Synthesis of core-shell Fe3O4@SiO2@MS (M = Pb, Zn, and Hg) microspheres and their application as photocatalysts

In this work, we report the fabrication of core-shell Fe₃O₄@SiO₂@MS (M = Pb, Zn, and Hg) microspheres through a wet-chemical approach. The Fe₃O₄@SiO₂@MS microspheres have both ferromagnetic and photocatalytic properties. The sulfide nanoparticles on the surfaces of microspheres can degrade organic dyes under the illumination of UV light. Furthermore, the microspheres are easily separated from the solution after the photocatalytic process due to the ferromagnetic Fe₃O₄ core. The photocatalysts can be recycled for further use with slightly lower photocatalytic efficiency.     

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.     

Conducting and magnetic behaviors of polyaniline coated multi-walled carbon nanotube composites containing monodispersed magnetite nanoparticles

High conductivity and supermagnetism of polyaniline (PANI)-coated multi-walled carbon nanotube (MWCNT) composites containing monodispersed 6 nm iron oxide (Fe₃O₄) nanoparticles has been successfully synthesized by in situ chemical oxidative polymerization using anionic surfactant dodecylbenzenesulfonic acid sodium salt. Hydrophilic 6 nm spherical Fe₃O₄ nanoparticles fabricated by the thermal decomposition process were chemically modified using 11-aminoundecanoic acid tetramethylammonium salt. The modified nanoparticles were further mixed with carboxylic acid containing multi-walled carbon nanotubes (c-MWCNTs) in an aqueous solution to form one-dimensional Fe₃O₄ coated c-MWCNT template and PANI/c-MWCNT nanocomposite were then synthesized via in situ chemical oxidative polymerization in HCl solution. Structural and morphological analysis using FESEM, HRTEM and XRD showed that the fabricated Fe₃O₄ coated c-MWCNT/PANI nanocomposites are one-dimensional core (Fe₃O₄ coated c-MWCNT)–shell (PANI) structures. The electrical conductivity of 1 wt% Fe₃O₄ coated c-MWCNT/PANI nanocomposites at room temperature is 37.7 S/cm, which is decreased to 28.6 S/cm with the loading of 5 wt% Fe₃O₄ nanoparticles. The magnetic properties of Fe₃O₄ coated c-MWCNT/PANI nanocomposites exhibit supermagnetism with saturation magnetization in the range of 0.04–0.15 emu/g, which increases as the amount of Fe₃O₄ nanoparticles increases.     

Magnetic properties of hydrophilic iron oxide/polyaniline nanocomposites synthesized by in situ chemical oxidative polymerization

This work describes the preparation and characterization of polyaniline (PANI)/hydrophilic iron oxide nanocomposites synthesized from monodispersed 13 nm iron oxide (Fe₃O₄) nanoparticles and aniline monomer in HCl solution by in situ chemical oxidative polymerization. Hydrophilic 13 nm spherical Fe₃O₄ nanoparticles fabricated using the thermal decomposition process were modified using 11-aminoundecanoic acid tetramethylammonium salt. The modified Fe₃O₄ nanoparticles that served as cores were dispersed in an aqueous solution with anionic surfactant dodecylbenzenesulfonic acid sodium salt to form spherical templates and the PANI/Fe₃O₄ nanocomposites were then synthesized via in situ chemical oxidative polymerization on the surface of spherical templates. Structural and morphological analysis using X-ray diffraction and high-resolution transmission electron microscopy showed that the fabricated PANI/Fe₃O₄ nanocomposites are core (Fe₃O₄)-shell (PANI) structures. The magnetic properties of PANI/Fe₃O₄ nanocomposites exhibit supermagnetism with saturation magnetization in the range of 0.23–0.91 emu/g, depending on the amount of 13 nm Fe₃O₄ nanoparticles.     

