Nanocrystalline SrCexFe12?xO19 (x?=?0.00, 0.02, 0.04, 0.06, 0.08) microfibers by sol–gel method

The SrCe_xFe_12?xO₁₉ (x????0.08) ferrite microfibers were prepared via sol?Cgel method from starting reagents of metal nitrate salts and citric acid. The obtained microfibers were characterized by TG-DSC, X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM). The XRD patterns show that the main phase is M-type strontium hexaferrite without other impurity phases when calcined at 750?°C for 1?h, and the Ce³⁺ ions doping has not resulted in crystal structural changes of the Sr ferrite magnetoplumbite type structure. The SEM and TEM images indicate that samples with different calcination temperature and various values of x possess the diameters of below 10???m and homogeneous hexagonal plate-like morphology. The VSM results show that saturation magnetization (Ms) gradually increases with increase of calcination temperature while decreases with increase of addition of Ce³⁺ ions, and coercive force (Hc) reveals an increase at first and then decreases with increase of calcination temperature and Ce³⁺ ions content.     

Synthesis of SrFe12O19 magnetic nanoparticles by EDTA complex method

A modified polyacrylamide gel route was used to prepare SrFe₁₂O₁₉ magnetic nanoparticles; ethylenediaminetetraacetic acid (EDTA) was used as a carboxyl chelating agent. The phase purity, morphology and magnetic properties of as-prepared samples were analyzed via X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometery (VSM). XRD analysis indicates that high-purity SrFe₁₂O₁₉ magnetic nanoparticles can be synthesized at 700°C in air. The characteristic peaks of as-prepared sample at 210, 283, 321, 340, 381, 411, 432, 475, 532, 618, 686, and 726 cm^–1 were observed in Raman spectra. SEM and TEM show that the synthesized SrFe₁₂O₁₉ magnetic nanoparticles are uniform with the mean particle size of ~60 nm. VSM measurement shows that the maximum magnetic energy product (BH)_max of sample prepared using EDTA as a chelating agent is higher than that of sample prepared using citric acid as a chelating agent.

     

A simple route to synthesize nanocrystalline nickel ferrite (NiFe2O4) in the presence of octanoic acid as a surfactant

Nanocrystalline nickel ferrite (NiFe₂O₄) powder was prepared by a co-precipitation method from Ni and Fe chlorides. The as-prepared samples were characterized by powder X-ray diffractometry (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR) and vibrating sample magnetometry (VSM). SEM and TEM indicated that the particles were spherical with particle sizes in the range 25 ± 5 nm. The magnetic properties of the sample were measured by using a vibrating sample magnetometer, which showed that the sample exhibited typical ferromagnetic behavior at room temperature, while a finite coercivity of 245.5 Oe was present at 300 K. The saturation magnetization of the sample (23.13 emu/g) was significantly lower than that for the reported multidomain bulk particles (55 emu/g), reflecting the ultrafine nature of the sample.     

Synthesis,characterization and application of nano‐CoAl2O4 as an efficient catalyst in the preparation of hexahydroquinolines

In this work, nano‐CoAl₂O₄ was prepared and characterized by FT‐IR, energy dispersive X‐ray analysis (EDX), X‐ray diffraction patterns (XRD), scanning electron microscopy (SEM), vibrating sample magnetometer (VSM) and transmission electron microscopy (TEM). Nano‐CoAl₂O₄ was applied for the synthesis of hexahydroquinoline derivatives by the condensation reaction between ethyl acetoacetate, dimedone and various aldehydes. These reactions were carried out at 80 °C under solvent‐free conditions.     

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     

An Fe3O4 nanoparticle-supported Mn (II)-azo Schiff complex acts as a heterogeneous catalyst in alcoholysis of epoxides

In this paper, an azo-containing Schiff base complex of manganese [Mn²⁺-azo ligand@APTES-SiO₂@Fe₃O₄] immobilized on chemically modified Fe₃O₄ nanoparticles has been used as a magnetically retrievable catalyst for the alcoholysis of different epoxides to their corresponding alkoxy alcohols with methanol, ethanol and n-propanol. The newly magnetic nanoparticles (MNPs) were characterized by Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and vibrating sample magnetometry (VSM).     

