Structure and magnetic properties of regenerated cellulose/Fe3O4 nanocomposite films

Cellulose nanocomposites containing high contents of Fe₃O₄ nanoparticles were successfully prepared with regenerated cellulose films as a matrix and mixture solutions of Fe²⁺/Fe³⁺ as precursors. The structure and properties of the magnetic nanocomposite films were investigated with X‐ray diffraction, scanning electron microscopy, transmission electron microscopy, thermogravimetric analysis, and vibrating sample magnetometry. Fe₃O₄ nanoparticles as prepared were irregular spheres and were homogeneously dispersed in the cellulose matrix. With an increase in the concentration of precursors from 0.2 to 1.0 mol/L, the content of Fe₃O₄ nanoparticles in the dried nanocomposites increased from 12 to 39 wt %, and the particle diameter increased from 32 to 64 nm. The cellulose nanocomposite films demonstrated superparamagnetic behavior, and their saturation magnetizations were in the range 4.2–21.2 emu/g, which were related to the increase in Fe₃O₄ nanoparticle content. With increasing nanophase content, the nanocomposite films displayed significantly anisotropic magnetic properties in the parallel and perpendicular directions. This study provided a green and facile method for the preparation of biobased nanocomposite films with high nanophase content and excellent magnetic properties. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

New Magnetic Polymer Nanocomposites on the Basis of Isotactic Polypropylene and Magnetite Nanoparticles for Adsorption of Ultrahigh Frequency Electromagnetic Waves

In this study, we report about the preparation of magnetic polymer nanocomposites on the basis of isotactic polypropylene and magnetite Fe₃O₄ nanoparticles. The structure and composition of polymer nanocomposite materials have been studied by scanning electron microscopy, atomic force microscopy, and X-ray dispersive analysis. The magnetic properties of polymer nanocomposites based on PP+Fe₃O₄have been investigated. It is found that not significant adhesion and agglomeration of nanoparticles occur, by increasing the nanoparticle content in polymer matrix up to 40%, and therefore they act as single-domain nanoparticles. The samples of nanocomposites based on PP+Fe₃O₄, with up to 40% content of Fe₃O₄, exhibit superparamagnetic properties. It was also found out that the magnetic polymer nanocomposite material based on PP+Fe₃O₄ is able to absorb ultrahigh frequency electromagnetic waves in the frequencies range from 0.1 to 30?GHz. The increase in Fe₃O₄ concentration from 5 to 40% at the 400?µm thicknesses of the films leads to an increase in absorption of electromagnetic waves of high frequency from 15 to 22.7%.     

Modification of Mg<Subscript>3</Subscript>Si<Subscript>2</Subscript>O<Subscript>5</Subscript>(OH)<Subscript>4</Subscript> nanotubes by magnetite nanoparticles

The magnetite nanoparticles and nanocomposite “Nanotube of hydrosilicate Mg—magnetite nanoparticles—Mg-ChR-NT/Fe₃O₄-NP” were obtained by coprecipitation. The composition of the synthesized samples has been established by X-ray diffraction. Using transmission electron microscopy, the presence of magnetite nanoparticles has been detected both inside the NTs and at the external surface of the NT walls. The specific surface of the NTs, nanoparticles, and composite is determined.     

Room temperature in situ chemical synthesis of Fe3O4/graphene

A simple, cost-effective, efficient, and green approach to synthesize iron oxide/graphene (Fe₃O₄/rGO) nanocomposite using in situ deposition of Fe₃O₄ nanoparticles on reduced graphene oxide (rGO) sheets is reported. In the redox reaction, the oxidation state of iron(II) is increased to iron(III) while the graphene oxide (GO) is reduced to rGO. The GO peak is not observed in the X-ray diffraction (XRD) pattern of the nanocomposite, thus providing evidence for the reduction of the GO. The XRD spectra do have peaks that can be attributed to cubic Fe₃O_4. The field emission scanning electron microscopy (FESEM) images show Fe₃O₄ nanoparticles uniformly decorating rGO sheets. At a low concentration of Fe²⁺, there is a significant increase in the intensity of the FESEM images of the resulting rGO sheets. Elemental mapping using energy dispersive X-ray (EDX) analysis shows that these areas have a significant Fe concentration, but no morphological structure could be identified in the image. When the concentration of Fe²⁺ is increased, the Fe₃O₄ nanoparticles are formed on the rGO sheets. Separation of the Fe₃O₄/rGO nanocomposite from the solution could be achieved by applying an external magnetic field, thus demonstrating the magnetic properties of the nanocomposite. The Fe₃O₄ particle size, magnetic properties, and dispersibility of the nanocomposite could be altered by adjusting the weight ratio of GO to Fe²⁺ in the starting material.     