Fe3O4/SiO2/Bi2WO6磁性复合光催化剂的制备及其光催化性能

钨酸铋(Bi₂WO₆),结构最简单的Aurivillius相化合物,是近期受到研究者关注的新型光催化材料。然而,光催化剂粉末在反应介质中难被回收,工业化应用成本较高。本文用三步方法合成了可回收的Fe₃O₄/SiO₂/Bi₂WO₆磁性复合光催化剂,通过溶剂热法合成具有磁性的Fe₃O₄,用溶胶凝胶法在Fe₃O₄表面覆盖SiO₂层,后将磁性颗粒与Bi₂WO₆纳米片相结合。光催化剂的形貌结构及性能通过XRD、SEM、PL、UV-vis进行表征测试。结果表明,直径约500 nm的Fe₃O₄微球附着在边长约500 nm的Bi₂WO₆纳米片的表面,SiO₂在两者之间起到了粘连作用。光催化剂Fe₃O₄/SiO₂/Bi₂WO₆对于罗丹明B的光降解活性较好,且有一定磁性,可以通过外加磁场将其从溶液中分离,有较大的应用潜力。     

Preparation and characterization of magnetic Fe3O4/CRGO nanocomposites for enzyme immobilization

A one-step hydrothermal procedure to form Fe₃O₄ nanospheres on chemically reduced graphene oxide (CRGO) surfaces was proposed, and these nanocomposites were used as substrates for enzyme immobilization. The as-prepared Fe₃O₄/CRGO nanocomposites were characterized using scanning electron microscopy (SEM), X-ray powder diffraction (XRD), FT-IR and vibrating sample magnetometer. Fe₃O₄ microspheres are randomly distributed on graphene sheets, and the average diameter of Fe₃O₄ microspheres is about 260 nm. Horseradish peroxidase (HRP) was used as a model enzyme to investigate the immobilization activity. The HRP loading was 23.3 mg/g supports and retained 70% of the first use after ten cycles. The catalyzed capability of immobilized HRP was investigated and the immobilized HRP exhibited broader pH stability and excellent reusability. The results show that the Fe₃O₄/CRGO nanocomposites are appropriate for the immobilization of enzyme, and could have potential use in practical.     

Fabrication by Electrophoretic Deposition of Nano-Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> and Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@SiO<Subscript>2</Subscript> 3D Structure on Carbon Fibers as Supercapacitor Materials

Core–shell nanostructured magnetic Fe₃O₄@SiO₂ with particle size ranging from 3 nm to 40 nm has been synthesized via a facile precipitation method. Tetraethyl orthosilicate was employed as surfactant to prepare core–shell structures from Fe₃O₄ nanoparticles synthesized from pomegranate peel extract using a green method. X-ray diffraction analysis, Fourier-transform infrared and ultraviolet–visible (UV–Vis) spectroscopies, transmission electron microscopy, and scanning electron microscopy with energy-dispersive spectroscopy were employed to characterize the samples. The prepared Fe₃O₄ nanoparticles were approximately 12 nm in size, and the thickness of the SiO₂ shell was?~?4 nm. Evaluation of the magnetic properties indicated lower saturation magnetization for Fe₃O₄@SiO₂ powder (~?11.26 emu/g) compared with Fe₃O₄ powder (~?13.30 emu/g), supporting successful wrapping of the Fe₃O₄ nanoparticles by SiO₂. As-prepared powders were deposited on carbon fibers (CFs) using electrophoretic deposition and their electrochemical behavior investigated. The rectangular-shaped cyclic voltagrams of Fe₃O₄@CF and Fe₃O₄@C@CF samples indicated electrochemical double-layer capacitor (EDLC) behavior. The higher specific capacitance of 477 F/g for Fe₃O₄@C@CF (at scan rate of 0.05 V/s in the potential range of ??1.13 to 0.45 V) compared with 205 F/g for Fe₃O₄@CF (at the same scan rate in the potential range of?~???1.04 to 0.24 V) makes the former a superior candidate for use in energy storage applications.     