Preparation and characterization of rapid magnetic recyclable Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@SiO<Subscript>2</Subscript>@TiO<Subscript>2</Subscript>–Sn photocatalyst

Effective procedure to synthesize Fe₃O₄@SiO₂@TiO₂–Sn magnetically separable photocatalyst by a combination of co-precipitation, sol–gel and photodeposition methods was introduced. Products were characterized by XRD, SEM, VSM, EDS, DRS, TEM, ICP-OES and IR techniques. The dimensions of catalyst particle size were evaluated by scanning electron microscopy, and results approved nanoscale size for product. In addition, studying the magnetic nature by VSM analysis showed superparamagnetic properties for all samples. XRD pattern indicates that TiO₂ coated on Fe₃O₄@SiO₂ core well crystallized at 400 °C in anatase phase. Synthesized photocatalyst shows good photocatalytic performance in decolorization of rhodamine B aqueous solution. The composite nanoparticles showed high recycling efficiency and stability over five separation cycles.     

Palladium nanoparticles supported on modified hollow Fe3O4@TiO2: Preparation,characterization, and catalytic activity in Suzuki cross‐coupling reactions

Hollow Fe₃O₄@TiO₂‐NH₂/Pd as a light‐weight, magnetically heterogeneous catalyst was successfully prepared, and characterized by using different techniques including X‐ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT‐IR), field‐emission scanning electron microscopy (FE‐SEM), transmission electron microscopy (TEM), energy‐dispersive X‐ray spectroscopy (EDX), vibrating sample magnetometer (VSM) measurements, and thermogravimetric analysis (TGA). Then this heterogeneous catalyst was tested in the Suzuki cross‐coupling reaction, and the results confirmed the success of this method. The catalyst could be separated easily using an external magnet and reused at least in five runs successfully without any appreciable loss in its catalytic activity.     

离子热法合成多级孔CuAPO-5分子筛

采用丁二酸、氯化胆碱与四乙基溴化铵三元低共熔体为溶剂和模板剂,借助微波辐射快速合成了具有多级孔结构的CuAPO-5分子筛.系统地考察了P₂O₅/Al₂O₃、HF/Al₂O₃与CuO/Al₂O₃的物质量之比,铝源及铜源对CuAPO-5分子筛合成的影响.利用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和N₂物理吸脱附等检测手段对合成产物的结晶度、形貌和孔结构等进行了表征.通过SEM可知在一定的条件下,可得到具有六角纳米盘状特殊形貌的CuAPO-5分子筛.N₂物理吸脱附、SEM和TEM分析表明该分子筛是一种同时存在微孔和介孔的多级孔磷酸铝分子筛材料.     

离子热法合成多级孔CuAPO-5分子筛

采用丁二酸、氯化胆碱与四乙基溴化铵三元低共熔体为溶剂和模板剂,借助微波辐射快速合成了具有多级孔结构的CuAPO-5分子筛。系统地考察了P2O5/Al2O3、HF/Al2O3与Cu O/Al2O3的物质量之比,铝源及铜源对CuAPO-5分子筛合成的影响。利用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和N2物理吸脱附等检测手段对合成产物的结晶度、形貌和孔结构等进行了表征。通过SEM可知在一定的条件下,可得到具有六角纳米盘状特殊形貌的CuAPO-5分子筛。N2物理吸脱附、SEM和TEM分析表明该分子筛是一种同时存在微孔和介孔的多级孔磷酸铝分子筛材料。     

Self-assembly of Fe3O4 nanocrystal-clusters into cauliflower-like architectures: Synthesis and characterization

Large-scale cauliflower-like Fe₃O₄ architectures consist of well-assembled magnetite nanocrystal clusters have been synthesized by a simple solvothermal process. The as-synthesized Fe₃O₄ samples were characterized by XRD, XPS, FT-IR, SEM, TEM, etc. The results show that the samples exhibit cauliflower-like hierarchical microstructures. The influences of synthesis parameters on the morphology of the samples were experimentally investigated. Magnetic properties of the Fe₃O₄ cauliflower-like hierarchical microstructures have been detected by VSM at room temperature, showing a relatively low saturation magnetization of 65 emu/g and an enhanced coercive force of 247 Oe.     

Efficient and selective oxidation of alcohols in water employing palladium supported nanomagnetic Fe3O4@hyperbranched polyethylenimine (Fe3O4@HPEI.Pd) as a new organic–inorganic hybrid nanocatalyst

Palladium immobilized magnetic nanoFe₃O₄@hyperbranched polyethylenimine (Fe₃O₄@HPEI.Pd) was prepared according to a simple and cost effective pathway and it was employed as a new efficient and selective organic–inorganic hybrid nanocatalyst for the aqueous oxidation of primary and secondary alcohols to their corresponding products in good yields applying oxone (potassium hydrogen monopersulfate) and H₂O₂ as an oxidant at room temperature. Moreover, the catalytic system was reused at least 13 times without significant loss of activity. The complete characterization of this efficient nanocatalyst was investigated by FTIR, UV–Vis, TEM, SEM, XRD, TGA, VSM, ICP and EDX techniques.     

