Preparation of polybenzoxazine-functionalized Fe3O4 nanoparticles through in situ Diels–Alder polymerization for high performance magnetic polybenzoxazine/Fe3O4 nanocomposites

Hybrids and nanocomposites of polymer and magnetic Fe₃O₄ nanoparticles have been utilized as magnetically-responsive materials and magnetically-directed nanoparticles. In this work, we prepare polymer-functionalized Fe₃O₄ nanoparticles through in situ Diels–Alder polymerization using maleimide-functionalized Fe₃O₄ nanoparticle as a precursor. Polybenzoxazine-functionalized Fe₃O₄ nanoparticles (MNP-PBz) have been obtained and characterized with Fourier Transform Infrared, X ray photoelectron, and Raman spectroscopies. The high saturation magnetization value of 51.9 emu g⁻¹ of the MNP-PBz nanoparticles demonstrates its superparamagnetism. Moreover, MNP-FBz has been utilized as a nanofiller for preparation of cured PBz/MNP-PBz nanocomposites, which contain various MNP-PBz contents of 67, 50, 33, and 17 wt.%. The sample of PBz/MNP-PBz-67 shows a storage modulus of 8.0 GPa, a saturation magnetization value of 37.6 emu g⁻¹, and a glass transition temperature above 380 °C. As a result, the PBz/MNP-PBz nanocomposites could be classified as magnetically-responsive high performance materials.     

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.     

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.     

Preparation and characterization of bio-functionalized iron oxide nanoparticles for biomedical application

Amine modified iron oxide (Fe₃O₄) nanoparticles were synthesized by thermal decomposition method and were further used to bio-functionalize by grafting of N-hydroxysuccinimide (NHS) ester of folate and ethylenediaminetetraacetate (EDTA). Fe₃O₄ nanoparticles of ~ 22 nm were confirmed from X-ray diffraction (XRD) and transmission electron microscopy (TEM) studies. FT-IR studies indicated two bands at 1515 cm^− 1and 1646 cm^− 1, which can be attributed to carboxylic group and the amide linkage respectively, revealing the conjugation of folate with Fe₃O₄. The conjugation of the chelating agent showed strong C=O stretch and Fe-O vibrations at 1647 and 588 cm^− 1 respectively. The value of saturation magnetization for Fe₃O₄ nanoparticles was found to be 88 emu/g, which further reduced to 18 and 32% upon functionalization with EDTA and NHS ester folate, respectively. These amine modified Fe₃O₄ nanoparticles can also be functionalized with other bifunctional chelators, such as amino acids based diethylene triamine pentaacetic acid (DTPA), and thus find potential applications in radio-labeling, biosensors and cancer detection, etc.     

Synthesis and spectroscopic investigations of Mn3O4 nanoparticles

Trimanganese tetraoxide (Mn₃O₄) nanoparticles have been synthesized via hydrothermal process. Nevertheless, homogeneous nanoparticles of Mn₃O₄ with platelet lozange shape were obtained. The crystallite size ranged from 40 to 70 nm. The Mn₃O₄ product was investigated by X-ray diffraction, transmission electron microscopy (MET), and impedance spectroscopy. Electrical conductivity measurements showed that the as-synthesized Mn₃O₄ nanomaterial has a conductivity value which goes from 1.8 10⁻⁷ Ω⁻¹ cm⁻¹ at 298 K, to 23 10⁻⁵ Ω⁻¹ cm⁻¹ at 493 K. The temperature dependence of the conductivity between 298 and 493 K obeys to Arrhenius law with an activation energy of 0.48 eV.     

