One-pot method fabrication of superparamagnetic sulfonated polystyrene/Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>/graphene oxide micro-nano composites

In this work, using monodispersed sulfonated polystyrene (SPS) microspheres as carriers, FeCl₃·6H₂O and FeSO₄·7H₂O as precursors, NaOH as precipitant in the presence of graphene oxide (GO), SPS/Fe₃O₄/GO micro-nano composites were fabricated by a simple one-pot method employing an inverse coprecipitation in-situ compound technology. The SPS/Fe₃O₄/GO micro-nano composites were characterized by scanning electron microscopy, transmission electron microscopy, X-ray powder diffractometer, Fourier transform infrared spectroscopy, nitrogen adsorption/desorption isotherms and vibrating sample magnetometer. The results show that the SPS/Fe₃O₄/GO micro-nano composites were fabricated with SPS as core, GO and Fe₃O₄ nanoparticles as shell. The SPS/Fe₃O₄/GO micro-nano composites had larger BET specific surface area, average pore width and micropore volume than the pure SPS microspheres. Meanwhile, the SPS/Fe₃O₄/GO micro-nano composites had superparamagnetism and hydrophilic property. The saturation magnetization (M_s) of the SPS/Fe₃O₄/GO micro-nano composites was 10.86 emu/g, which was enough to ensure the convenient magnetic separation of solid and liquid phase.     

Synthesis of spinel Ni<Subscript>0.75</Subscript>Zn<Subscript>0.25</Subscript>Fe<Subscript>2</Subscript>O<Subscript>4</Subscript> and the properties of a coating obtained by gas-flame spraying

Ferrite Ni_0.75Zn_0.25Fe₂O₄ was prepared by the solid-state synthesis and thermal decomposition of the complex oxalate Ni_0.75Zn_0.25Fe₂(C₂O₄)₃ · 6H₂O. The oxalate precursor and the products obtained at different stages of the thermal decomposition were identified by differential thermal analysis and X-ray and X-ray photoelectron spectroscopy. The properties of a ferromagnetic coating deposited on a substrate by gasflame coating were studied. The magnetic properties of the Ni-Zn ferrite product and the ferromagnetic coating were also investigated.     

Preparation of stable magnetic nanofluids containing Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@PPy nanoparticles by a novel one-pot route

Stable magnetic nanofluids containing Fe₃O₄@Polypyrrole (PPy) nanoparticles (NPs) were prepared by using a facile and novel method, in which one-pot route was used. FeCl₃·6H₂O was applied as the iron source, and the oxidizing agent to produce PPy. Trisodium citrate (Na₃cit) was used as the reducing reagent to form Fe₃O₄ NPs. The as-prepared nanofluid can keep long-term stability. The Fe₃O₄@PPy NPs can still keep dispersing well after the nanofluid has been standing for 1 month and no sedimentation is found. The polymerization reaction of the pyrrole monomers took place with Fe³⁺ ions as the initiator, in which these Fe³⁺ ions remained in the solution adsorbed on the surface of the Fe₃O₄ NPs. Thus, the core-shell NPs of Fe₃O₄@PPy were obtained. The particle size of the as-prepared Fe₃O₄@PPy can be easily controlled from 7 to 30 nm by the polymerization reaction of the pyrrole monomers. The steric stabilization and weight of the NPs affect the stability of the nanofluids. The as-prepared Fe₃O₄@PPy NPs exhibit superparamagnetic behavior.     

Synthesis and properties of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanoparticles by sol-vothermal method using iron(III) acetylacetonate

Well dispersed Fe₃O₄ nanoparticles were synthesized at 180°C by sol-vothermal method, using iron (III) acetylacetonate as iron source and poly-vinilpyrrolidone (PVP) as special surfactant. The factors affecting reaction system, such as reaction temperature and time, the amount of iron source and surfactant are discussed. The synthesized Fe₃O₄ particles show excellent saturation magnetization and super-paramagnetic properties, demonstrating their potential applicability in magnetic nanodevices and bio-medicine.     

High toughening and low friction of novel bismaleimide composites with organic functionalized serpentine@Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>

A novel hybrid particles Srp@Fe₃O₄/OA, composed of phyllosilicate Serpentine (Srp), magnetic Fe₃O₄ and oleic acid (OA), has been explored via a two-step process. Then the as-prepared Srp@Fe₃O₄/OA particles were firstly mixed with bismaleimide resin (BMI) to constructe a series of Srp@Fe₃O₄/OA/BMI composites, the mechanical properties, tribological properties and thermal stability of the Srp@Fe₃O₄/OA/BMI composites are subsequently investigated. The characterization results indicate that the 0.3 wt% Srp@Fe₃O₄/OA/BMI composite shows the maximum impact strength (19.0 kJ·m^?2) and minimum friction coefficient (0.21), higher 52.7% and lower 55% than those of the neat BMI resin, respectively. The significantly enhanced toughness and tribological performance of the Srp@Fe₃O₄/OA/BMI composites are mainly due to the increase of the free volume and the uniformly distribution of Srp@Fe₃O₄/OA, as well as the good interfacial adhesion between BMI matrix and Srp@Fe₃O₄/OA particles.     

