Fabrication,characterization and X-band microwave absorption properties of PAni/Fe3O4/PVA nanofiber composites materials

This work presents a study of microwave absorption properties of PAni/Fe₃O₄/PVA nanofiber composites with different ratio of Fe₃O₄ nanoparticles. The morphology of the composites nanofibers study by Field Emission Scanning Electron Microscopes (FESEM) and Transmission Electron Microscope (TEM) showed that the low content of Fe₃O₄ nanoparticles presence in the composites nanofibers indicates very much uniform surface, in the composites nanofiber without many bends, but some bends develop at higher content of Fe₃O₄ nanoparticles as indicated in the TEM image. Image-J software was used to further investigate the diameter of the composites nanofiber and found to be in the range of 152 to 195 nm. The nanofiber composites show excellent electric and magnetic properties and therefore vary with the addition of Fe₃O₄ nanoparticles in the composites nanofiber. In addition the PAni/Fe₃O₄/PVA composites nanofibers were further characterized by X-ray diffraction spectra (XRD) and Four Transformation infrared spectra (FTIR). The XRD pattern shows the presence of PAni nanotubes containing Fe₃O₄ nanoparticles by indicating peaks at 23.4⁰ and 35.43⁰ which was further supported by FTIR analysis. Microwave vector network analyzers (MVNA) were used to estimate the microwave absorption properties of the composites nanofibers. The absorption parameters was found to be −6.4 dB at 12.9 GHz within the range of X-band microwave absorption frequency, this reflection loss is attributed to the multiple absorption mechanisms as a result of the improved of impedance matching between dielectric and magnetic loss of the absorbent materials demonstrating that these materials can be used as protective material for electromagnetic radiation.     

Synthesis and characterization of novel magnetic Fe3O4/polyphosphazene nanofibers

Novel magnetic Fe₃O₄/polyphosphazene nanofibers were successfully prepared via a facile approach by ultrasonic irradiation. The structure and morphology were characterized by SEM, TEM, EDX, IR and XRD. The characterization results show that the magnetic Fe₃O₄/polyphosphazene nanofibers are several microns in length and 50–100 nm in diameter with Fe₃O₄ nanoparticles of 5–10 nm attached on the surface. The interaction between Fe₃O₄ nanoparticles and polyphosphazene nanofibers was thought as coordination behavior. TG curves show that the magnetic Fe₃O₄/polyphosphazene nanofibers have good thermostability and high magnetism content of about 44%. Magnetic studies show that the magnetic nanofibers exhibit good superparamagnetic properties with high magnetization saturation value of about 36 emu/g.     

Controlled assembly of superparamagnetic iron oxide nanoparticles on electrospun PU nanofibrous membrane: A novel heat-generating substrate for magnetic hyperthermia application

A facile method of fabricating novel heat-generating membranes composed of electrospun polyurethane (PU) nanofibers decorated with superparamagnetic iron oxide nanoparticles (NPs) is reported. Electrospinning was used to produce polymeric nanofibrous matrix, whereas polyol immersion technique allowed in situ assembly of well-dispersed Fe₃O₄ NPs on the nanofibrous membranes without any surfactant, and without sensitizing and stabilizing reagent. The assembly phenomena can be explained by the hydrogen-bonding interactions between the amide groups in the PU matrix and the hydroxyl groups capped on the surface of the Fe₃O₄ NPs. The prepared nanocomposite fibers showed acceptable magnetization value of 33.12 emu/g, after measuring the magnetic hysteresis loops using SQUID. Moreover, the inductive heating property of electrospun magnetic nanofibrous membranes under an alternating current (AC) magnetic field was investigated. We observed a progressive increase in the heating rate with the increase in the amount of magnetic Fe₃O₄ NPs in/on the membranes. The present electrospun magnetic nanofibrous membrane may be a potential candidate as a novel heat-generating substrate for localized hyperthermia cancer therapy.     

Novel fabrication of magnetic thermoplastic nanofibers via melt extrusion of immiscible blends

A novel technique of fabricating magnetic thermoplastic nanofibers by the control of the phase separation of immiscible polymer blends during melt extrusion was presented. The magnetic poly(vinyl alcohol‐co‐ethylene) (PVA‐co‐PE)/Fe₃O₄ composite nanofibers were prepared via the melt extrusion of cellulose acetate butyrate matrix and PVA‐co‐PE preloaded with different amounts of Fe₃O₄ nanoparticles. The morphologies of magnetic composite nanofibers were characterized by scanning electron microscopy. The uniform dispersion of Fe₃O₄ nanoparticles in nanofiber matrixes and crystal structures were confirmed using transmission electron microscopy and wide angle X‐ray diffraction. Thermogravimetric analysis was employed to quantify the exact loading amount of Fe₃O₄ nanoparticles in the composite nanofibers. The magnetic measurements showed that composite nanofibers displayed superparamagnetic behavior at room temperature. With increasing content of Fe₃O₄ nanoparticles, the saturation magnetization of the magnetic composite nanofiber significantly improved. The prepared magnetic composite nanofibers might have found potential applications in the sensors and bio‐molecular separation fields. Copyright © 2012 John Wiley & Sons, Ltd.     