Arsenic (III,V) removal from aqueous solution by ultrafine α-Fe2O3 nanoparticles synthesized from solvent thermal method

Ultrafine iron oxide (α-Fe₂O₃) nanoparticles were synthesized by a solvent thermal process and used to remove arsenic ions from both lab-prepared and natural water samples. The α-Fe₂O₃ nanoparticles assumed a near-sphere shape with an average size of about 5 nm. They aggregated into a highly porous structure with a high specific surface area of ∼162 m²/g, while their surface was covered by high-affinity hydroxyl groups. The arsenic adsorption experiment results demonstrated that they were effective, especially at low equilibrium arsenic concentrations, in removing both As(III) and As(V) from lab-prepared and natural water samples. Near the neutral pH, the adsorption capacities of the α-Fe₂O₃ nanoparticles on As(III) and As(V) from lab-prepared samples were found to be no less than 95 mg/g and 47 mg/g, respectively. In the presence of most competing ions, these α-Fe₂O₃ nanoparticles maintained their arsenic adsorption capacity even at very high competing anion concentrations. Without the pre-oxidation and/or the pH adjustment, these α-Fe₂O₃ nanoparticles effectively removed both As(III) and As(V) from a contaminated natural lake water sample to meet the USEPA drinking water standard for arsenic.     

Removal of reactive red-120 and 4-(2-pyridylazo) resorcinol from aqueous samples by Fe3O4 magnetic nanoparticles using ionic liquid as modifier

The nanoparticles of Fe₃O₄ as well as the binary nanoparticles of ionic liquid and Fe₃O₄ (IL-Fe₃O₄) were synthesized for removal of reactive red 120 (RR-120) and 4-(2-pyridylazo) resorcinol (PAR) as model azo dyes from aqueous solutions. The mean size and the surface morphology of the nanoparticles were characterized by TEM, DLS, XRD, FTIR and TGA techniques. Adsorption of RR-120 and PAR was studied in a batch reactor at different experimental conditions such as nanoparticle dosage, dye concentration, pH of the solution, ionic strength, and contact time. Experimental results indicated that the IL-Fe₃O₄ nanoparticles had removed more than 98% of both dyes under the optimum operational conditions of a dosage of 60 mg, a pH of 2.5, and a contact time of 2 min when initial dyes concentrations of 10-200 mg L⁻¹ were used. The maximum adsorption capacity of IL-Fe₃O₄ was 166.67 and 49.26 mg g⁻¹ for RR-120 and PAR, respectively. The isotherm experiments revealed that the Langmuir model attained better fits to the equilibrium data than the Freundlich model. The Langmuir adsorption constants were 5.99 and 3.62 L mg⁻¹ for adsorptions of RR-120 and PAR, respectively. Both adsorption processes were endothermic and dyes could be desorbed from IL-Fe₃O₄ by using a mixed NaCl-acetone solution and adsorbent was reusable.     

Amperometric hydrogen peroxide biosensor based on cobalt ferrite-chitosan nanocomposite

A novel H₂O₂ biosensor based on horseradish peroxidase (HRP) immobilized into CoFe₂O₄-chitosan nanocomposite has been developed for the detection of hydrogen peroxide. The nanocomposite films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). HRP has been entrapped into CoFe₂O₄-chitosan nanocomposite film and the immobilized enzyme could retain its bioactivity. This biosensor exhibited a fast amperometric response to hydrogen peroxide. The linear range for H₂O₂ determination was from 3 × 10^− 2 to 8 mM, with a detection limit of 2 × 10^− 3 mM based on S/N = 3. The response time of the biosensor was 4 s. The effects of the pH and the temperature of the immobilized HRP electrode were also studied.     

Low temperature synthesis of Fe3O4 nanoparticles and its application in lithium ion batteries

Well dispersed Fe₃O₄ nanoparticles with mean size about 160 nm are synthesized by a simple chemical method at atmosphere pressure. The products are characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and Raman spectrum. Electrochemical properties of the as-synthesized Fe₃O₄ nanoparticles as anode electrodes of lithium ion batteries are studied by conventional charge/discharge tests, showing initial discharge and charge capacities of 1140 mAh g⁻¹ and 1038 mAh g⁻¹ at a current density of 0.1 mA cm⁻². The charge and discharge capacities of Fe₃O₄ electrode decrease along with the increase of cycle number, arriving at minimum values near the 70th cycle. After that, the discharge and charge capacities of Fe₃O₄ electrode begin to increase along with the increase of cycle number, arriving at 791 and 799 mAh g⁻¹ after 393 cycles. The morphology and size of the electrode after charge and discharge tests are characterized by SEM, which exhibits a large number of dispersive particles with mean size about 150 nm.     