Preparation and characterization of spindle-like Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> mesoporous nanoparticles

Magnetic spindle-like Fe₃O₄ mesoporous nanoparticles with a length of 200 nm and diameter of 60 nm were successfully synthesized by reducing the spindle-like α-Fe₂O₃ NPs which were prepared by forced hydrolysis method. The obtained samples were characterized by transmission electron microscopy, powder X-ray diffraction, attenuated total reflection fourier transform infrared spectroscopy, field emission scanning electron microscopy, vibrating sample magnetometer, and nitrogen adsorption-desorption analysis techniques. The results show that α-Fe₂O₃ phase transformed into Fe₃O₄ phase after annealing in hydrogen atmosphere at 350°C. The as-prepared spindle-like Fe₃O₄ mesoporous NPs possess high Brunauer-Emmett-Teller (BET) surface area up to ca. 7.9 m² g^-1. In addition, the Fe₃O₄ NPs present higher saturation magnetization (85.2 emu g^-1) and excellent magnetic response behaviors, which have great potential applications in magnetic separation technology.     

Effect of surface modification of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanoparticles on the preparation of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>/polystyrene composite particles via miniemulsion polymerization

Fe₃O₄ nanoparticles were modified by n-octadecyltrimethoxysilane (C18TMS) and 3-trimethoxysilylpropylmethacrylate (MPS). The modified Fe₃O₄ nanoparticles were used to prepare Fe₃O₄/polystyrene composite particles by miniemulsion polymerization. The effect of surface modification of Fe₃O₄ on the preparation of Fe₃O₄/polystyrene composite particles was investigated by transmission electron microscopy, Fourier transform infrared spectrophotometer (FT-IR), contact angle, and vibrating sample magnetometer (VSM). It was found that C18TMS modified Fe₃O₄ nanoparticles with high hydrophobic property lead to the negative effect on the preparation of the Fe₃O₄/polystyrene composite particles. The obtained composite particles exhibited asymmetric phase-separated structure and wide size distribution. Furthermore, un-encapsulated Fe₃O₄ were found in composite particles solution. MPS modified Fe₃O₄ nanoparticles showed poor hydrophobic properties and resulted in the obtained Fe₃O₄/polystyrene composite particles with regular morphology and narrow size distribution because the ended C=C of MPS on the surface of Fe₃O₄ nanoparticles could copolymerize with styrene which weakened the phase separation distinctly.     

Synthesis of Heterogeneous Li<Subscript>4</Subscript>Ti<Subscript>5</Subscript>O<Subscript>12</Subscript> Nanostructured Anodes with Long-Term Cycle Stability

The 0D-1D Lithium titanate (Li₄Ti₅O₁₂) heterogeneous nanostructures were synthesized through the solvothermal reaction using lithium hydroxide monohydrate (Li(OH)·H₂O) and protonated trititanate (H₂Ti₃O₇) nanowires as the templates in an ethanol/water mixed solvent with subsequent heat treatment. A scanning electron microscope (SEM) and a high resolution transmission electron microscope (HRTEM) were used to reveal that the Li₄Ti₅O₁₂ powders had 0D-1D heterogeneous nanostructures with nanoparticles (0D) on the surface of wires (1D). The composition of the mixed solvents and the volume ratio of ethanol modulated the primary particle size of the Li₄Ti₅O₁₂ nanoparticles. The Li₄Ti₅O₁₂ heterogeneous nanostructures exhibited good capacity retention of 125 mAh/g after 500 cycles at 1C and a superior high-rate performance of 114 mAh/g at 20C.     

Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@SiO<Subscript>2</Subscript>@TiO<Subscript>2</Subscript>-OSO<Subscript>3</Subscript>H: an efficient hierarchical nanocatalyst for the organic quinazolines syntheses

A sulfonic acid functionalized titanium dioxide quasi-superparamagnetic nanocatalyst Fe₃O₄@SiO₂@TiO₂-OSO₃H with average size of 61 nm and semispherical shape with surface area about 97 m² g^?1 with saturation magnetization 17.7 emu g^?1 and the coercivity 9.84 Oe was successfully synthesized. The structure and morphology of the nanocatalyst was characterized by Fourier transform infrared spectroscopy (FT-IR), energy-dispersive X-ray spectroscopy, X-ray diffraction pattern, transmission electron microscopy, field-emission scanning electron microscopy, vibrating sample magnetometer and Brunauer–Emmett–Teller surface area analysis. The catalytic usage of the nanocatalyst was exemplified in synthesis of 2,3-dihydroquinazolin-4(1H)-one and spiroquinazolin-4(3H)-one derivatives in deep eutectic solvents (DESs) based on choline chloride and urea. We suggest that the synergistic effects in catalytic activities of titanium dioxide, organic acid and the CO₂ capture property of DES are the main reasons for the improvement of catalytic activity. The synthesized spiroquinazolinones and dihydroquinazolinones derivatives were characterized by FT-IR, ¹H and ¹³C nuclear magnetic resonance spectroscopy. The magnetic nanocatalyst exhibit high catalytic activity and can be simply separated from reaction media by an external magnet in a few seconds and could be reused for six cycles without significant loos in activity, which indicates the good immobilization of sulfonic acid on the magnetic titanium dioxide support. Furthermore, the solvent which has been used in this work can be readily isolated and reused for several times.     

Experimental and theoretical analysis of element mercury adsorption on Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>/Ag composites

A novel magnetic nano-sorbent Fe₃O₄/Ag was synthesized and applied to capture the elemental mercury from the simulated flue gas. The morphology, components and crystal phase of the sorbents were characterized by transmission electron microscope (TEM), energy dispersive spectrometry (EDS) and X-ray diffraction (XRD), respectively. The mercury removal performance of the sorbents was investigated through the fixed-bed tests. The results indicated that silver was successfully loaded on the surface of Fe₃O₄ particles, which could significantly enhance the Hg⁰ removal performance of the sorbents. Flue gas components, including CO₂, SO₂, and NO, have little impact on the Hg⁰ removal performance of Fe₃O₄/Ag sorbents, while O₂ has a slightly positive effect. The Hg⁰ removal efficiency decreased with the increasing of temperature, Hg⁰ inlet concentration and gas hourly space velocity. Only one broad mercury desorption peak at approximately 210 °C could be observed during the temperature-programmed desorption (TPD) process, which indicated that mercury species existing on the surface of Fe₃O₄/Ag sorbents might be elemental mercury instead of oxidized mercury. Furthermore, the reusability tests showed that the Fe₃O₄/Ag sorbents could be efficiently regenerated and reused. Finally, the theoretical analysis based on the DFT method showed that a weak chemisorption of Hg⁰ on Fe₃O₄ sorbents changed to a strong chemisorption when silver was loaded. The results of theoretical analysis conformed to the experiments results well.     

Infrared Signature of Novel Super-Thermite (Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>/Mg) Fluorocarbon Nanocomposite for Effective Countermeasures of Infrared Seekers

Infrared (IR) guided missiles are real threat; they caused 90% of aircraft damage. Fluorocarbon polymer nanocomposite based on super-thermites can offer superior thermal signature to countermeasure IR guided missile seekers. This study reports on the sustainable fabrication of mono-dispersed colloidal Fe₂O₃ nanoparticles with 3 nm average particle size. Fe₂O₃ nanoparticles were dispersed in acetone for subsequent integration in fluorocarbon polymer. The impact of Fe₂O₃ content on thermal signature was evaluated using (FT-MIR 2–6 μm) spectrophotometer. Nanocomposite polymer with 8 wt% Fe₂O₃ offered an increase in the average intensity of α (2–3 μm) and β (4–5 μm) bands by 50 and 85% respectively to that of reference formulation. Quantification of stimulated emitting species in the combustion flame was conducted using ICT thermodynamic code. The developed nanothermite particles extended the primary reaction zone by 183%. Full discussions about combustion zones with associated exothermic chemical reactions have been represented.     

Gd<Superscript>3+</Superscript> doped Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanoparticles with proper magnetic and supercapacitive characteristics: A novel synthesis platform and characterization

A novel electrochemical procedure was developed for the facile preparation of Gd-doped iron oxide nanoparticles (GdIO-NPs). A simple galvanostatic deposition (i=10 mA cm^-2) was done in an additive-free aqueous solution containing FeCl₂·4H₂O, Fe(NO₃)₃·9H₂O and GdCl₃·6H₂O. The XRD, FE-SEM, EDS and TEM characterizations showed that the product is composed of 15% GdIO-NPs with 10 nm in size. VSM analysis proved that the GdIO-NPs are superparamagnetic. The cyclic voltammetry and charge-discharge tests showed that the prepared GdIO-NPs are capable to deliver specific capacity as high as 190.1 F g^-1 at 0.5A g^-1 and capacity retention of 95.1% after 2000 cycling. Based on the results, it was concluded that the developed electrochemical strategy acts as an efficient procedure for the preparation of lanthanide doped MNPs with proper magnetic and supercapacitive characters.     