Synthesis and properties of thermoresponsive magnetic polymer composites and their electrospun nanofibers

The thermoresponsive magnetic polymer composites and nanofibers were fabricated. Their thermal and magnetic properties were also investigated. Fe₃O₄ nanoparticles were prepared by coprecipitation method. Further condensation reaction was used to fabricate the double‐layer lauric acid modified Fe₃O₄ (DLF) nanoparticles dispersed well in water. Thermal properties of poly(N‐isopropylacrylamide) (PNIPAAm) and DLF/PNIPAAm composites and their aqueous solutions were measured by TGA and DSC. With the increasing of DLF content, the interaction between DLF and PNIPAAm caused the lower critical solution temperature (LCST) of polymer solution to shift from 33 to 31.25 °C. The effects of concentration and pH on LCST were also studied. The DLF/PNIPAAm nanofibers were fabricated by electrospinning. Their diameters were around 100–250 nm. Magnetization curves of DLF/PNIPAAm composite and nanofibers were overlapped and the saturated magnetizations were the same. Magnetic attraction behaviors of DLF/PNIPAAm polymer solution at temperatures below and above LCST were different. Aggregation of DLF/PNIPAAm above LCST enhanced magnetic moment density as well as magnetic attraction ability. © 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2014 , 52, 848–856     

磁靶向纳米Fe3O4-TiO2复合物的制备及其对肝癌细胞的光催化杀伤效应

采用三种低温溶胶-凝胶法制备了具有不同Fe₃O₄掺杂量的磁靶向纳米Fe₃O₄-TiO₂复合物, 通过X射线衍射(XRD)、透射电镜(TEM)、傅里叶变换红外(FTIR)光谱、紫外-可见(UV-Vis)光谱、荧光光谱(FS)及磁性能分析等表征方法筛选出包覆均匀、分散性好、磁性能优异及光催化活性较高的纳米Fe₃O₄-TiO₂复合物. 以四甲基偶氮唑蓝(MTT)法检测肝癌细胞(HepG2)的存活率, 考察纳米Fe₃O₄-TiO₂复合物在外磁场作用下对HepG2 细胞的光催化杀伤效应. 结果表明: 采用方法三制备的5%(质量分数)Fe₃O₄-TiO₂复合物具备核-壳结构, 在混悬液中分散性较好, 平均粒径约为50 nm, 具有较强的光催化活性和良好的磁响应性, 同时将纳米TiO₂的光响应范围拓宽至444 nm; 在外磁场作用下, 紫外光和可见光激发纳米Fe₃O₄-TiO₂复合物对HepG2细胞的杀伤效应差异不大, 且均强于纳米TiO₂; 其杀伤效应在0-1.0 T范围内随着外磁场强度的增大而增强.     

用于高效去除水中孔雀石绿的三层结构磁性复合材料Fe3O4@聚丙烯酸@ZiF-8的制备

设计并合成了一种以磁性纳米粒子为核,聚合物为中间层,金属有机骨架材料为外层的三层结构磁性复合材料(Fe₃O₄@PAA@ZIF-8)。首先利用溶剂热法制备Fe₃O₄纳米粒子,然后通过蒸馏沉淀聚合法在Fe₃O₄纳米粒子表面包覆聚丙烯酸(PAA)层,最后通过原位沉积法在PAA外部包覆ZIF-8。在对Fe₃O₄@PAA@ZIF-8的组成和结构进行表征的基础上,深入研究其对孔雀石绿(MG)的吸附性能。透射电子显微镜(TEM)显示Fe₃O₄@PAA@ZIF-8具有明显的三层结构,Fe₃O₄的平均粒径为117nm,PAA层厚度约为17 nm,ZIF-8层的厚度约为14 nm。Fe₃O₄@PAA@ZIF-8对MG的吸附量随着p H的升高而增大,吸附过程符合准二阶动力学模型和Langmuir等温吸附模...     

用于高效去除水中孔雀石绿的三层结构磁性复合材料Fe3O4@聚丙烯酸@ZiF-8的制备

设计并合成了一种以磁性纳米粒子为核，聚合物为中间层，金属有机骨架材料为外层的三层结构磁性复合材料(Fe₃O₄@PAA@ZIF 8)。首先利用溶剂热法制备Fe₃O₄纳米粒子，然后通过蒸馏沉淀聚合法在Fe₃O₄纳米粒子表面包覆聚丙烯酸(PAA)层，最后通过原位沉积法在PAA外部包覆ZIF 8。在对Fe₃O₄@PAA@ZIF 8的组成和结构进行表征的基础上，深入研究其对孔雀石绿(MG)的吸附性能。透射电子显微镜(TEM)显示 Fe₃O₄@PAA@ZIF 8 具有明显的三层结构，Fe₃O₄的平均粒径为 117nm，PAA 层厚度约为 17 nm，ZIF 8层的厚度约为 14 nm。Fe₃O₄@PAA@ZIF 8对 MG 的吸附量随着 pH 的升高而增大，吸附过程符合准二阶动力学模型和 Langmuir等温吸附模型。此外，Fe₃O₄@PAA@ZIF 8还表现出良好的重复利用性能，8次循环利用后对MG(500 mg·L^-1)的最大吸附量仍可达982 mg·g^-1。     

