Temperature dependence of magnetic property and photocatalytic activity of Fe3O4/hydroxyapatite nanoparticles

Fe₃O₄/hydroxyapatite (HAP) nanoparticles have been developed as a novel photocatalyst support, based on the embedment of magnetic Fe₃O₄ particles into HAP shell via homogeneous precipitation method. The resultant nanoparticles were characterized by transmission electron microscope (TEM) and X-ray diffraction (XRD). These particles were almost spherical in shape, rather monodisperse and have a unique size of about 25 nm in diameter. The effect of calcination temperature on magnetic property and photocatalytic activity of Fe₃O₄/HAP nanoparticles was investigated in detail. The obtained results showed that the Fe₃O₄/HAP nanoparticles calcined at 400 °C possessed good magnetism and photocatalytic activity in comparison with that calcined at other temperatures.     

The formation of magnetite nanoparticles on the sidewalls of multi-walled carbon nanotubes

Linear polyethyleneimine (PEI) was used as a non-covalent functionalizing agent to modify multi-walled carbon nanotubes (MWCNTs). Fe₃O₄ nanoparticles were then formed along the sidewalls of the as-modified MWCNTs through a simple solvothermal method. X-ray diffraction, Fourier transform infrared spectrometry, transmission electron microscopy, and vibrating sample magnetometry were used to characterize the MWCNT/Fe₃O₄ nanocomposites. Results indicated that Fe₃O₄ nanoparticles with diameters ranging from 50 to 200 nm were attached to the surface of the MWCNTs by electrostatic interaction. PEI was found to improve the electrical conductivity of the MWCNT/Fe₃O₄ nanocomposites. The magnetic saturation value of these magnetic nanocomposites was 61.8 emu g⁻¹. These magnetic MWCNT/Fe₃O₄ nanocomposites are expected to have wide applications in bionanoscience and technology.     

溶胶-凝胶法制备核壳SiO2/Fe3O4复合纳米粒子的研究

采用溶胶-凝胶法,以尺寸约10nm的Fe3O4纳米粒子为种子,碱催化正硅酸已酯(TEOS)水解、缩合,制备了磁性可控的核壳结构SiO2/Fe3O4复合纳米粒子.系统研究了醇水比、NH4OH及TEOS的浓度对复合纳米粒子形貌和性能的影响,并分析了SiO2/Fe3O4复合纳米粒子的生成机理.结果表明,SiO2的生长主要是SiO2初级粒子在Fe3O4表面的聚集生长,醇水比为4∶1、NH4OH浓度为0.3mol/L和TEOS浓度低于0.02mol/L时,随TEOS浓度的增大,SiO2壳层增厚,复合粒子饱和磁化强度下降,矫顽力基本不变,仍具有良好的超顺磁性.     

Facile fabrication of SiO2/Al2O3 composite microspheres with a simple electrostatic attraction strategy

SiO₂/Al₂O₃ composite microspheres with SiO₂ core/Al₂O₃ shell structure and high surface area were prepared by depositing Al₂O₃ colloid particles on the surface of monodispersed microporous silica microspheres using a simple electrostatic attraction and heterogeneous nucleation strategy, and then calcined at 600 °C for 4 h. The prepared products were characterized with differential thermal analysis and thermogravimetric analysis (DTA/TG), scanning electron microscopy (SEM), transmission electron microscopy (TEM), nitrogen adsorption and X-ray photoelectron spectroscopy (XPS). It was found that uniform alumina coating could be deposited on the surface of silica microspheres by adjusting the pH values of the reaction solution to an optimal pH value of about 6.0. The specific surface area and pore volume of the SiO₂/Al₂O₃ composite microspheres calcined at 600 °C were 653 m² g⁻¹ and 0.34 ml g⁻¹, respectively.     

Photoluminescence of Fe2O3 nanoparticles prepared by laser oxidation of Fe catalysts in carbon nanotubes

Iron oxide nanoparticles have been produced on the top surface of aligned multi-walled carbon nanotubes by CO₂ laser processing. They were characterized to be Fe₂O₃ nanoparticles by X-ray photoelectron spectroscopy, X-ray diffraction and high resolution scanning electronic microscopy. Absorption bands in the visible region were found to be redshifted compared with the absorption of Fe₂O₃ nanoparticles prepared by traditional chemical methods. Photoluminescence from these Fe₂O₃ nanoparticles shows a broad emission band in the near infrared region for both excitations at 514 and 633 nm. Particle size is considered to be responsible for the unique optical properties of the Fe₂O₃ nanoparticles.     