Multicomponent oxide thin-film transistors fabricated by a double-layer inkjet printing process

In this work we report on the fabrication and characterization of multicomponent metal oxide thin-film transistors with a double-layer inkjet printing process. Both the active area and source-drain electrodes of the devices are printed with inks based on metal salt precursors to form Ga₂O₃-In₂O₃-ZnO and In₂O₃-SnO respectively. Electrical characterization has shown that the devices' performance, apart from the active area composition, can also be affected by the printing drop spacing. In general, devices printed with Ga:In:Zn 2:4:1 composition present the highest field effect mobility (~ 1.75-3 cm² V⁻¹ s⁻¹). More stable devices with improved switching, but with a compromise over field effect mobility (~ 0.5-0.9 cm² V⁻¹ s⁻¹) were obtained for the 2:4:2 composition.     

A facile route to sonochemical synthesis of magnetic iron oxide (Fe3O4) nanoparticles

A facile sonochemical approach was applied for the large scale synthesis of iron oxide magnetic nanoparticles (NPs) using inexpensive and non-toxic metal salts as reactants. The as-prepared magnetic iron oxide NPs has been characterized by XRD, TEM, EDS, and VSM. X-ray diffraction (XRD) and EDS analysis revealed that Fe₃O₄ NPs have been successfully synthesized in a single reaction by this simple method. Transmission electron microscopy (TEM) data demonstrated that the particles were narrow range in size distribution with 11 nm average particle size. Moreover, TEM measurements also show that the synthesized nanoparticles are almost spherical in shape. The magnetization curve from vibrating sample magnetometer (VSM) measurement shows that as-synthesized NPs were nearly superparamagnetic in magnetic properties with very low coercivity, and magnetization values were 80 emu/g, which is very near to the bulk value of iron oxide. The estimated value of mass susceptibility of as-synthesized nanoparticles is Xg = 5.71 × 10^− 4 m³/kg.     

Intense low threshold nonlinear absorption and nonlinear refraction in a new organic–polymer nanocomposite

Intense reverse saturable absorption is reported for the first time in solid films of a new organic–polymer nanocomposite, cast by doping Biebrich Scarlet dye in a vinyl polymer host polyvinyl alcohol for various concentrations, as studied employing the Z-scan technique at 442 nm under different peak incident intensities ranging from 9.37 × 10² to 104.18 × 10² W cm⁻². The sample also exhibited nonlinear refraction under the experimental conditions. The estimated values of the effective coefficients of nonlinear absorption β_eff(0.27 × 10⁻² to 45.5 × 10⁻² cm W⁻¹) as well as nonlinear refraction n₂ (−1.5 × 10⁻⁷ to −2.75 × 10⁻⁷ cm² W⁻¹) measured up to the highest reported ones for low power continuous wave excitation. The composite films were characterized as nanoclusters consisting of dye molecules encapsulated between larger molecules of the amorphous polymer and having a low average roughness (≈1 nm) for the surface. These results, together with the simple and flexible processing method for the dye–polymer composite, imply that BS–PVA composite films have promising optical properties as an efficient low threshold nanocomposite material for potential applications in nonlinear optical devices.     