A Novel Coordination Polymer with Helical Chain: Synthesis and Crystal Structure of [Cu<Subscript>4</Subscript>(PMEP-Sal)<Subscript>4</Subscript>·H<Subscript>2</Subscript>O]<Subscript><Emphasis Type="Italic">n</Emphasis></Subscript>

Summary A novel coordination polymer, [Cu₄(PMEP-sal)₄·H₂O] _n (PMEP-sal = 4-(2′-hydroxyl benxoylhydrazinyl) ethylidene-5-methyl-2-phenyl-pyrazole-3-one), is synthesized. Single crystal X-ray analysis reveals the polymer contains tetranuclear building blocks in helical arrangement.     

A Resumable Fluorescent Probe BHN-Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@SiO<Subscript>2</Subscript> Hybrid Nanostructure for Fe<Superscript>3+</Superscript> and its Application in Bioimaging

A multifunctional fluorescent probe BHN-Fe₃O₄@SiO₂ nanostructure for Fe³⁺ was designed and developed. It has a good selective response to Fe³⁺ with fluorescence quenching and can be recycled using an external magnetic field. With adding EDTA (2.5?×?10^?5 M) to the consequent product Fe³⁺-BHN-Fe₃O₄@SiO₂, Fe³⁺ can be removed from the complex, and its fluorescence probing ability recovers, which means that this constituted on-off type fluorescence probe could be reversed and reused. At the same time, the probe has been successfully applied for quantitatively detecting Fe³⁺ in a linear mode with a low limit of detection 1.25?×?10^?8 M. Furthermore, the BHN-Fe₃O₄@SiO₂ nanostructure probe is successfully used to detect Fe³⁺ in living HeLa cells, which shows its great potential in bioimaging detection.     

Preparation and properties of poly(acrylic acid-co-styrene)/Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanocomposites

Poly(acrylic acid-co-styrene)/Fe₃O₄ nanocomposites were prepared using poly(acrylic acid-co-styrene) (P(AA-co-St)) and nano-Fe₃O₄ particles. The resultant materials were characterized by transmission electron microscope (TEM), Fourier transform infrared (FTIR), thermogravimetric analysis (TGA), advanced rheology expand system and superconducting quantum interference device (SQUID) magnetometer. The diameter of the magnetic particles was around 3–14 nm. The experimental results reveal that the acrylic acid segment of P(AA-co-St) can react with nano-Fe₃O₄. With increasing reaction time the storage modulus, loss modulus, complex viscosity and shear stress of the P(AA-co-St)/Fe₃O₄ ethanol suspension were increased, and the suspension changed from liquid-like behavior to gel-like behavior for the reaction between P(AA-co-St) and Fe₃O₄, as found during the rheology measurements. The thermal stability of P(AA-co-St) decreased with the addition of nano-Fe₃O₄, and the nanocomposites exhibited superparamagnetic properties above the blocking temperature.     

Chitosan- and dehydroascorbic acid-coated Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanoparticles: preparation,characterization and their potential as draw solute in forward osmosis process

Forward osmosis (FO) is a natural osmosis process that has attracted a significant attention due to its many advantages. However, the development of FO process depends on the development of proper draw solutions. In this work, chitosan (CS)-coated Fe₃O₄ nanoparticles and dehydroascorbic acid (DHAA)-coated Fe₃O₄ nanoparticles were successfully synthesized by co-precipitation method and their performance as draw solutes was investigated for application in FO systems. CS and DHAA could improve the surface hydrophilicity of the Fe₃O₄ nanoparticles. The synthesized nanoparticles were characterized by field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FTIR) and vibrating sample magnetometry (VSM) which the results presented a small size, crystalline morphology and high magnetization value for their structure as well as a good dispersion in water. Cellulose triacetate/cellulose acetate (CTA/CA)-based membranes were also prepared by immersion precipitation and used as FO membranes. The synthesized FO membranes were characterized by FESEM. The performance evaluation of synthesized nanoparticles revealed that the water flux of Fe₃O₄ nanoparticles capped with DHAA was higher than that of the chitosan-coated Fe₃O₄ nanoparticles. At the end of the process, the Fe₃O₄ nanoparticles were easily separated from the diluted draw solution by applying the magnetic field.     