Study on synthesis of superparamagnetic spinel cobalt ferrite nanoparticles as layered double hydroxides by co-precipitation method

Cobalt ferrite layered double hydroxide (LDH) nanoparticles with cubic structure were synthesized by the co-precipitation method: addition of NaOH solution to a solution of Co²⁺ and Fe³⁺. Formation of nanoparticles was confirmed by XRD, SEM, TEM, PSA, FT-IR, TGA, DSC, and magnetic characteristics were measured using VSM. Crystals produced by calcination at 900°C possessed high coercivity and pronounced physical and chemical stability. Nanoparticles of CoFe₂O₄ formed outer layers with poor crystallization on the surface of cobalt ferrite nanocrystals.     

Ultrasonic-assisted synthesis of PMMA/Ni0.5Zn0.5Fe2O4 nanocomposite in mixed surfactant system

PMMA/Ni_0.5Zn_0.5Fe₂O₄ nanocomposite with superparamagnetic behavior was synthesized by in situ emulsion polymerization of methylmethacrylate (MMA) monomer in the presence of Ni_0.5Zn_0.5Fe₂O₄ colloidal suspension assisted by ultrasonic irradiation. The obtained samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectra (FT-IR), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM). XRD and FT-IR spectra confirmed the formation of PMMA/Ni_0.5Zn_0.5Fe₂O₄ nanocomposite. TEM images showed that Ni_0.5Zn_0.5Fe₂O₄ nanoparticles with the particle sizes of about 12 nm were well dispersed in the polymer matrix. The nanocomposite at room temperature exhibited superparamagnetic behavior under applied magnetic field. The formation mechanism of PMMA/Ni_0.5Zn_0.5Fe₂O₄ nanocomposite was proposed as well.     

Oxoperoxo tungsten(VI) complex immobilized on Schiff base-modified Fe3O4 magnetic nanoparticles as a heterogeneous catalyst for oxidation of alcohols with hydrogen peroxide

Oxoperoxo tungsten(VI) complex immobilized on Schiff base-modified Fe₃O₄ super paramagnetic nanoparticles were synthesized and appropriately characterized using FT-IR, XRD, SEM, TEM, EDX, BET, and VSM analysis. The synthesized nanoparticles efficiently catalyzed oxidation of benzylic alcohols with H₂O₂ as oxidant in high yields, with high to excellent selectivity. The catalyst can be recovered using an external magnetic field and recycled for subsequent oxidation reactions without any appreciable loss of efficiency. The simple preparation, high activity, excellent selectivity, and simple recoverability of the catalyst are advantageous.     

Applications of iron and nickel immobilized on hydroxyapatite‐core‐shell γ‐Fe2O3 as a nanomagnetic catalyst for the chemoselective oxidation of sulfides to sulfoxides under solvent‐free conditions

In the present study, Fe²⁺ and Ni²⁺ immobilized on hydroxyapatite‐core‐shell γ‐Fe₂O₃ (γ‐Fe₂O₃@HAp‐Fe²⁺ and γ‐Fe₂O₃@HAp‐Ni²⁺) with a high surface area has been synthesized and characterized by Fourier transform infrared (FTIR), X‐ray diffraction (XRD), vibrating sample magnetometer (VSM), transmission electron microscopy (TEM), and scanning electron microscope (SEM) techniques. Then, γ‐Fe₂O₃@HAp‐Fe²⁺ and γ‐Fe₂O₃@HAp‐Ni²⁺ were used as a new and magnetically recoverable nano catalyst for the selective oxidation of sulfides to sulfoxides with 33% aqueous H₂O₂ (0.5 mL) as an oxidant at room temperature in good to excellent yields and short reaction time. Nontoxicity of reagent, mild reaction condition, inexpensive and high catalytic activity, simple experimental procedure, short period of conversion and excellent yields, and ease of recovery from the reaction mixture using an external magnet are the advantages of the present method.     

