Study on Fe3O4/polyaniline electromagnetic composite hollow spheres prepared against sulfonated polystyrene colloid template

Fe₃O₄/polyaniline (PANI) composite hollow spheres were prepared by using sulfonated polystyrene (SPS) microspheres as templates. The sulfonic acid groups were applied to induce absorbing Fe₃O₄ nanoparticle, and subsequently, conductive PANI was grown. Finally, the polystyrene cores were selectively dissolved to yield composite hollow microspheres with electromagnetic properties. The analysis results indicated that the adsorption of Fe₃O₄ on template core by electrostatic interaction resulted in magnetic composite microspheres. The conductivity of composite hollow spheres was remarkably increased after polyvinylpyrrolidone modification which favored the growth of PANI on SPS/Fe₃O₄ and enhanced the integrity of hollow microspheres. The saturated magnetization of the composite hollow microspheres was tuned from 2.7 to 9.1 emu/g, and the conductivity was in the range from 10^?2 to 10⁰?S/cm.     

Synthesis of Highly Dispersed Fe3O4 Submicrometer Spheres in a One‐Pot Anion‐induced Solvothermal System

A facile, anion‐induced, one‐pot solvothermal method was successfully developed to prepare two kinds of highly dispersed magnetic Fe₃O₄ submicrometer spheres at 200°C in 12 h. The diameters of the as‐prepared Fe₃O₄ submicrometer spheres are ~500 and ~200 nm, respectively. With the guidance of OAc ⁻ ions, the size and morphology of the Fe₃O₄ spheres could be well controlled. The saturation magnetization of the Fe₃O₄ spheres was measured to be 84 and 74 emu/g, respectively. The assembly of tiny precursor nuclei into the Fe₃O₄ spheres relies on Ostwald ripening. The synthesized Fe₃O₄ submicrometer spheres show good magnetic response, good water solubility, and uniform size.     

Magnetic and Thermal Properties of Novel Poly(ether-amide)/Fe3O4 Nanocomposite Containing Phosphine Oxide Group

New poly(ether-amide) nanocomposite containing phosphine oxide was prepared via solution polymerization process from synthesized poly(ether-amide) and Fe₃O₄ nanoparticles in a solution of N,N-dimethylformamide. Uniform monodisperse Fe₃O₄ nanoparticles were synthesized at room temperature via a facile sonochemical reaction. Poly(ether-amide) (PEA) as the polymer matrix was synthesized from reaction of 1,4-(4-carboxy phenoxy)butane (1) and bis(3-amino phenyl)phenyl phosphine oxide (2) via a direct polycondensation reaction. Nanoparticle and nanocomposite were characterized using X-ray diffraction, scanning electron microscopy, transmission electron microscopy and Fourier transform infrared. The effect of the presence of Fe₃O₄ nanoparticles on the thermal properties of PEA was studied using thermogravimetric analysis in nitrogen atmospheres. The magnetic properties of the sample were also investigated using an alternating gradient force magnetometer. We found that the Fe₃O₄ nanoparticles exhibit a ferromagnetic behaviour with a saturation magnetization of 59 emu/g and a coercivity of 104 Oe at room temperature. The coercivity of PEA/Fe₃O₄ nanocomposites is found to be 126 Oe, higher than 104 Oe which is obtained for Fe₃O₄.     

Thermal Plasma Synthesis of Superparamagnetic Iron Oxide Nanoparticles

Superparamagnetic iron oxide nanoparticles were synthesized by injecting ferrocene vapor and oxygen into an argon/helium DC thermal plasma. Size distributions of particles in the reactor exhaust were measured online using an aerosol extraction probe interfaced to a scanning mobility particle sizer, and particles were collected on transmission electron microscopy (TEM) grids and glass fiber filters for off-line characterization. The morphology, chemical and phase composition of the nanoparticles were characterized using TEM and X-ray diffraction, and the magnetic properties of the particles were analyzed with a vibrating sample magnetometer and a magnetic property measurement system. Aerosol at the reactor exhaust consisted of both single nanocrystals and small agglomerates, with a modal mobility diameter of 8?C9?nm. Powder synthesized with optimum oxygen flow rate consisted primarily of magnetite (Fe₃O₄), and had a room-temperature saturation magnetization of 40.15 emu/g, with a coercivity and remanence of 26 Oe and 1.5 emu/g, respectively.     