Research of mica/Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> pearlescent pigment by co-precipitation

Experiments on preparation of mica/Fe₃O₄ pearlescent pigment were performed to discuss influences of several crucial parameters on final products. The samples were characterized by XRD, HRSEM, FTIR and color measurement, the content of Fe₃O₄ on the mica surface was also analyzed by XPS. It was found that the smoothness, compactness and colour deepness of the coating were influenced by different pH values and temperatures. The optimum preparation parameters of mica/Fe₃O₄ pearlescent pigment were obtained: the value of pH ≥ 9.2; the concentration of sodium hydroxide was 0.5 mol/l; the concentration ratio of Fe³⁺ to Fe²⁺ was 1.6 : 1; the velocity of magnetic stirring was 138 ≤ v ≤ 151 r/min; reaction temperature was 70–80°C; calcination temperature was 350°C and calcination time was 3 h.     

Synthesis and characterization of zeolite mazzite analogue in Na<Subscript>2</Subscript>O–Al<Subscript>2</Subscript>O<Subscript>3</Subscript>–SiO<Subscript>2</Subscript>–Piperazine–H<Subscript>2</Subscript>O

Zeolite Mazzite (MAZ) analogue was synthesized directly using piperazine as a structure directing agent. The reactive gel composition used was (5.0–7.0) piperazine:(6.0–7.0) Na₂O:Al₂O₃:20.0SiO₂:400H₂O. Using this composition, the reaction time was shortened greatly to 4 days and the crystallization time was reduced as well. The DTA data showed that piperazine, in as-synthesized zeolite omega decomposed easily. The decomposition of the piperazine occurred at 400–480°C. NH₃-TPD analysis proved that zeolite H-omega from piperazine had strong surface acidity with ammonia desorption temperature up to 590°C.     

Synthesis of polyvinyl alcohol hydrogel grafted by modified Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanoparticles: characterization and doxorubicin delivery studies

During the last two decades, serious efforts have been directed towards the synthesis and coating magnetic nanoparticles for biomedical applications. Among many different types of polymeric coating materials that have been utilized in previous studies, we have selected polyvinyl alcohol (PVA). In this study, we report a novel type of magnetite nanocomposite-based PVA hydrogel. For this purpose, first, Fe₃O₄ nanoparticles were modified through hexamethylene diisocyanate (HMDI) and then PVA was modified by bromoacetyl bromide to produce bromoacetylated PVA. The modified PVA was cross-linked through various diamines such as ethylene-diamine, propylene-diamine and hexamethylenediamine. The prepared weak tridimensional PVA hydrogels were further reacted through unreacted hydroxyl groups with Fe₃O₄, modified by HMDI to form magnetite hard tridimensional hydrogels. The swelling behavior of the prepared magnetite nanocomposites were investigated and showed a fast initial swelling followed by a mild increase until attaining equilibrium. The structural, morphological, thermal and magnetic properties of the synthesized magnetite nanocomposites were confirmed by FTIR, thermal gravimetric analysis, vibrating sample magnetometer and scanning electron microscopy. The doxorubicin anti-tumor drug was loaded on a selected synthesized magnetic hydrogel and in vitro drug release studies were done in phosphate buffer solution in 37 °C.     

Structural evolution of hierarchical porous NiO/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composites and their application for removal of dyes by adsorption

Hierarchical porous NiO/Al₂O₃ composites were successfully prepared by two-steps. First, the core-shell structured Al₂O₃ microspheres were prepared via a template-free hydrothermal route using KAl(SO₄)₂·12H₂O and Al₂(SO₄)₃·18H₂O as aluminum source. Then, the NiO/Al₂O₃ composites with micro- and nano-hierarchical structures were prepared by a hydrothermal method combining the subsequent calcination process. The obtained characterization result presented that the morphology of hierarchical Al₂O₃ microsphere tuned to irregular platelets by simply varying Ni/Al ratios. The BET analysis showed that the special surface area from 52.12m² g^?1 to 214.8m² g^?1 after two hydrothermal complex process. Effects of Ni/Al ratio, adsorbent dosage, Congo red (CR) concentration, coexisting ions, adsorption time and temperature were investigated. The obtained results indicated that NiO/Al₂O₃ composite had the high adsorption efficiency (99.6%) and great adsorption capacity (186.9mg g^?1) under the optimum conditions. The adsorption isotherm and kinetics data were found to be well fitted and in good agreement with the Langmuir isotherm model and pseudo-second order model, respectively. The hierarchical porous NiO/Al₂O₃ composites presented remarkably higher adsorption efficiency during five recycling, which showed their potential as the highly efficient adsorbent for removal of CR in wastewater.