Immobilization of serum albumin on the synthesized three layers core–shell structures of super-paramagnetic iron oxide nanoparticles

In this study, the synthesis of four layer structures coated on magnetite nanoparticles such that Fe₃O₄/SiO₂/APTES/PEG/BSA was investigated. Magnetite nanoparticles were synthesized by co-precipitating Fe²⁺ and Fe³⁺ in an ammonia solution with the average size of 25 nm. To fabricate Fe₃O₄/SiO₂ core–shells, the magnetite nanoparticles coated by silica with Stöber method. The fabricated nanoparticles were treated by 3-aminopropyl-triethoxysilane to achieve Fe₃O₄/SiO₂/APTES nanostructures. Moreover, the nanoparticles were also attached to reactive polyethylene glycol chains. Eventually, the nanoparticles activated with bovine serum albumin for bio-application. X-ray diffraction, transmission electron microscopy, Fourier transform infrared spectroscopy, UV–vis spectroscopy and vibrating sample magnetometer were used to support the characterization.     

Novel conductive magnetic nanocomposite based on poly (indole-co-thiophene) as a hemoglobin diagnostic biosensor: Synthesis,characterization and physical properties

The novel conductive nanocomposite has been successfully prepared by emulsion polymerization. First, magnetite nanoparticles were synthesized via coprecipitation reaction. Then, poly (indole-co-thiophene)@Fe₃O₄ nanocomposite was prepared via emulsion copolymerization of indole and thiophene monomers using sodium dodecyl sulfate as an emulsifier and ammonium persulfate as an oxidant in the presence of Fe₃O₄ nanoparticles. Characterization of the synthesized copolymer, Poly (In-co-T), and its magnetic nanocomposite were studied by Fourier transform infrared spectra, X-ray diffraction, scanning electron microscopy, thermal gravimetric analysis, differential scanning calorimetric, UV-vis spectrophotometer, and vibrating sample magnetometer. Also, the electrical conductivity of copolymer and nanocomposite were determined by four-probe instrument. Results showed a synergic effect in thermal stability by good interaction between polymer chain and magnetic nanoparticles. The conductivity of the nanocomposite was higher than bare copolymer, and increase of nanoparticles content caused an increment in the conductivity of the nanocomposites. The applicable properties of proposed conductive nanocomposite as a base at electrochemical biosensing have been investigated.     

Synthesis of magnetic citric‐acid‐functionalized graphene oxide and its application in the removal of methylene blue from contaminated water

A magnetic nanocomposite of citric‐acid‐functionalized graphene oxide was prepared by an easy method. First, citric acid (CA) was covalently attached to acyl‐chloride‐functionalized graphene oxide (GO). Then, Fe₃O₄ magnetic nanoparticles (MNPs) were chemically deposited onto the resulting adsorbent. CA, as a good stabilizer for MNPs, was covalently attached to the GO; thus MNPs were adsorbed much more strongly to this framework and subsequent leaching decreased and less agglomeration occurred. The attachment of CA onto GO and the formation of the hybrid were confirmed by Fourier transform infrared spectroscopy, scanning electron microscopy, X‐ray diffraction spectrometry and transmission electron microscopy. The specific saturation magnetization of the magnetic CA‐grafted GO (GO‐CA‐Fe₃O₄) was 57.8 emu g^?1 and the average size of the nanoparticles was found to be 25 nm by transmission electron microscopy. The magnetic nanocomposite was employed as an adsorbent of methylene blue from contaminated water. The adsorption tests demonstrated that it took only 30 min to attain equilibrium. The adsorption capacity in the concentration range studied was 112 mg g^?1. The GO‐CA‐Fe₃O₄ nanocomposite was easily manipulated in an external magnetic field which eases the separation and leads to the removal of dyes. Thus the prepared nanocomposite has great potential in removing organic dyes. © 2014 Society of Chemical Industry     