Microwave-hydrothermal synthesis of γ-Fe2O3 nanoparticles and their magnetic properties

Nanosized γ-Fe₂O₃ is synthesized by the microwave-hydrothermal method. Powder X-ray diffraction and transmission electron microscopic studies showed that the average particle size is 10 nm. Magnetic studies reveal that the γ-Fe₂O₃ nanoparticles are superparamagnetic at room temperature, with a superparamagnetic blocking temperature of 200 K. The magnetic characteristics of the nanoparticles indicate their strongly interacting nature.     

Structure and electrochemical performance of Fe3O4/graphene nanocomposite as anode material for lithium-ion batteries

Using hydrothermal method, Fe₃O₄/graphene nanocomposite is prepared by synthesizing Fe₃O₄ particles in graphene. The synthesized Fe₃O₄ is nano-sized sphere particles (100–200 nm) and uniformly distributed on the planes of graphene. Fe₃O₄/graphene nanocomposite as anode material for lithium ion batteries shows high reversible specific capacity of 771 mAh g⁻¹ at 50th cycle and good rate capability. The excellent electrochemical performance of the nanocomposite can be attributed to the high surface area and good electronic conductivity of graphene. Due to the high surface area, graphene can prevent Fe₃O₄ nanoparticles from aggregating and provide enough space to buffer the volume change during the Li insertion/extraction processes in Fe₃O₄ nanoparticles.     

Fabrication of superparamagnetic hydroxyapatite with highly ordered three-dimensional pores

Hydroxyapatite (HA) with highly ordered three-dimensional pores, whose size is about 300 nm, was prepared by colloidal template method. The effect of the surface modification of silica spheres on the order degree of porous structure was investigated by field emission scanning electron microscopy (FESEM). Then, superparamagnetic Fe₃O₄ nanoparticles were fabricated via redox reaction, followed by coating with silica via a sol–gel process, in which a certain amount of TEOS was used in order to control the thickness of the silica shell. X-ray diffraction (XRD), transmission electron microscopy (TEM), and magnetometry were applied to characterize the properties. Finally, Fe₃O₄ magnetic nanoparticles coated with silica were adsorbed in the mesopores of HA with highly ordered three-dimensional pores by capillarity. The influence of dispersing agent on the adsorption results has been studied. Magnetometry was applied to characterize the magnetic properties of superparamagnetic HA. The quantities of adsorbed SiO₂/Fe₃O₄ nanoparticles with core–shell have been compared by variation of saturation magnetization before and after adsorption.     

Ultrafine magnetic particles dispersed in silica: Characterization of cobalt iron citrate precursor and magnetic properties

Ultrafine magnetic particles dispersed in a silica matrix were successfully obtained by treatment of a cross-linked cobalt iron citrate precursor, synthesized by a modified Pechini route, with 0.001 M K₂Cr₂O₇ at 130 °C. The IR and NMR spectroscopic characterization of the precursor gel containing Co²⁺ and Fe³⁺ shows that the citric acid reacts with the metallic ions by coordination, the ethylene glycol by esterification and the tetraethylorthosilicate by substitution. SQUID measurements of the composite indicate superparamagnetic behavior. The blocking temperature, from the peak of the zero-field-cooled measurements, was 3 K at 1000 Oe. The magnetic diameter calculated using Langevin's equation was 4 nm.     

Preparation and characterization of porous ultrafine Fe2O3 particles

Porous ultrafine Fe₂O₃ particles were prepared by homogeneous precipitation method. Fe³⁺ and urea were chosen as starting materials and anionic surfactant as the template. It is shown that the reaction results in the precipitation of a gelatinous hydrous iron oxide/surfactant mixture, which gives ultrafine Fe₂O₃ particles after drying and calcinations. The products were characterized by XRD, TEM, TG/DTA and BET. Conventional XRD patterns show that the products are mixture of γ-Fe₂O₃ and α-Fe₂O₃ phase after being sintered at 350 °C, and γ-Fe₂O₃ transforms entirely to α-Fe₂O₃ when sintered at 650 °C. The low-angle XRD patterns indicate that the mesostructure can only exist between 350 and 400 °C. TEM results show that the Fe₂O₃ particles have diameters of about 30 nm and lengths ranging from 100 to 120 nm; in each particle, there are several vermiculate-like mesopores with diameter of about 20-25 nm. The BET surface areas in excess of 50 m²/g are obtained after calcinations at 350 °C. The BJH desorption average pore width is around 22 nm, which is in agreement with the TEM results. The results show that anionic surfactant and sintering temperature are important to obtain this special morphology.     

