around 4.4 nm while LSMO@Au nanoparticles have mean diameters between 7.15 and 4.8 nm depending on the gold quantity involved in the capping process. XRD studies show that both core and shell systems have the expected crystalline structure. The formation of the core–shell structure is sustained by the shift of the plasmon resonance wavelength maximum observed in the UV–vis absorbtion spectra of the LSMO@Au samples depending on the gold concentration. The magnetization versus applied magnetic field of the bare LSMO nanoparticles and LSMO@Au samples shows no hysteresis loop indicating the superparamagnetic behavior of these systems. The analysis of the temperature dependences of FC and ZFC magnetizations shows that for all the samples the axial anisotropy energy barriers are increased due to the magnetic dipolar interactions between neighbor nanoparticles.     

Magnetic and structural properties of BaFe12−xGaxO19 nanoparticles

The structural and magnetic properties of barium hexaferrite nanoparticles (BaFe_12?xGa_xO₁₉) with x = 0.0–1.0, prepared by ball milling were investigated using XRD, TEM, and VSM. It was found that the particles and crystallites have similar mean size of ～41 nm for all investigated samples. The saturation magnetization decreased slightly and nonlinearly with increasing x, and this was attributed to different preferential site occupation of Ga at low and high concentration ranges. The coercivity decreased slightly with increasing x for low concentrations of Ga (x ≤ 0.2), and then increased with increasing Ga concentration up to x = 1.0. This behavior of the coercivity was attributed to the change in the exchange coupling, which was confirmed by the variation of SFD, remanence ratio and Curie temperature with Ga concentration in the samples.     

氨基功能化CoFe2O4-SiO2 磁性复合材料的制备及其在去除水中重金属离子的吸附性能

钴-铁氧体纳米粒子(CoFe₂O₄ NPs)通过改良的共沉淀法制备,CoFe₂O₄-SiO₂磁性复合材料通过st?ber法合成,为了吸附重金属离子CoFe₂O₄-SiO₂进行了氨基功能化。这种吸附剂的晶体结构、形貌、颗粒尺寸、化学组成和分子结构采用X射线衍射图谱(XRD)、扫描电子显微镜(SEM)以及傅里叶变换红外光谱(FTIR)进行表征。此复合材料具有优良的磁性能,由于其高的饱和磁化强度,磁铁可以将其在30秒内快速分离。同时,CoFe₂O₄ NPs的磁性能可以通过烧结温度进行调节,随烧结温度提高,磁性能增强。溶液的pH及反应时间对重金属离子吸附的影响进行了研究,此外此吸附剂对Cu (II)、Cd (II)、Mn (II) 和Zn (II)具有较高的吸附容量和去除率,这一结果使此复合材料可以潜在应用于废水中重金属离子的吸附上。     

Microemulsion synthesis and magnetic properies of BaAl<Subscript>4</Subscript>Fe<Subscript>8</Subscript>O<Subscript>19</Subscript> powders

Al-substituted M-type hexaferrite is a highly anisotropic ferromagnetic material. In the present study, we report the synthesis and the characterization of BaAl₄Fe₈O₁₉ powder from two microemulsion systems of po1yoxyethylene octylphenol ether/1, 2-propylene glycol, or ethanol/cyclohexane/water and cetrimonium bromide/1, 2-propylene glycol/cyclohexane/water. Two microemulsion systems were found to give wide stable regions. The synthesized powders were characterized with x-ray diffraction, scanning electron microscopy, and vibrating sample magnetometer. The experiment results indicated that the surfactant, co-surfactant, and oil/water ratio remarkably affected the particle size, size distribution, anisotropy and magnetic property of the powders. The powder prepared with microemulsion of po1yoxyethylene octylphenol ether/1, 2-propylene glycol/cyclohexane/water exhibited best particle character, that is, uniform thin particle morphology, large shape anisotropy, small particle size, large coercivity of 8.73 kOe, and saturation magnetization of 20.821 emu·g⁻¹.     