Microwave‐Assisted Synthesis of Magnetic Hydroxyapatite for Removal of Heavy Metals from Groundwater

A simple, fast, and economic methodology to fabricate a highly efficient superparamagnetic Fe₃O₄/hydroxyapatite nanocomposite (MHAP) was successfully developed. Hydroxyapatite was functionalized with magnetite nanoparticles through coprecipitation‐assisted microwave processes to improve the magnetic properties. The synthesized magnetic hybrid adsorbent matrix was investigated by different methods. Transmission electron microscopy demonstrated a good impregnation of Fe₃O₄ on the hydroxyapatite matrix with uniform morphology. Magnetic hysteresis measurement revealed that MHAP nanocomposites exhibit excellent strong, soft‐magnetic properties. The synergistic effect was an evidence for iron and manganese ion removal, enlightening their potentialities in treatment of polluted ground water.     

Characterization of stabilized porous magnetite core–shell nanogel composites based on crosslinked acrylamide/sodium acrylate copolymers

Stabilized and dispersed superparamagnetic porous nanogels based on sodium acrylate (AA‐Na) and acrylamide (AM) in a surfactant‐free aqueous system were synthesized via solution polymerization at room temperature. The formation of magnetite nanoparticles was confirmed and their properties characterized using Fourier transform infrared spectroscopy. Extensive characterization of the magnetic polymer particles using transmission electron microscopy (TEM), dynamic light scattering and zeta potential measurements revealed that Fe₃O₄ nanoparticles were incorporated into the shells of poly(AM/AA‐Na). The average particle size was 5–8 nm as determined from TEM. AM/AA‐Na nanoparticles with a diameter of about 11 nm were effectively assembled onto the negatively charged surface of the as‐synthesized Fe₃O₄ nanoparticles via electrostatic interaction. Crosslinked magnetite nanocomposites were prepared by in situ development of surface‐modified magnetite nanoparticles in an AM/AA‐Na hydrogel. Scanning electron microscopy was used to study the surface morphology of the prepared composites. The morphology, phase composition and crystallinity of the prepared nanocomposites were characterized. Atomic force microscopy and argon adsorption–desorption measurements of Fe₃O₄.AM/AA indicated that the architecture of the polymer network can be a hollow porous sphere or a solid phase, depending on the AA‐Na content. © 2013 Society of Chemical Industry     

Phase Transformation of Iron Oxide Nanoparticles by Varying the Molar Ratio of Fe2+:Fe3+

Co‐precipitation from a solution of ferrous/ferric mixed salt with the ratio of Fe²⁺:Fe³⁺ = 1:2 in air atmosphere is not a reliable method to synthesize magnetite (Fe₃O₄) nanoparticles because of the fact that Fe²⁺ oxidizes to Fe³⁺ and the molar ratio of Fe²⁺:Fe³⁺ changes. Therefore, the phase composition changes from magnetite to maghemite (γ‐Fe₂O₃). The influence of the initial molar ratio of Fe²⁺:Fe³⁺ on the phase composition of nanoparticles, their crystallinity and magnetic properties was studied. Experimental data from XRD, FTIR, SEM, and VSM reveal that the appropriate method to synthesize magnetite nanoparticles is reverse precipitation from only ferrous salt. It is found that by decreasing the synthesis temperature and by increasing the concentration of alkaline solution and the ratio of Fe²⁺:Fe³⁺ the crystallinity and the specific saturation magnetization (σ_s) are increased.     