Synthesis and characteristics of poly(3-pyrrol-1-ylpropanoic acid) (PPyAA)-Fe3O4 nanocomposite

Poly(3-pyrrol-1-ylpropanoic acid) (PPyAA)-Fe₃O₄ nanocomposite was successfully synthesized by an in situ polymerization of 1-(2-carboxyethyl) pyrrole in the presence of synthesized Fe₃O₄ nanoparticles. Evaluation of structural, morphological, electrical and magnetic properties of the nanocomposite was performed by XRD, FT-IR, TEM, TGA, magnetization and conductivity measurements, respectively. XRD analysis reveals the inorganic phase as Fe₃O₄ and TGA shows about 90 wt% loading of Fe₃O₄ in the nanocomposite. FT-IR analysis indicates a successful conjugation of Fe₃O₄ particles with polypyrrole acetic acid. Magnetization measurements show that polypyrrole acetic acid coating decreases the saturation magnetization of Fe₃O₄ significantly. This reduction has been explained by the pinning of the surface spins by the possible adsorption of non-magnetic ions during the polymerization process. The conductivity and dielectric permittivity measurements strongly depend on the thermally activated polarization mechanism and thermal transition of PPyAA in the nanocomposite structure. Large value of dielectric permittivity (?′) of the nanocomposite at lower frequency is attributed to the predominance of species like Fe²⁺ ions and grain boundary defects (interfacial polarization).     

Magnetite nanoparticles by organic-phase synthetic route for carbon nanotube growth

In the present study, monodisperse Fe₃O₄ nanoparticles with diameters ranging from 10 nm to 25 nm were synthesized using a simple organic-phase synthetic route and these monodispersed nanoparticles were then used as catalyst for seed growth of carbon nanotube. Fe₃O₄ nanoparticles were reduced to iron nanoparticles assembly by Argon mixed with 5% Hydrogen gas at 400 °C and then it was examined by atomic force microscopy (AFM), thermomechanical analysis (TMA) and powder diffraction X-ray spectroscopic techniques. XRD indicates that iron clusters are bcc in nature and AFM image shows that the iron nanoparticles assemblies are 50–65 nm in size. To control the agglomeration of iron nanoparticles, nanoporous hybrid support material of Al₂O₃ and SiO₂ was used. However, this matrix also fails to stop the agglomeration of iron nanoparticles mainly due to the inhomogeneous distribution of pore diameters. TMA analysis of iron clusters shows a temperature-dependent morphology, therefore, the CNTs growth temperature critically ascertain the nature and structure of CNTs.     

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.     

Preparation of Ni0.5Zn0.5Fe2O4/SiO2 nanocomposites and their adsorption of bovine serum albumin

The magnetic nanocomposites of (1 − x)Ni_0.5Zn_0.5Fe₂O₄/xSiO₂ (x = 0-0.2) were synthesized by the citrate-gel process and their absorption behavior of bovine serum albumin (BSA) was investigated by UV spectroscopy at room temperature. The gel precursor and resultant nanocomposites were characterized by FTIR, XRD, TEM and BET techniques. The results show that the single ferrite phase of Ni_0.5Zn_0.5Fe₂O₄ is formed at 400 °C, with high saturation magnetization and small coercivity. A porous, amorphous silica layer is located at the ferrite nanograin boundaries, with the silica content increasing from 0 to 0.20, the average grain size of Ni_0.5Zn_0.5Fe₂O₄ calcined at 400 °C reduced from about 18-8 nm. Consequently, the specific surface area of the nanocomposites ascends clearly with the increase of silica content, which is largely contributed by the increase in the thickness of the porous silica layer. The Ni_0.5Zn_0.5Fe₂O₄/SiO₂ nanocomposites demonstrate a better adsorption capability than the bare Ni_0.5Zn_0.5Fe₂O₄ nanoparticles for BSA. With the increase of the silica content from 0 to 0.05 and the specific surface area from about 49-57 m²/g, the BSA adsorption capability of the Ni_0.5Zn_0.5Fe₂O₄/SiO₂ nanocomposites calcined at 400 °C improve dramatically from 22 to 49 mg/g. However, with a further increase of the silica content from 0.05 to 0.2, the specific surface area increase from about 57-120 m²/g, the BSA adsorption for the nanocomposites remains around 49 mg/g, owing to the pores in the porous silica layer which are too small to let the BSA protein molecules in.     