Influence of cooling field on the magnetic properties of Ni/NiO nanostructure

Nanoparticles of Ni/NiO structure were prepared by sol–gel route followed by the annealing in presence of controlled oxygen and argon gas mixture. When the sample was cooled down to 5 K from room temperature in a static magnetic field, a systematic shift of the magnetic hysteresis loop was observed. The shift was absent when the sample was cooled in zero field. For cooling the sample in field-cooled mode a small horizontal shift was noticed along with a moderate vertical shift of the hysteresis loop at the saturation of magnetization, which indicates the typical manifestation of exchange bias effect. The horizontal shift increases with decreasing particle size retaining almost unchanged relative vertical shift, where vertical shift is found to be uncorrelated with the horizontal shift. The exchange bias like effect in the Ni/NiO nanostructure is suggested at the Ni/NiO interface, where Ni is ferromagnetic and NiO is in the disordered magnetic state.     

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

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

Folate-conjugated Fe3O4 nanoparticles for in vivo tumor labeling

Highly biocompatible superparamagnetic Fe₃O₄ nanoparticles were synthesized by amide of folic acid (FA) ligands and the NH₂-group onto the surface of Fe₃O₄ nanoparticles. The as-synthesized folate-conjugated Fe₃O₄ nanoparticles were characterized by X-ray diffraction diffractometer, transmission electron microscope, FT-IR spectrometer, vibrating sample magnetometer, and dynamic light scattering instrument. The in vivo labeling effect of folate-conjugated Fe₃O₄ nanoparticles on the hepatoma cells was investigated in tumor-bearing rat. The results demonstrate that the as-prepared nanoparticles have cubic structure of Fe₃O₄ with a particle size of about 8 nm and hydrated diameter of 25.7 nm at a saturation magnetization of 51 A·m²/kg. These nanoparticles possess good physiological stability, low cytotoxicity on human skin fibroblasts and negligible effect on Wistar rats at the concentration as high as 3 mg/kg body mass. The folate-conjugated Fe₃O₄ nanoparticles could be effectively mediated into the human hepatoma Bel 7402 cells through the binding of folate and folic acid receptor, enhancing the signal contrast of tumor tissue and surrounding normal tissue in MRI imaging. It is in favor of the tumor cells labeling, tracing, magnetic resonance imaging (MRI) target detection and magnetic hyperthermia.     

Size effects and interactions in La0.7Ca0.3MnO3 nanoparticles

La_0.7Ca_0.3MnO₃ (LCMO) nanoparticles with average diameter of 16-73 nm were prepared by reactive milling and thermal processing methods. Interaction and size effects on the magnetic properties of the LCMO nanoparticle samples were investigated. Phenomena related to the interparticle interaction, such as an un-overlapping of the M(H_ext,T)/M_S vs. H_ext/T scaling plots and a Curie-Weiss rather than Curie law behavior of the dc susceptibility at high temperatures were analyzed. The magnetization curves of interacting nanoparticles were well described by using the mean-field approximation. The dependence of the blocking temperature T_B on the strength of the interactions, magnetic anisotropy, as well as the thermal dependence of magnetization deviates from the expected Bloch law was also estimated.     

Polyacrylamide gel synthesis and photocatalytic performance of Bi2Fe4O9 nanoparticles

In this report, a polyacrylamide gel route is introduced to synthesize Bi₂Fe₄O₉ nanoparticles. It is demonstrated that high-phase-purity Bi₂Fe₄O₉ nanoparticles can be prepared using different chelating agents. Interestingly, however, the particle size of the products is found to be dependent on the choice of chelating agent. The use of EDTA as the chelating agent allows the production of Bi₂Fe₄O₉ nanopowder with a relatively smaller particle size. The photocatalytic experiments reveal that the as-prepared Bi₂Fe₄O₉ nanoparticles possess excellent photocatalytic activity for oxidative decomposition of methyl red under ultraviolet and visible light irradiation. Magnetic hysteresis loop measurement shows that the Bi₂Fe₄O₉ nanoparticles exhibit a weak ferromagnetic behavior at room temperature.     