Synthesis of a new magnetic nano-island titania photocatalyst and investigation of its photocatalytic activity

In this study, a new magnetic nano-island titania photocatalyst (Fe₃O₄@SiO₂·TiO₂) was designed and fabricated. Precipitation, sol-gel, and hydrothermal methods were utilized to synthesize the magnetite, silica shell, and titania islands, respectively. Characterization of the synthesized catalyst was carried out by XRD, EDS, FTIR, SEM, TEM, and VSM analysis. The TEM analysis revealed that the overall size of the catalyst is about 490 nm, and titania island on the magnetic core was about 50 nm. VSM analysis showed that the photocatalyst has a fantastic paramagnetic property with magnetic saturation of 52 emu g^?1. Furthermore, photocatalytic activity of the synthesized catalyst was evaluated in the removal of p-nitrophenol as a typical pollutant of nitro-aromatic compounds such that its degradation and mineralization efficiency were obtained at 82 and 45% after 100 and 200 min of the process, respectively, using 100 ppm of the photocatalyst in pH = 6.5.     

Copper-based Schiff Base Complex Immobilized on Core-shell Fe3O4@SiO2 as a magnetically recyclable and highly efficient nanocatalyst for green synthesis of 2-amino-4H-chromene derivatives

Fe₃O₄-supported copper (II) Schiff-Base complex has been synthesized through post-modification with 1,3-phenylenediamine followed by further post-modification with salicylaldehyde and coordination with Cu(II) ion. The resulted Fe₃O₄@SiO₂-imine/phenoxy-Cu(II) magnetic nanoparticles (MNPs) were characterized by various techniques including SEM, TEM, XRD, XPS, EDX, VSM, FT-IR, and ICP. The catalytic activity as a magnetically recyclable heterogeneous catalyst for one-pot, three-component synthesis of 2-amino-4H-chromene derivatives was examined. The catalyst is efficient in the reaction and can be recovered by magnetic separation and recycled several times without significant loss in the catalytic activity.     

Olefins oxidation with molecular O2 in the presence of chiral Mn (III) salen complex supported on magnetic CoFe2O4@SiO2@CPTMS

In the present study, CoFe₂O₄@SiO₂@CPTMS nanocomposite was synthesized and the homogeneous chiral Mn‐salen complex was anchored covalently onto the surface of CoFe₂O₄@SiO₂@CPTMS nanocomposite. The heterogeneous Mn‐salen magnetic nanocatalyst (CoFe₂O₄@SiO₂@CPTMS@ chiral Mn (III) Complex) was characterized by different techniques including transmission electron microscopy (TEM), Fourier transform infrared (FT‐IR), vibrating sample magnetometer (VSM), scanning electron microscopy (SEM), powder X‐ray diffraction (XRD) and thermogravimetric analysis (TGA). Then, the aerobic enantioselective oxidation of olefins to the corresponding epoxide was investigated in the presence of magnetic chiral CoFe₂O₄@SiO₂@Mn (III) complex at ambient conditions within 90 min. The results showed the corresponding products were synthesized with excellent yields and selectivity. In addition, the heterogeneous CoFe₂O₄@SiO₂@ CPTMS@ chiral Mn (III) complex has benefits such as high selectivity and comparable catalytic reactivity with its homogeneous analog as well as mild reaction condition, facile recovery, and recycling of the heterogeneous catalyst.     

Fabrication and characterization of Fe_3O_4@SiO_2@TiO_2@Ho nanostructures as a novel and highly efficient photocatalyst for degradation of organic pollution

In this work we synthesize a novel and highly efficient photocatalyst for degradation of methyl orange and rhodamine B. In addition, a new method for synthesis of Fe_3O_4@SiO_2@TiO_2@Ho magnetic core-shell nanoparticles with spherical morphology is proposed. The crystal structures, morphology and chemical properties of the as-synthesized nanoparticles were characterized using Fourier transform infrared spectroscopy(FT-IR), scanning electron microscopy(SEM), transmission electron microscopy(TEM), energy dispersive X-ray(EDS), X-ray diffraction(XRD), UV–vis diffuse reflectance spectroscopy(DRS) and vibrating sample magnetometer(VSM) techniques. The photocatalytic activity of Fe_3O_4@SiO_2@TiO_2@Ho was investigated by degradation of methyl orange(MO) as cationic dye and rhodamine B(Rh B) as anionic dye in aqueous solution under UV/vis irradiation. The results indicate that about 92.1% of Rh B and78.4% of MO were degraded after 120 and 150 min, respectively. These degradation results show that Fe_3O_4@SiO_2@TiO_2@Ho nanoparticles are better photocatalyst than Fe3O4@Si O2@TiO 2@Ho for degradation of MO and Rh B. As well as, the catalyst shows high recovery and stability even after several separation cycles.