One-pot solvothermal synthesis of sandwich-like graphene nanosheets/Fe3O4 hybrid material and its microwave electromagnetic properties

A novel sandwich-like graphene nanosheets (GNs)/Fe₃O₄ hybrid material was synthesized through a facile one-pot solvothermal method using FeCl₃ as iron source, ethylene glycol as the reducing agent and graphene nanosheets as templates. The Fe₃O₄ nanoparticles, with the average diameters of ca. 40 nm, were self-assembled on the graphene nanosheets through electrostatic attraction and formed sandwich-like nanostructure. The ferromagnetic signature emerged with the saturated magnetization of ~ 72.3 emu g^− 1, and the coercive force of ~ 196.1 Oe at 300 K. The magnetic loss was caused mainly by natural resonance which is in agreement with the Kittel equation. The novel electromagnetic hybrid material is believed to have potential applications in the microwave absorbing performances.     

A true nanocomposite: Single crystalline Au nanoparticles on single crystalline Fe3O4 nanoparticles

An Au/Fe₃O₄ nanocomposite catalyst was fabricated through a simple deposition-precipitation method. The Au/Fe₃O₄ nanocomposite is a true nanocomposite that has single crystalline Au nanoparticles supported on single crystalline Fe₃O₄ nanoparticles. Lattice fringes from both Au and Fe₃O₄ single nanoparticles were simultaneously observed by transmission electron microscope (TEM). This nanocomposite catalyst showed much high activity in low temperature CO oxidation reaction. The Au/Fe₃O₄ nanocomposite catalyst reaches 100% CO conversion at 40 °C. In comparison, Au/commercial Fe₃O₄ catalyst needs 375 °C to convert CO. This Au/Fe₃O₄ nanocomposite is an ideal sample to study synergetic effect between the catalyst and the support at nanoscale.     

Giant magnetostriction in magnetite nanoparticles

Typically the value of the magnetostrictive coefficient (λ) observed for bulk magnetic materials such as cubic ferrites is 10⁻⁶. However, giant magnetostriction (λ ≤ 10⁻³) is only observed in a few bulk intermetallic materials based on alloys of rare earth and iron such as TbFe, TbFe₂, DyFe₂ and Terefenol-D. While giant magnetostriction is known in nanostructured films, we show for the first time, this phenomenon occurs in magnetic nanoparticles. By using in-field small angle X-ray scattering (SAXS) as a tool, we demonstrate that a 4% relative change in dimension of the particle can be observed in 5.0 nm Fe₃O₄ nanoparticles at room temperature with 1 kG magnetic field. Also, we propose that the observed values are due to interaction effects and magnetoelastic coupling of particle magnetic moments and external magnetic field.     

Microwave assisted fast fabrication of Fe3O4-MWCNTs nanocomposites and their application as MRI contrast agents

Uniform Fe₃O₄ nanoparticles with diameters of 3-5 nm are successfully decorated onto the external walls of multiwall carbon nanotubes (MWCNTs) by in situ high-temperature decomposition of Fe(acac)₃ in polyol solution under the irradiation of microwave. With this method, reaction time of forming Fe₃O₄-MWCNTs nanocomposites has been significantly shortened to 15 min. The resulting Fe₃O₄-MWCNTs nanocomposites show superparamagnetic property at room temperature and can be remained as stable aqueous dispersion for 2 months. Longitudinal relaxivity (r₁) and transverse relaxivity (r₂) of the magnetic MWCNTs are 8.34 Fe mM⁻¹ S⁻¹ and 146 Fe mM⁻¹ S⁻¹ respectively. The much higher r₂ value and the obvious change in the gray scale of MR images confer the Fe₃O₄-MWCNTs nanocomposites as potential candidates for T₂-weighted MRI contrast agents.     

Solution synthesis and electrochemical capacitance performance of Mn3O4 polyhedral nanocrystals via thermolysis of a hydrogen-bonded polymer

Hausmannite Mn₃O₄ polyhedral nanocrystals have been successfully synthesized via a simple solution-based thermolysis route using a three-dimensional hydrogen-bonded polymer as precursor. The as-obtained product was characterized by means of powder X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). Possible formation mechanism of polyhedral nanocrystals was proposed based on the role of organic ligand dissociation from the polymer precursor at elevated temperature. The electrochemical capacitance performance of Mn₃O₄ electrode was investigated by cyclic voltammetry and galvanostatic charge/discharge measurements. A maximum specific capacitance of 178 F g⁻¹ was obtained for the nanocrystals in a potential range from −0.1 to 0.8 V vs. SCE in a 0.5 M sodium sulfate solution at a current density of 0.2 A g⁻¹.     