Synthesis and characterization of magnetite (Fe3O4)—Polyvinyl alcohol‐based nanocomposites and study of superparamagnetism

The aim of this investigation was to design iron oxide containing nanocomposites which could display superparamagnetic behavior and thus find application in biomedical and allied fields. To achieve the proposed objectives methyl methacrylate was polymerized by a redox system comprising of metabisulphite and persulphate in the immediate presence of a crosslinker, N,N′‐methylene bis acrylamide and a preformed polymer, i.e., polyvinyl alcohol. Into the prepared polymer matrix nanosized magnetite (Fe₃O₄) particles were evenly dispersed by in situ precipitation of Fe²⁺/Fe³⁺ ions. The nanocomposite materials were characterized by techniques like FTIR, SEM, TEM, XRD, and DSC. The magnetic behavior of nanocomposites and bulk magnetite particles was studied under varying applied magnetic fields and their superparamagnetic property was examined. The iron‐oxide polymer nanocomposites were also studied for microhardness. POLYM. COMPOS., 2010. © 2009 Society of Plastics Engineers     

Gold deposition on Fe3O4/(co)Poly(N‐octadecyl methacrylate) hybrid particles to obtain nanocomposites With ternary intrinsic features

Here, nanocomposite particles with three domains including magnetite nanoparticles, poly(N‐octadecyl methacrylate) (PODMA) or poly(N‐octadecyl methacrylate‐co‐1‐vinylimidazole) (P(ODMA‐co‐VIMZ)), and gold nanoparticles were prepared. Fe₃O₄ nanoparticles with narrow particle size distribution were prepared through a synthetic route in an organic phase in order to achieve good control of the size and size distribution and prevent their aggregation during their preparation. These magnetite nanoparticles, ～ 5 nm in size, were then encapsulated and well‐dispersed in PODMA and P(ODMA‐co‐VIMZ) matrices via a miniemulsion polymerization process to obtain the corresponding nanocomposite particles. The results revealed that Fe₃O₄ nanoparticles were encapsulated and did not migrate towards the monomer/water interface during polymerization. The resulting latex was used as a precursor for the adsorption of Au³⁺ ions on the surface of the polymeric particles and subsequent reduction to produce Fe₃O₄/P(ODMA‐co‐VIMZ)/Au nanocomposite particles. The morphology of the particles from each step was fully characterized by TEM and AFM, and the results of DLS analysis showed their size and size distribution. Measurement of magnetic properties illustrated the superparamagnetic characteristic of the products and it was observed that the encapsulation process and deposition of gold had no effect on the magnetic properties of the resulting particles. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Removal of heavy metal ions from aqueous solutions by radiation‐induced chitosan/(acrylamidoglycolic acid‐co‐acrylic acid) magnetic nanopolymer

An effective method was developed to isolate toxic heavy metal ions from the aqueous solution by the magnetic nanopolymers. The magnetic sorbent was prepared with radiation‐induced crosslinking polymerization of chitosan (CS), 2‐acrylamido‐glycolic acid (AMGA), and acrylic acid (AAc), which stabilized by magnetite (Fe₃O₄) as nanoparticles. The formation of magnetic nanoparticles (MNPs) into the hydrogel networks was confirmed by Fourier transform infrared spectroscopy, X‐ray diffraction, transmission electron microscopy, and Scanning electron microscopy, which revealed the formation of MNPs throughout the hydrogel networks. The swelling behavior of the hydrogels and magnetic ones was evaluated at different pH values. The adsorption activity for heavy metals such as Cu²⁺ and Co²⁺ by nonmagnetic and magnetic hydrogels, Fe₃O₄/CS/(AMGA‐co‐AAc), in terms of adsorption amount was studied. It was revealed that hydrogel networks with magnetic properties can effectively be used in the removal of heavy metal ions pollutants and provide advantageous over conventional ones. POLYM. ENG. SCI., 55:1441–1449, 2015. © 2015 Society of Plastics Engineers     

Enhanced cycling performance of Fe3O4-graphene nanocomposite as an anode material for lithium-ion batteries