The effect of Au/Ag ratios on surface composition and optical properties of co-sputtered alloy nanoparticles in Au–Ag:SiO2 thin films

Gold–silver alloy nanoparticles with various Au concentrations in sputtered SiO₂ thin films were synthesized by using RF reactive magnetron co-sputtering and then heat-treated in reducing Ar + H₂ atmosphere at different temperatures. The UV–visible absorption spectra of the bimetallic systems confirmed the formation of alloy nanoparticles. The optical absorption of the Au–Ag alloy nanoparticles exhibited only one plasmon resonance absorption peak located at 450 nm between the absorption bands of pure Au and Ag nanoparticles at 400 and 520 nm, respectively, for the thin films annealed at 800 °C. The maximum absorption wavelength of the surface plasmon band showed a red shift with increasing Au content. XPS results indicated that the alloys were in metallic state, and they had a greater tendency to lose electrons as compared to their corresponding monometallic state. Moreover, the positive and negative shift of the Au(4f) core-level binding energies was observed for low and high Au concentration, respectively. Also a negative shift of the Ag(3d) binding energies was increased by increasing Au concentration. Diffusion of the particles toward the surface by increasing the temperature has also been illustrated by AFM images. Based on AFM observations, we have found that the particle size reduced from 35 to 20 nm by increasing the annealing temperature from 600 to 800 °C, while particle size increased by increasing Au concentration in films. In addition, lateral force microscopy (LFM) analysis showed that the alloy particles were uniformly distributed on the surface.     

The effect of annealing on the structure,magnetic properties and AC heating of CoFe2O4 for biomedical applications

Single and nanosized spinel CoFe₂O₄ phase has been prepared successfully by a simple combination of mechanical milling from a mixture of Fe₂O₃ and Co₃O₄ powder precursors followed by a subsequent annealing. X-ray diffraction analysis reveals that the estimated crystallite size of CoFe₂O₄ increases with increasing temperature but remains at the nanoscale, i.e. 85 nm at 900 °C. Moreover, magnetic measurements show that a great enhancement in the saturation magnetization was achieved whereas a large hysteresis loop was observed (i.e.72 emu/g at 900 °C). Evaluation and applicability of CoFe₂O₄ nanoparticles under high frequency AC magnetic field for heating in biomedical applications were examined. It was found that under fixed amplitude (516 Oe) and frequency (229 kHz), the prepared nanoparticles generate significant heat: after 5 s the temperature was around 97 °C for the as-milled powder and reached almost 178 °C for the powder annealed at 900 °C.     

Maghemite polymer nanocomposites with modulated magnetic properties

A method is presented for the production of maghemite polymer nanocomposites with modulated magnetic properties. Magnetic nanocomposites prepared using this method show regular variation in the magnetic blocking temperature from 2 K to 300 K, and variation in the saturation magnetization from 0 to 50 emu g⁻¹ (Fe₂O₃). The method is based on the in situ formation of maghemite nanoparticles in nitrogen-base polymer matrixes. The particle size can be varied regularly from 1.5 nm to 16 nm by changing the ratio of iron loading in the polymer and/or the Fe(II)/Fe(III) ratios. The particles are isolated and uniformly distributed within the matrix. The materials were characterized by electron microscopy, electron energy loss spectroscopy, Mössbauer spectroscopy, infrared spectroscopy, small angle X-ray scattering, wide angle X-ray scattering and magnetic measurements. The nanocomposites obtained are useful model material for the study of the magnetic behavior of magnetic nanoparticles, as well as for use in many industrial and biomedical applications.     

Interstitial effects of B addition on the metamagnetic transition and magnetocaloric effect in tetragonal Cu2Sb-type Mn1.95Cu0.05Sb alloys

Mn_1.95Cu_0.05SbB_x (x = 0, 0.06 and 0.1) alloys had been prepared and B interstitial effects on metamagnetic transition were studied. The metamagnetic transition temperature was reduced and thermal hysteresis was widened by higher B concentration. The saturation magnetization and the magnetic entropy change were increased by moderate amount of B addition. However, too high B composition led into the sluggish metamagnetic transition. By relating with crystallographic structure, our results further indicated that the electron density of the atoms at MnⅡ position plays critical role on influencing the metamagnetic transition in tetragonal Cu₂Sb-type Mn_1.95Cu_0.05Sb alloys.     

Solvent effects in the synthesis of MgFe2O4 nanopowders by reverse micelle processing

Nanopowders of MgFe₂O₄ have been synthesized by the novel and facile reverse microemulsion route. The effects of changing the continuous phase on the particle size and the magnetic property have been studied. The average particle size, morphology and saturation magnetization are shown to be dependent on the continuous phase. The average diameters of the particle prepared with heptane are 20.9 ± 4.3 nm. On the contrary, the product with toluene and cyclohexane is highly aggregated. The values of saturation magnetization for our samples prepared with heptane, toluene and cyclohexane are 14.5, 30 and 37 emu/g.     