Catalytic oxidation of carbon monoxide over radiolytically prepared Pt nanoparticles supported on glass

Platinum nanoparticles have been prepared by radiolytic and chemical methods in the presence of stabilizer gelatin and SiO₂ nanoparticles. The formation of Pt nanoparticles was confirmed using UV-vis absorption spectroscopy and transmission electron microscopy (TEM). The prepared particles were coated on the inner walls of the tubular pyrex reactor and tested for their catalytic activity for oxidation of CO. It was observed that Pt nanoparticles prepared in the presence of a stabilizer (gelatin) showed a higher tendency to adhere to the inner walls of the pyrex reactor as compared to that prepared in the presence of silica nanoparticles. The catalyst was found to be active at ≥150 °C giving CO₂. Chemically reduced Pt nanoparticles stabilized on silica nanoparticles gave ∼7% CO conversion per hour. However, radiolytically prepared Pt nanoparticles stabilized by gelatin gave ∼10% conversion per hour. Catalytic activity of radiolytically prepared platinum catalyst, coated on the inner walls of the reactor, was evaluated as a function of CO concentration and reaction temperature. The rate of reaction increased with increase in reaction temperature and the activation energy for the reaction was found to be ∼108.8 kJ mol⁻¹. The rate of CO₂ formation was almost constant (∼1.5 × 10⁻⁴ mol dm⁻³ h⁻¹) at constant O₂ concentration (6.5 × 10⁻³ mol dm⁻³) with increase in CO concentration from 2 × 10⁻⁴ mol dm⁻³ to 3.25 × 10⁻³ mol dm⁻³. The data indicate that catalytic oxidation of CO takes place by Eley-Rideal mechanism.     

Synthesis,characterization and electrochemical properties of three-dimensionally ordered macroporous α-Fe2O3

Three-dimensionally ordered macroporous (3DOM) α-Fe₂O₃ electrode materials with large pore sizes and interconnected macroporous frameworks were successfully synthesized by a simply modified colloidal crystal templating strategy. The obtained samples were characterized by means of thermogravimetry, powder X-ray diffraction, nitrogen physisorption, scanning and transmission electron microscopy. The electrochemical properties of the 3DOM α-Fe₂O₃ were evaluated with cyclic voltammetry and discharge–charge experiments in an organic electrolyte containing a lithium salt. The results showed that the 3DOM α-Fe₂O₃ possessed a potential to be used as an anode material for lithium ion batteries with high initial discharge and charge capacities of 1883 and 1139 mAh g⁻¹, respectively. After 60th cycle, the reversible capacity could still be as high as 681 mAh g⁻¹ with a stable Coulombic efficiency of around 95%.     

Room temperature ferromagnetic multilayer thin film based on indium oxide and iron oxide for transparent spintronic applications

Pulsed laser deposition technique is used for fabrication of multilayer thin film of indium oxide (In₂O₃) and iron oxide (Fe₃O₄). X-ray diffraction study shows that In₂O₃ film is highly oriented along (222) direction. The optical band gap of the multilayer is observed to be 3.65 eV. The film shows n-type behavior with resistivity, carrier concentration, and mobility of 5.59 × 10⁻⁴ Ω.cm, 2.33 × 10²⁰ cm⁻³, and 48 cm ²v⁻¹ s⁻¹ respectively. Magnetic measurement shows that the film is ferromagnetic at room temperature. Hysteresis measurements at 5 K after field cooling show a shift and broadening of the hysteresis loop, which is due to exchange bias coupling.