Fe₃O₄-graphene nanocomposite was prepared by a gas/liquid interface reaction. The structure and morphology of the Fe₃O₄-graphene nanocomposite were characterized by X-ray diffraction, scanning electron microscopy and high-resolution transmission electron microscopy. The electrochemical performances were evaluated in coin-type cells. Electrochemical tests show that the Fe₃O₄-22.7 wt.% graphene nanocomposite exhibits much higher capacity retention with a large reversible specific capacity of 1048 mAh g⁻¹ (99% of the initial reversible specific capacity) at the 90th cycle in comparison with that of the bare Fe₃O₄ nanoparticles (only 226 mAh g⁻¹ at the 34th cycle). The enhanced cycling performance can be attributed to the facts that the graphene sheets distributed between the Fe₃O₄ nanoparticles can prevent the aggregation of the Fe₃O₄ nanoparticles, and the Fe₃O₄-graphene nanocomposite can provide buffering spaces against the volume changes of Fe₃O₄ nanoparticles during electrochemical cycling.     

Preparation and structural properties of Fe3O4–polyimide hybrid nanocomposites

Polyimide films in which magnetic Fe₃O₄ nanoparticles are uniformly distributed are prepared. Before the preparation of the Fe₃O₄–polyimide composites, pure magnetite nanoparticles (Fe₃O₄) have been synthesized in water by co-precipitation (from ferric chlorides). Its surface was firstly modified with the 3-aminopropyl triethoxysilane. The prepared polyimide–Fe₃O₄ nanocomposite films were characterized for their structure, morphology, and thermal behavior employing Fourier transform infrared spectroscopy, scanning electron micrograph, X-ray diffraction, and thermal analysis (DTA/TGA/DSC) techniques.     

Achieving ultra-high electromagnetic wave absorption by anchoring Co0.33Ni0.33Mn0.33Fe2O4 nanoparticles on graphene sheets using microwave-assisted polyol method

The Co_0.33Ni_0.33Mn_0.33Fe₂O₄/graphene nanocomposite for electromagnetic wave absorption was successfully synthesized from metal chlorides solutions and graphite powder by a simple and rapid microwave-assisted polyol method via anchoring the Co_0.33Ni_0.33Mn_0.33Fe₂O₄ nanoparticles on the layered graphene sheets. The Fe³⁺, Co²⁺, Ni²⁺ and Mn²⁺ ions in the solutions were attracted by graphene oxide obtained from graphite and converted to the precursors Fe(OH)₃, Co(OH)₂, Ni(OH)₂, and Mn(OH)₂ under slightly alkaline conditions. After the transformations of the precursors to Co-Ni-Mn ferrites and conversion of graphene oxide to graphene under microwave irradiation at 170?°C in just 25?min, the Co_0.33Ni_0.33Mn_0.33Fe₂O₄/graphene nanocomposite was prepared. The composition and structure of the nanocomposite were characterized by X-ray diffraction (XRD), inductive coupled plasma emission spectroscopy (ICP), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy (RS), transmission electron microscopy (TEM), etc. It was found that with the filling ratio of only 20?wt% and the thickness of 2.3?mm, the nanocomposite showed an ultra-wide effective absorption bandwidth (less than ?10?dB) of 8.48?GHz (from 9.52 to 18.00?GHz) with the minimum reflection loss of ??24.29?dB. Compared to pure graphene sheets, Co_0.33Ni_0.33Mn_0.33Fe₂O₄ nanoparticles and the counterparts reported in literature, the nanocomposite exhibited much better electromagnetic wave absorption, mainly attributed to strong wave attenuation, as a result of synergistic effects of dielectric loss, conductive loss and magnetic loss, and to good impedance matching. In view of its thin thickness, light weight and outstanding electromagnetic wave absorption property, the nanocomposite could be used as a very promising electromagnetic wave absorber.     

Cr(III)‐containing Fe3O4/mercaptopropanoic acid‐poly(2‐hydroxyethyl acrylate) nanocomposite: Highly active magnetic catalyst for direct hydroxylation of benzene

In this study, polymer‐grafted magnetic nanoparticles containing chromium(III) ions incorporated onto Fe₃O₄/mercaptopropanoic acid‐poly(2‐hydroxyethyl acrylate) was prepared via a simple and in situ method. The obtained magnetic nanocomposite exhibited high catalytic activity and excellent selectivity in direct hydroxylation of benzene in the presence of hydrogen peroxide under solvent‐free condition. The magnetic catalyst could be also separated by an external magnet and reused seven times without any significant loss of activity/selectivity. Due to the Lewis acidity of the Fe³⁺ groups in the structure of magnetic nanoparticles, the high efficiency of this catalyst is possibly due to the synergetic effect of Cr³⁺ and Fe³⁺ groups in the structure of magnetic nanocomposite. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40383.     