Synthesis and characterizations of Ni-Fe@spinel oxide core-shell nanoparticles

Core-shell Ni-Fe@ferrite nanoparticles with an average diameter of 14 nm and shell thickness of 3 nm were synthesized through a redox-transmetalation process. The alloy core and spinel oxide shell were verified by X-ray photoelectron spectroscopy, X-ray diffraction, and transmission electron microscopy. The hydrophobic oleylamine molecules on the surface were replaced by hydrophilic meso-2,3-Dimercaptosuccinic acid to make the nanoparticles to be water-soluble. X-ray diffraction study of the as-prepared core-shell nanoparticles indicates that they remained face centered cubic alloy core and spinel shell form in air. Magnetic measurements indicate that the core-shell nanoparticles exhibit superparamagnetic and exchange bias characteristics at 300 K and 5 K, respectively.     

Preparation, characterization and microwave absorption properties of polyaniline/Co0.5Zn0.5Fe2O4 nanocomposite

The polyaniline (PAni)/Co_0.5Zn_0.5Fe₂O₄ nanocomposite was prepared by an in situ polymerization in an aqueous solution. The products were characterized by Fourier transform infrared (FT-IR) spectrometer, ultraviolet-visible (UV-vis) spectrometer, X-ray diffraction (XRD) and transmission electron microscope (TEM). The average particle size of the PAni/Co_0.5Zn_0.5Fe₂O₄ was estimated to be about 70 nm by TEM. The reflection loss (dB) of the nanocomposite was measured at different microwave frequencies in X-band (8.2-12.4 GHz), U-band (12.4-18 GHz) and K-band (18-26.5 GHz) by radar cross-section (RCS) method according to the national standard GJB-2038-94. The results showed the reflection loss of the PAni/Co_0.5Zn_0.5Fe₂O₄ nanocomposite was higher than that of the PAni. The maximum reflection loss of the PAni/Co_0.5Zn_0.5Fe₂O₄ nanocomposite was about −39.9 dB at 22.4 GHz with a bandwidth of 5 GHz (full frequency width at about a half of the peak response). In conclusion, this sample is a good microwave shielding and absorbing materials at higher frequency.     

Facile preparation of carbon coated magnetic Fe3O4 particles by a combined reduction/CVD process

In this work, we report a simple method for the preparation of magnetic carbon coated Fe₃O₄ particles by a single step combined reduction of Fe₂O₃ together with a Chemical Vapor Deposition process using methane. The temperature programmed reaction monitored by Mössbauer, X-ray Diffraction and Raman analyses showed that Fe₂O₃ is directly reduced by methane at temperatures between 600 and 900 °C to produce mainly Fe₃O₄ particles coated with up to 4 wt% of amorphous carbon. These magnetic materials can be separated into two fractions by simple dispersion in water, i.e., a settled material composed of large magnetic particles and a suspended material composed of nanoparticles with an average size of 100-200 nm as revealed by Scanning Electron Microscopy and High-resolution Transmission Electron Microscopy. Different uses for these materials, e.g., adsorbents, catalyst supports, rapid coagulation systems, are proposed.     

Fabrication of surface silvered polyimide/iron oxide composite films with both superparamagnetism and electrical conductivity

Surface silvered polyimide (PI)/Fe₂O₃ composite films with both superparamagnetic and surface electrically conductive properties have been fabricated by an in situ technique. Iron (III) 2,4-pentanedionate was incorporated into a PI precursor poly(amic acid) solution and thermally decomposed to form iron oxide nanoparticles in the process of thermal imidization, preparing PI/Fe₂O₃ nanocomposite films. The establishment of a silver layer on the PI/Fe₂O₃ film surface involved the steps of chemical etching by the alkaline aqueous solution, ion exchange with silver ions and chemical reduction by glucose. The formed Fe₂O₃ particles of the nano scale endow the film with typical superparamagnetic response. By employing the etching time of only 10 min and a reduction time of no more than 15 min, the well-established silver layers have formed on the upside surface. The corresponding reflectivity and resistivity reached to the value of 76.15% and 0.7 Ω/square respectively.     

Preparation and magnetic properties of spindle porous iron nanoparticles

Spindle porous iron nanoparticles were firstly synthesized by reducing the pre-synthesized hematite (α-Fe₂O₃) spindle particles with hydrogen gas. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption/desorption isotherms and vibrating sample magnetometry (VSM). A lattice shrinkage mechanism was employed to explain the formation process of the porous structure, and the adsorbed phosphate was proposed as a protective shell in the reduction process. N₂ adsorption/desorption result showed a Brunauer-Emmett-Teller (BET) surface area of 29.7 m²/g and a continuous pore size distribution from 2 nm to 100 nm. The magnetic hysteresis loop of the synthesized iron particles showed a saturation magnetization of 84.65 emu/g and a coercivity of 442.36 Oe at room temperature.     