Fe3O4八面体微晶的水热法制备与表征

在乙二醇与水( ＝5∶8)的混合溶剂中, 通过K₄[Fe(CN)₆]与NaOH在200 ℃水热反应12 h, 制备了Fe₃O₄的八面体. 采用X射线衍射仪、扫描电镜和透射电子显微镜对产物进行表征, 并在室温下测试了它的磁学性能, 结果表明, Fe₃O₄八面体为单晶面心立方相结构, 尺寸约为0.7～6.3 μm. 它的矫顽力(H_c)为77.5 Oe, 饱和磁化强度(M_s)为98.53 emu/g, 剩余磁化强度(M_r)为6.27 emu/g. 研究了乙二醇, NaOH的浓度, 反应温度和时间对产物形貌的影响, 结果表明乙二醇在Fe₃O₄八面体的形成过程中起着关键作用, 并提出了可能的生长机理.     

Constructing magnetic polyaniline/metal hybrid nanostructures using polyaniline/Fe3O4 composite hollow spheres as supports

Polyaniline (PANI)/Fe₃O₄ composite hollow spheres have been successfully synthesized in one step using sulfonated polystyrene (PS) spheres as templates. The magnetic PANI hollow spheres were used as supports for noble metal nanoparticles (NPs) such as Au and Pd. The morphology, composition and magnetic properties of the resulting products were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, inductively coupled plasma (ICP) atomic spectra and vibrating sample magnetometer. The catalytic activity of magnetic PANI/Au composite shells on the oxidation of dopamine was investigated by cyclic voltammetry. The obtained results provide our product with a practical application for the detection of dopamine. On the other hand, the catalytic activity of magnetic PANI/Pd composite shells on the reduction of 4-nitroaniline was investigated by spectroscopic methods and compared with Pd/C catalyst which was already widely used in industrial production.     

Luminescence functionalization of magnetite/multiwalled carbon nanotubes by YVO4:Eu3+ phosphors

Multifunctional nanocomposites with magnetic and luminescent properties were synthesized by a combination process of hydrothermal and sol–gel techniques. In this process, multiwalled carbon nanotubes (MWNTs) were decorated with Fe₃O₄ beads, forming Fe₃O₄/MWNTs nanoparticles. Then, the surface of Fe₃O₄/MWNTs samples was functionalized by the deposition of YVO₄:Eu³⁺ phosphors. X-ray diffraction, field emission scanning electron microscopy, energy disperse X-ray spectroscopy, transmission electron microscopy, and photoluminescence spectra were used to characterize the samples. The results reveal that the nanocomposites exhibit high magnetization (38 emu/g) and show the characteristic emission of Eu³⁺ (⁵D₀ → ⁷F_1–4). This functionalized nanocomposite is expected to find potential applications in biomedical areas.     

Synthesis and properties of magnetite Fe3O4 via a simple hydrothermal route

Magnetic Fe₃O₄ crystals were synthesized by a simple hydrothermal method using K₄Fe(CN)₆ as single precursor. The chemical compositions and morphologies of the as-prepared samples were characterized in detail by X-ray diffraction (XRD), X-ray photoelectron spectra (XPS) and scanning electron microscopy (SEM). The experimental results show that the magnetic Fe₃O₄ particles are facilely prepared by the hydrothermal reaction of K₄Fe(CN)₆ and NaOH at 200 °C. Regular octahedral Fe₃O₄ crystals are obtained when Na₂S₂O₃ is added to the reaction system. The possible mechanism was discussed to elucidate the formation of the magnetic Fe₃O₄ crystals. Besides, the magnetic investigations show that the values of saturation magnetization and coercivity of octahedral Fe₃O₄ are about 87 emu/g and 184 Oe, respectively. Octahedral Fe₃O₄ also exhibits relatively good catalytic performance in the oxidation of styrene.     

Structural,morphological and magnetic properties of nano-crystalline zinc substituted cobalt ferrite system

Nano-crystalline zinc-substituted cobalt ferrite powders, Co_1−xZn_xFe₂O₄ (x = 0, 0.25, 0.5, 0.75 and 1), have been synthesized by the combustion route. The structural, morphological and magnetic properties of the products were determined and characterized in detail by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and vibrating sample magnetometer (VSM). X-ray analysis showed that the samples were cubic spinel. The increase in zinc concentration resulted in an increase in the lattice constant, unit cell volume, X-ray density, ionic radii, the distance between the magnetic ions and bond lengths on tetrahedral sites and octahedral sites of cubic spinel structure. Opposite behavior was observed for the average crystallite size of the as synthesized solids. The variation of saturation magnetization (M_s) value of the samples was studied. The maximum saturation magnetization value of the Co_o.25Zn_0.75Fe₂O₄ sample reached 76.87 emu/g. The high saturation magnetization of these samples suggests that this method is suitable for preparing high-quality nano-crystalline magnetic ferrites for practical applications.     