Synthesis and characterization of hollow Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> submicrospheres by a simple solvothermal synthesis

Hollow single crystal Fe₃O₄ submicrospheres, which exhibit excellent magnetic properties, have been synthesized by a simple solvothermal process. These Fe₃O₄ particles have nanocrystallites with an average diameter of about 300 nm and are constructed with a hollow sphere structure that has an inside diameter of about 70 nm. The growth of the hollow Fe₃O₄ submicrospheres involves the cooperation of Ostwald ripening and oriented re-aggregation with increasing reaction time. As the oriented aggregation continues, adjacent nanocrystals fuse together along the (311) direction and the final product is formed as hollow spheres. Optional re-aggregation of the Fe₃O₄ hollow spheres may happen in the EG and N₂H₄·H₂O solution. The synthesized Fe₃O₄ particles show different magnetic properties and can be adjustable with morphological variation.     

Synthesis,characterization, electrical transport and magnetic properties of PEDOT–DBSA–Fe3O4 conducting nanocomposite

Electrical transport and magnetic properties of newly synthesized conducting polymer nanocomposites involving poly(3,4-ethylenedioxythiophene) (PEDOT) and Fe₃O₄ nanoparticles are studied. Nanocomposite samples of varying proportions of inorganic to organic components were synthesized by adding EDOT monomer stabilized in miceller solution of DBSA (dodecylbenzene sulphonic acid) to aqueous colloidal dispersion of Fe₃O₄ nanoparticles, followed by oxidative polymerization using ammonium peroxodisulphate (APS). Transmission electron microscopic (TEM) photographs show presence of distinct spherical Fe₃O₄ naonparticles having diameter range of 20–40 nm and they are incorporated within the polymer chain in the nanocomposite samples. Temperature-dependent DC conductivity analysis indicates a smooth cross-over of the charge conduction from the high temperature 3D Mott's variable range hopping (VRH) mechanism to the 2D ES (Efros and Shklovoskii)-VRH behaviour at low temperature. Temperature-dependent DC magnetization studies reveal enhancement of blocking temperature (T_B) in the nanocomposite samples compared to that of bare Fe₃O₄ nanoparticles. Core shell morphology of the nanoparticles seems to be the cause for lowering the value of saturation magnetization of the Fe₃O₄ nanoparticles. Estimated magnetic domain sizes are comparable to those of grain sizes for the nanocomposite samples having lower content of nanoparticles (P₅₀ and P₁₀₀). Temperature-dependent AC-susceptibility data also supports the superparamagnetic behaviour.     

Preparation of micro-nano hollow multiphase ceramic microspheres containing MnFe2O4 absorbent by self-reactive quenching method

Fe–Fe2O3–MnO2–sucrose–epoxy resin and O2 as reaction system and feed gas,separately,were used to prepare micro-nano hollow multiphase ceramic microspheres containing MnFe2O4absorbent by self-reactive quenching method which is integrated with flame jet,selfpropagating high-temperature synthesis(SHS),and rapidly solidification.The morphologies and phase compositions of hollow microspheres were studied by scanning electron microscope(SEM),transmission electron microscope(TEM),X-ray diffraction(XRD),and energy dispersive spectroscopy.The results show that the quenching products are regular spherical substantially with hollow structure,particle size is between few hundreds nanometers and 5 lm.Phase compositions are diphase of Fe3O4,Mn3O4,and MnFe2O4,and the spinel soft magnetic ferrite MnFe2O4 with microwave magnetic properties is in majority.Collisions with each other,burst as well as‘‘refinement’’of agglomerate powders in flame field may be the main reasons for the formation of micro-nano hollow multiphase ceramic microspheres containing MnFeOabsorbent.     