Influence of magnetic casting on the permeability and anti-fouling properties of a novel iron oxide/alumina/polysulfone mixed matrix membrane

Novel mixed matrix membranes (MMMs) were fabricated using Fe₃O₄, and Al₂O₃ nanoparticles (NPs) were added to the polysulfone (PSf) and N-methylpyrrolidone (NMP) solution. The nanocomposite membranes were fabricated using the NIPS (non-solvent induced phase separation) method. In order to create preferential permeation pathways for water across the MMMs, membrane formation is accomplished with an external magnetic field. Using magnetic casting cause the targeted placement of NPs in the best location and orientation. The performance of the prepared membranes was examined in terms of pure water flux and fouling parameters. Magnetic casting considerably increased pure water flux and decreased the total resistance of the optimum mixed matrix membrane, which contains 0.2% wt. of Fe₃O₄ NPs to 1175 L/m²h and 13.4 * 10¹¹ (m⁻¹), respectively. This is explained by the ordering of magnetic nanoparticles on the membrane sub-layer cast under the magnetic field of 500 mT, which changed the sub-layer structure. Less rough membrane surface of the mixed matrix membranes offered preferable anti-fouling properties against fouling by BSA proteins. The characterization of fabricated membranes was carried out using field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), energy dispersive X-ray (EDX), and water contact angle measurement methods.     

Magnetite-based glass-ceramics prepared by controlled crystallization of borosilicate glasses: Effect of nucleating agents on magnetic properties and relaxation

The specific magnetic structure and magnetic relaxation phenomena in magnetite nanoentities grown in a glassy matrix by controlled crystallization of Fe-containing borosilicate and boroaluminosilicate glasses in the presence of two types of nucleating agents, Cr₂O₃ and P₂O₅, were investigated. The structure, morphology and magnetic properties are strongly influenced by the nucleating agents. Cr₂O₃ generates magnetite-based glass ceramics with magnetite configurations showing an upward relaxation of magnetization at low and high temperatures but downward at intermediate temperatures. The magnetite grown with P₂O₅ displays only downward relaxation but with different signs of the temperature derivative of the relaxation rate S in different temperature ranges. The observed effects are discussed with respect to the following factors: i) the existence of a multimodal size distribution of the magnetite (nano)particles as revealed by high resolution electron microscopy; ii) the degree of occupation of different sublattices of the magnetite structure with Fe³⁺ and Fe²⁺ ions; and iii) the interplay between the relaxation mechanisms in different temperature ranges.     

Electrospun polyacrylonitrile nanocomposite fibers reinforced with Fe3O4 nanoparticles: Fabrication and property analysis

The manufacturing of pure polyacrylonitrile (PAN) fibers and magnetic PAN/Fe₃O₄ nanocomposite fibers is explored by an electrospinning process. A uniform, bead-free fiber production process is developed by optimizing electrospinning conditions: polymer concentration, applied electric voltage, feedrate, and distance between needle tip to collector. The experiments demonstrate that slight changes in operating parameters may result in significant variations in the fiber morphology. The fiber formation mechanism for both pure PAN and the Fe₃O₄ nanoparticles suspended in PAN solutions is explained from the rheologial behavior of the solution. The nanocomposite fibers were characterized by scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectrophotometer, and X-ray diffraction (XRD). FT-IR and XRD results indicate that the introduction of Fe₃O₄ nanoparticles into the polymer matrix has a significant effect on the crystallinity of PAN and a strong interaction between PAN and Fe₃O₄ nanoparticles. The magnetic properties of the nanoparticles in the polymer nanocomposite fibers are different from those of the dried as-received nanoparticles.