Magnetic Silica‐Coated Sub‐Microspheres with Immobilized Metal Ions for the Selective Removal of Bovine Hemoglobin from Bovine Blood

Magnetic silica‐coated magnetite (Fe₃O₄) sub‐microspheres with immobilized metal‐affinity ligands are prepared for protein adsorption. First, magnetite sub‐microspheres were synthesized by a hydrothermal method. Then silica was coated on the surface of Fe₃O₄ particles using a sol–gel method to obtain magnetic silica sub‐microspheres with core‐shell morphology. Next, the trichloro(4‐chloromethylphenyl) silane was immobilized on them, reacted with iminodiacetic acid (IDA), and charged with Cu²⁺. The obtained magnetic silica sub‐microspheres with immobilized Cu²⁺ were applied for the absorption of bovine hemoglobin (BHb) and the removal of BHb from bovine blood. The size, morphology, and magnetic properties of the resulting magnetic micro(nano) spheres were investigated by using scanning microscopy (SEM), transmission electron microscopy (TEM), X‐ray diffraction (XRD), and a vibrating sample magnetometer (VSM). The measurements showed that the magnetic sub‐microspheres are spherical in shape, very uniform in size with a core‐shell, and are almost superparamagnetic. The saturation magnetization of silica‐coated magnetite (Fe₃O₄) sub‐microspheres reached about 33 emu g^?1. Protein adsorption results showed that the sub‐microspheres had a high adsorption capacity for BHb (418.6 mg g^?1), low nonspecific adsorption, and good removal of BHb from bovine blood. This opens a novel route for future applications in removing abundant proteins in proteomic analysis.     

Hydrophilic dual‐responsive magnetite/PMAA core/shell microspheres with high magnetic susceptibility and ph sensitivity via distillation‐precipitation polymerization

A facile and effective approach to preparation of dual‐responsive magnetic core/shell composite microspheres is reported. The magnetite(Fe₃O₄)/poly(methacrylic acid) (PMAA) composite microspheres were synthesized through encapsulating γ‐methacryloxypropyltrimethoxysilane (MPS)‐modified magnetite colloid nanocrystal clusters (MCNCs) with crosslinked PMAA shell. First, the 200‐nm‐sized MCNCs were fabricated through solvothermal reaction, and then the MCNCs were modified with MPS to form active vinyl groups on the surface of MCNCs, and finally, a pH‐responsive shell of PMAA was coated onto the surface of MCNCs by distillation‐precipitation polymerization. The transmission electron microscopy (TEM) and vibrating sample magnetometer characterization showed that the obtained composite microspheres had well‐defined core/shell structure and high saturation magnetization value (35 emu/g). The experimental results indicated that the thickness and degree of crosslinking of PMAA shell could be well‐controlled. The pH‐induced change in size exhibited by the core/shell microspheres reflected the PMAA shell contained large amount of carboxyl groups. The carboxyl groups and high saturation magnetization make these microspheres have a great potential in biomolecule separation and drug carriers. Moreover, we also demonstrated that other magnetic polymeric microspheres, such as Fe₃O₄/PAA, Fe₃O₄/PAM, and Fe₃O₄/PNIPAM, could be synthesized by this approach. © 2011 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2011.     

Alginate-Coated Fe3O4 Hollow Microspheres for Drug Delivery

Novel hollow Fe₃O₄ nanoparticles for drug delivery were synthesized via a one-step templatefree approach. These nanoparticles were obtained by modifing the Fe₃O₄ nanoparticles with 3-aminopropyltrimethoxy silane, and then grafting alginate onto the surface of amine magnetic. The hollow structure of Fe₃O₄ spheres was characterized by TEM, XRD, and XPS. The M-H hysteresis loop indicated that the magnetic spheres exhibit superparamagnetic characteristics at room temperature. Daunorubicin acting as a model drug was loaded into the carrier, and the maximum percent of envelop and load were 28.4% and 14.2% respectively. The drug controlled releasing behaviors of the carriers were compared in different pH media.     