Magnetic properties of magnetite nanoparticles coated with mesoporous silica by sonochemical method

In this paper we present the magnetic properties of mesoporous silica-coated Fe₃O₄ nanoparticles. The coating of magnetite nanoparticles with mesoporous silica shell was performed under ultrasonic irradiation. The obtained mesoporous silica-coated magnetite nanoparticles were characterized by powder X-ray diffraction, focused ion beam-scanning electron microscopy, nitrogen adsorption-desorption isotherms and vibrating sample magnetometer. The hysteretic behavior was studied using first-order reversal curves diagrams. The X-ray diffraction result indicates that the extreme chemical and physical conditions created by acoustic cavitations have an insignificant effect on crystallographic structural characteristic of magnetite nanoparticles. Changes in the coercivity distributions of the magnetite nanoparticles were observed on the first-order reversal curves diagrams for the samples with coated particles compared with the samples containing uncoated particles of magnetite. The coated particles show an increased most probable coercivity of about 20% compared with the uncoated particles which can be associated with an increased anisotropy due to coating even if the interaction field distribution measured on the diagrams are virtually identical for coated/uncoated samples.     

Optical and magnetic properties of elliptical hematite (α-Fe2O3) nanoparticles coated with uniform continuous layers of silica of different thickness

Elliptical-type α-Fe₂O₃ nanoparticles with/without silica shell have been prepared. The core particles were coated with uniform continuous layers of silica of two different thicknesses by hydrolysis of TEOS. The obtained HCP structure elliptical α-Fe₂O₃ nanoparticles with ∼ 240 nm length and 100 nm width is polycrystalline in nature. The thicknesses of SiO₂ shell coated on α-Fe₂O₃ are about 55 and 30 nm, respectively. The optical and magnetic properties of these nanoparticles have been investigated.     

Size tuning of MAA capped CdSe and CdSe/CdS quantum dots and their stability in different pH environments

The present work reports synthesis of mercaptoacetic acid capped CdSe nanoparticles soluble in water at different temperatures and with different precursor ratios. This enabled to tune the particle size of QDs from 2.7 to 5.8 nm. The particles consist of nanocrystals; with mixed phase, hexagonal wurtzite as well as sphalerite cubic and are luminescent with quantum yield 10%. The quantum yield up to 20% has been obtained by growing a shell of CdS over the CdSe. HR-TEM images, XRD patterns and the photoluminescence excitation spectra shows epitaxial growth of CdS shell over CdSe and with average size 3.2 ± 1.2 and 4.7 ± 1.2 nm for CdSe and CdSe/CdS quantum dots respectively. FT-IR spectrum and the negative zeta potential value together confirms the attachment of mercaptoacetic acid to the QD surface, where the carboxylic acid group is facing towards solvent and provides stability due to electrostatic hindrance. Further, the QDs are checked for their stability and the luminescence in environments of different pH (4–11 pH). Both CdSe and CdSe/CdS agglomerate with total elimination of fluorescence for 4 pH medium, and no shift in the fluorescence emission peak observed for the 6–9 pH, therefore QDs can be applicable as the fluorescence tags in this specific range of pH.     

Synthesis,conductivity and dielectric characterization of salicylic acid–Fe3O4 nanocomposite

We report on the synthesis of water dispersible salicylic acid –Fe₃O₄ nanocomposites via a co-precipitation route by using Fe(III) and Fe(II) chloride salts, and salicylic acid. Crystalline phase was identified as Fe₃O₄ and the crystallite size was obtained as 13 ± 6 nm from X-ray line profile fitting. As compared to the particle size of 20 nm obtained from TEM analysis these particles show polycrystalline nature. The capping of salicylic acid around Fe₃O₄ nanoparticles was confirmed by FTIR spectroscopy, the interaction being via bridging oxygens of the carboxylate and the nanoparticle surface. ac and dc conductivity measurements performed on the nanocomposite revealed semiconductor characteristics and varying trends with temperature due to reorganization of the nanocomposite. Permittivity measurements showed increasing dielectric constant with increasing temperature as expected from semiconductors. Analysis of electrical modulus and dielectric permittivity functions suggest that ionic and polymer segmental motions are strongly coupled in the nanocomposite.