Confined growth of CuO, NiO, and Co3O4 nanocrystals in mesoporous silica (MS) spheres

The confined growth of CuO, NiO, and Co₃O₄ nanocrystals in the mesopores of the MS spheres with the help of polyelectrolyte (PE) multilayers by calcination method has been investigated. Measurements and analyses of SEM, XRD, TEM, and TGA showed that the metal oxide (CuO, NiO, or Co₃O₄) nanoparticles were almost confined in the mesopores of the MS spheres and had good crystallinity. And the resulting composite microspheres with good dispersion are still mesoporous. This approach can be used to prepare composite materials involving metal oxide nanaoparticles, which have potential application in catalytic field. And the results showed that cyclic voltammograms (CV) were valuable for the investigation of catalytic performances of CuO/MS, NiO/MS, and Co₃O₄/MS composite microspheres.     

Controlled synthesis of porous Fe3O4-decorated graphene with extraordinary electromagnetic wave absorption properties

Porous Fe₃O₄-decorated graphene (GN–Fe₃O₄) composites with different microstructures were successfully synthesized by a modified two-step method. The microstructure and morphology were confirmed by X-ray diffraction (XRD), transmission electron microscopy and scanning electron microscopy. XRD studies show that the products consist of highly crystallized Fe₃O₄ but disorderedly stacked GN sheets. Electron microscopy images reveal that Fe₃O₄ nanoparticles with different sizes and microstructures are uniformly coated on both sides of GN sheets, without large vacancies or apparent aggregation. Electromagnetic wave absorption properties of epoxy containing 30 wt.% GN–Fe₃O₄ composites were investigated at room temperature in the frequency range of 0.5–18 GHz. In particular, the porous, flower-like Fe₃O₄-decorated GN sample exhibits an enhanced dielectric loss due to the porous microstructure of Fe₃O₄. The multiple absorbing mechanisms attribute to the improved impedance matching which indicates the as-prepared porous GN–Fe₃O₄ composites could be a potential candidate for lightweight electromagnetic wave absorption materials.     

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.     

Synthesis and photocatalytic performance of Ag-loaded β-Bi2O3 microspheres under visible light irradiation

The visible-light-driven photocatalyst Ag/β-Bi₂O₃ microspheres were synthesized by a simple chemical method. First, β-Bi₂O₃ microspheres were obtained by a thermal treatment of sphere-like Bi₂O₂CO₃ precursor at 360 °C for 3 h in air and then Ag nanoparticles were in situ incorporated into β-Bi₂O₃ microspheres by impregnation method. The as-synthesized samples were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV-vis spectroscopy and photoluminescence measurements. The experimental results demonstrated that the visible light absorption of β-Bi₂O₃ photocatalyst is greatly enhanced with the incorporation of Ag nanoparticles. The SEM and TEM observations revealed that the Ag nanoparticles can be homogenously incorporated in the β-Bi₂O₃ microspheres. The photocatalytic activity of Ag/β-Bi₂O₃ sample was evaluated by the photodegradation of the Rhodamine-B under visible light irradiation as a function of Ag content. It is found that the photocatalytic efficiency of β-Bi₂O₃ can be significantly improved with the incorporation of Ag nanoparticles up to 2.0 wt% Ag. The mechanism for the enhanced photocatalytic activity is also presented.     

Recovery of gold(III) ions by a chitosancoated magnetic nano-adsorbent

The monodisperse chitosan-coated Fe₃O₄ nanoparticles with a mean diameter of 13.5 nm and 4.92 wt% chitosan were used as an anionic magnetic nano-adsorbent for the recovery of Au(III) ions from aqueous solutions. It was found that Au(III) ions could be fast and efficiently adsorbed, and the adsorption capacity increased with the decrease in pH due to the protonation of the amino groups of chitosan. The adsorption data obeyed the Langmuir equation with a maximum adsorption capacity of 59.52 mg/g (1210 mg/g based on the weight of chitosan) and a Langmuir adsorption equilibrium constant of 0.066 l/mg. From the studies on the adsorption kinetics and thermodynamics of Au(III) ions, it was found that the adsorption process obeyed the pseudo-second-order kinetic model. Furthermore, the time required to reach the equilibrium was significantly shorter than those using the micro-sized adsorbents due to the large available surface area.