单分散Fe3O4纳米颗粒的控制合成和表征

以十八烯为溶剂、乙酰丙酮铁为铁源,并在油酸、油胺的辅助作用下,通过热分解法成功合成了单分散Fe3O4纳米颗粒。讨论了实验参数如反应温度、表面活性剂的量和种类、溶剂、油酸、油胺对单分散Fe3O4纳米颗粒的尺寸及形貌的影响。利用X射线衍射（XRD）、透射电子显微镜（TEM）、选区电子衍射（SAED）和高分辨透射电子显微镜（HRTEM）对所得产物的物相、结构、尺寸和形貌进行了表征分析。通过振动样品磁强计（VSM）表征产物磁性能,表明在室温下,Fe3O4纳米颗粒的饱和磁化强度（Ms）和矫顽力（Hc）分别为74.0 emu/g,72.6 Oe。     

中空分级结构Fe3O4@C/rGO复合材料的合成及其储锂性能

以氧化石墨烯(GO)为基底,Fe(NO_3)_3·9H_2O、异丙醇、甘油为原料,通过溶剂热法和后续热处理过程2步合成了Fe_3O_4@C/rGO复合材料,实现了碳包覆的Fe_3O_4纳米粒子自组装形成的分级结构空心球在氧化石墨烯片上的原位生长。采用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和恒流充放电等手段分析了材料的物理化学性能与储锂性能。结果表明,该复合材料在5.0 A·g~(-1)的电流密度下,仍有437.7 mAh·g~(-1)的可逆容量,在1.0 A·g~(-1)下循环200圈后还有587.3 mAh·g~(-1)的放电比容量。这主要归因于还原态氧化石墨烯(rGO)对碳包覆Fe_3O_4分级空心球整体结构稳定性和导电性的提高。     

The Synthesis of Magnetic Lysozyme‐Imprinted Polymers by Means of Distillation–Precipitation Polymerization for Selective Protein Enrichment

A protein imprinting approach for the synthesis of core–shell structure nanoparticles with a magnetic core and molecularly imprinted polymer (MIP) shell was developed using a simple distillation–precipitation polymerization method. In this work, Fe₃O₄ magnetic nanoparticles were first synthesized through a solvothermal method and then were conveniently surface‐modified with 3‐(methacryloyloxy)propyltrimethoxylsilane as anchor molecules to donate vinyl groups. Next a high‐density MIP shell was coated onto the surface of the magnetic nanoparticles by the copolymerization of functional monomer acrylamide (AAm), cross‐linking agent N,N′‐methylenebisacrylamide (MBA), the initiator azodiisobutyronitrile (AIBN), and protein in acetonitrile heated at reflux. The morphology, adsorption, and recognition properties of the magnetic molecularly imprinted nanoparticles were investigated by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X‐ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), vibrating sample magnetometer (VSM), and rebinding experiments. The resulting MIP showed a high adsorption capacity (104.8 mg g^?1) and specific recognition (imprinting factor=7.6) to lysozyme (Lyz). The as‐prepared Fe₃O₄@Lyz‐MIP nanoparticles with a mean diameter of 320 nm were coated with an MIP shell that was 20 nm thick, which enabled Fe₃O₄@Lyz‐MIP to easily reach adsorption equilibrium. The high magnetization saturation (40.35 emu g^?1) endows the materials with the convenience of magnetic separation under an external magnetic field and allows them to be subsequently reused. Furthermore, Fe₃O₄@Lyz‐MIP could selectively extract a target protein from real egg‐white samples under an external magnetic field.     

Synthesis,composition, and magnetic properties of the ferrimagnetic NdCu3−xMn4+xO12 perovskite-like phases

A magnetic oxide with composition close of NdCu₃Mn₄O₁₂ with a perovskite-related cubic structure ($\text{a ? 7.30}$ Å, space group Im3, Z = 2) has been synthesized by using either the high-pressure or the hydrothermal technique. The composition is strongly dependent on the synthesis conditions. A partial reduction of Mn⁴⁺ in the octahedral sites, resulting in a partial substitution of Cu²⁺ by Mn³⁺ in the Jahn-Teller sites, leads to the actual formula Nd(Cu²⁺_3?xMn³⁺_x)(Mn⁴⁺_3?xMn³⁺_1+x)O₁₂. For the compound synthesized at 650°C/2 kbar, the value of the substitution parameter x, as determined by neutron diffraction, is 0.32. For samples synthesized at higher temperatures, larger values of x are obtained. The compound is ferrimagnetic with Néel temperature of 390 K and a spontaneous magnetization of 93 emu/g at 4 K (52 emu/g at room temperature). For larger x values, magnetizations up to 118 emu/g at 4 K are obtained.     