Structure and magnetic properties of Cd doped copper ferrite

This report presents the synthesis of copper cadmium ferrite (Cu_1−xCd_xFe₂O_4,x = 0.3, 0.4, 0.5, 0.6 and 0.7) by citrate precursor method and its subsequent characterization by using X-ray diffraction (XRD), electron diffraction spectroscopy (EDS) and vibrating sample magnetometer (VSM) techniques. XRD results confirm the single cubic spinel phase formation with the particle size of 40 nm, which decreased up to 20 nm with increases in Cd content, while the lattice parameter increased with increase in Cd content. By using VSM technique, a significant change in the magnetic properties was observed in CuFe₂O₄ system with Cd doping. It is seen that magnetic field H_C and remnant magnetization M_R increases with increasing concentration up to x = 0.6 except for x = 0.4 and 0.7.     

Effect of heat treatment on the magnetic properties of nanocrystalline spinel Li–Ni ferrite prepared by a simple soft chemistry route

A simple soft chemistry route was developed to synthesize nanocrystalline Li–Ni ferrite (Li_0.25Ni_0.5Fe_2.25O₄). The as-prepared ferrite samples were characterized by X-ray diffractometer (XRD), transmission electron microscope (TEM) and vibrating sample magnetometer (VSM). The effects of the annealing temperature on the particle sizes and magnetic properties of the synthesized Li–Ni ferrites were investigated. The results indicated that the ferrite samples obtained by this method had the single-phase spinel structure. Particle sizes estimated from Scherrer's formula increased with the annealing temperature. The magnetic properties of the ferrite samples showed strong dependence on the annealing temperature. The coercivity initially increased and then decreased with increasing annealing temperature whereas the saturation magnetization continuously increased.     

Microstructure,tribological behavior and magnetic properties of Fe−Ni−TiO2 composite coatings synthesized via pulse frequency variation

The Fe−Ni−TiO₂ nanocomposite coatings were electrodeposited by pulse frequency variation. The results showed that the nanocomposite with a very dense coating surface and a nanocrystalline structure was produced at higher frequencies. By increasing the pulse frequency from 10 to 500 Hz, the iron and TiO₂ nanoparticles contentswere increased in expense of nickel content. XRD patterns showed that by increasing the frequency to 500 Hz, an enhancement ofBCC phase was observed and the grain size of deposits was reduced to 35 nm. The microhardness and the surface roughness were increased to 647 HV and 125 nm at 500 Hz due to the grain size reduction and higher incorporation of TiO₂ nanoparticles into the Fe−Ni matrix (5.13 wt.%). Moreover, the friction coefficient and wear rate values were decreased by increasing the pulse frequency;while the saturation magnetization and coercivity values of the composite deposits were increased.     

Magnetic Properties of the Nanocrystalline Nd-Ho-Fe-Co-B Alloy at Low Temperatures: The Influence of Time and Annealing

A study is made of the effects of various factors such as time (7 years), temperature, high magnetic field up to 580 kOe and heat treatment (HT) on the morphological structure and magnetic hysteresis properties of a high-coercive nanocrystalline (Nd_0.55Ho_0.45)_2.7(Fe_0.8Co_0.2)₁₄B_1.2 alloy with a low temperature coefficient of remanence. We find a rather weak time effect on (Nd_0.55Ho_0.45)_2.7(Fe_0.8Co_0.2)₁₄B_1.2. After 7 years, the loss in the maximum magnetic energy product (BH)_max is no more than 5%. Annealing of the sample at 250 °C for 30 min decreases the amount of amorphous phase from 7.2 to 1.7%, while the grains’ size of the 2-14-1 phase increases from 83 to 109 nm. For the HT alloy, a magnetization jump is observed at H ~500 kOe. It can be attributed to the first-order magnetization process or a spin-flip magnetic transition. Rectangularity of the hysteresis loop degrades after annealing. In case of the short-time heat treatment, losses in (BH)_max are ~10%.