Synthesis and characterization of micron‐sized monodisperse superparamagnetic polymer particles with amino groups

Micron‐sized monodisperse superparamagnetic polyglycidyl methacrylate (PGMA) particles with functional amino groups were prepared by a process involving: (1) preparation of parent monodisperse PGMA particles by the dispersion polymerization method, (2) chemical modification of the PGMA particles with ethylenediamine (EDA) to yield amino groups, and (3) impregnation of iron ions (Fe²⁺ and Fe³⁺) inside the particles and subsequently precipitating them with ammonium hydroxide to form magnetite (Fe₃O₄) nanoparticles within the polymer particles. The resultant magnetic PGMA particles with amino groups were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), X‐ray diffractometry (XRD), and vibrating sample magnetometry (VSM). SEM showed that the magnetic particles had an average size of 2.6 μm and were highly monodisperse. TEM demonstrated that the magnetite nanoparticles distributed evenly within the polymer particles. The existence of amino groups in the magnetic polymer particles was confirmed by FTIR. XRD indicated that the magnetic nanoparticles within the polymer were pure Fe₃O₄ with a spinel structure. VSM results showed that the magnetic polymer particles were superparamagnetic, and saturation magnetization was found to be 16.3 emu/g. The Fe₃O₄ content of the magnetic particles was 24.3% based on total weight. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 3433–3439, 2005     

Preparation and Characterization of Fe3O4/Ethiodized‐oil Magnetic Fluids Used in Arterial Embolization Hyperthermia

Fe₃O₄ nanoparticles (NPs) were prepared by the co‐precipitation of Fe³⁺ and Fe²⁺ with ammonium hydroxide, and were modified by four different surfactants. The modified Fe₃O₄ NPs were characterized by Fourier transform infrared spectroscopy, X‐ray powder diffraction, transmission electron microscopy and vibrating sample magnetometer. Then, the modified Fe₃O₄ NPs were dispersed in ethiodized‐oil by mechanical agitation and ultrasonic vibration to obtain stable Fe₃O₄/ethiodized‐oil magnetic fluids (MFs). The magnetic properties and rheological properties of the MFs were measured using a Gouy magnetic balance and a rotational rheometer, respectively. The saturation magnetization of the Fe₃O₄ modified by oleic acid was 52.1 emu/g. Furthermore, the result showed that the inductive heating effect of oleic acid stabilized Fe₃O₄/ethiodized‐oil MF was remarkable and it only took 650 s for the temperature rising from 25°C to 65°C. The specific absorption rate of the MF was 50.16 W/(g of Fe). It had a potential application in arterial embolization hyperthermia.     

An easy synthesis of nanostructured magnetite-loaded functionalized carbon spheres and cobalt ferrite

An easy method in a solvothermal system has been developed to synthesize nanostructured magnetite (Fe₃O₄)-loaded functionalized carbon spheres (CSs) and cobalt ferrite (CoFe₂O₄). Surface-tunable CSs loaded with iron oxide (Fe₃O₄) nanoparticles were prepared using an acetylferrocene Schiff base (OPF), whereas spinel cobalt ferrite (CoFe₂O₄) was synthesized via metal complexes of a ferrocenyl Schiff base with phenol moiety (Co-OPF). The formed composite powder was investigated using X-ray powder diffraction, Raman spectrometry, Fourier transform infrared spectroscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and vibrating sample magnetometry. It was found that most of the iron oxide nanoparticles were evenly distributed upon the surface of the CSs. Furthermore, the surface of the iron oxide-loaded CSs has large numbers of functional groups. Good saturation magnetization was achieved for the formed magnetic nanoparticles.     

Microwave-assisted synthesis and characterization of hexagonal Fe3O4 nanoplates

Hexagonal magnetite (Fe₃O₄) nanoplates with an average edge length of 80 nm were successfully prepared in large quantities by a facile microwave-assisted route. The influences of experiment parameters such as reaction time, microwave power, and concentration of NaOH and other additive agents on the morphology and size of final products were investigated in detail. Phase structure, morphology and magnetic properties of products were carefully studied by X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), high-resolution transmission electron microscope (HRTEM), and vibrating sample magnetometer (VSM). Magnetic studies revealed that hexagonal Fe₃O₄ nanoplates have low saturation magnetization of 36.4 emu/g and the possible reason has been proposed.