Facile synthesis of multifunctional multiwalled carbon nanotubes/Fe3O4 nanoparticles/polyaniline composite nanotubes

With an average diameter of 100-150 nm, composite nanotubes of polyaniline (PANI)/multiwalled carbon nanotubes (MWNTs) containing Fe₃O₄ nanoparticles (NPs) were synthesized by a two-step method. First, we synthesized monodispersed Fe₃O₄ NPs (d=17.6 nm, σ=1.92 nm) on the surface of MWNTs and then decorated the nanocomposites with a PANI layer via a self-assembly method. SEM and TEM images indicated that the obtained samples had the morphologies of nanotubes. The molecular structure and composition of MWNTs/Fe₃O₄ NPs/PANI nanotubes were characterized by Fourier transform infrared spectra (FTIR), energy dispersive X-ray spectrometry (EDX), X-ray photoelectron spectra (XPS), X-ray diffraction (XRD) and Raman spectra. UV-vis spectra confirmed the existence of PANI and its response to acid and alkali. As a multifunctional material, the conductivity and magnetic properties of MWNTs/Fe₃O₄ NPs/PANI composites nanotubes were also investigated.     

Superparamagnetic POT/Fe3O4 nanoparticle composites with supported Au nanoparticles as recyclable high-performance nanocatalysts

A novel method has been developed to successfully synthesize Fe₃O₄ nanoparticles with tunable size and morphology supported on shells of poly(o-Toluidine)(POT) hollow microspheres. The as-prepared POT/Fe₃O₄ nanoparticle composites can be used as novel and magnetic-responsive catalyst supports to produce highly efficient and recyclable noble metal catalysts. The size of Fe₃O₄ nanoparticles supported on shells of POT hollow microspheres can be tuned from 4 to 12 nm by changing the concentration of Fe ions. The roles of the doping acid of POT and Zeta potentials of Fe₃O₄ nanoparticles and POT in the formation of the POT/Fe₃O₄ nanoparticle composites were discussed. Furthermore, gold nanoparticles that were supported on the as-synthesized POT/Fe₃O₄ nanoparticle composites have been achieved by utilizing the reactivity of POT towards Au ions. The size of gold nanoparticles can be tuned by altering the concentration of HAuCl₄. Finally, the catalytic activity of the obtained POT/Fe₃O₄/Au composites for 4-nitrophenol (4NP) reduction is investigated. The results demonstrate that such magnetic-responsive polymer-supported gold nanoparticles can be easily recovered and reused five times still remains high catalytic performance, which indicate their potential applications in the field of catalysis.     

基于Li_(0.35)Zn_(0.3)Fe_(2.35)O_4和碳纳米纤维双层吸波体的结构设计与吸收性能研究

通过静电纺丝技术和热处理制备了Li0.35Zn0.3Fe2.35O4纳米纤维和碳纳米纤维,并将它们各自均匀分散在硅橡胶基质中,测量了相应复合体在2~18 GHz频率范围内的相对复介电常数和复磁导率,并根据传输线理论评估了由它们所构成的单层和双层结构吸波体的微波吸收特性。结果显示由于Li0.35Zn0.3Fe2.35O4纳米纤维与碳纳米纤维的电磁特性的有机结合,双层吸波体的微波吸收性能明显优于同厚度的单层吸波体。当以厚为1.8 mm的Li0.35Zn0.3Fe2.35O4纳米纤维/硅橡胶复合体为吸收层和厚为0.2mm的碳纳米纤维/硅橡胶复合体为匹配层时,双层吸波体的反射率在13.9 GHz达到一个最小值-47.8 dB,反射率低于-10 dB的吸收带宽为8.8 GHz,频率范围为9.2~18 GHz,反射率小于-20 dB的频率范围为11.5~18 GHz,带宽为6.5 GHz,覆盖整个Ku波段。优化设计的双层吸波体有望作为一种轻质高效的Ku波段微波吸收材料。     

基于Li0.35Zn0.3Fe2.35O4和碳纳米纤维双层吸波体的结构设计与吸收性能研究

通过静电纺丝技术和热处理制备了Li_0.35Zn_0.3Fe_2.35O₄纳米纤维和碳纳米纤维,并将它们各自均匀分散在硅橡胶基质中,测量了相应复合体在2~18GHz频率范围内的相对复介电常数和复磁导率,并根据传输线理论评估了由它们所构成的单层和双层结构吸波体的微波吸收特性。结果显示由于Li_0.35Zn_0.3Fe_2.35O₄纳米纤维与碳纳米纤维的电磁特性的有机结合,双层吸波体的微波吸收性能明显优于同厚度的单层吸波体。当以厚为1.8mm的Li_0.35Zn_0.3Fe_2.35O₄纳米纤维/硅橡胶复合体为吸收层和厚为0.2mm的碳纳米纤维/硅橡胶复合体为匹配层时,双层吸波体的反射率在13.9GHz达到一个最小值-47.8dB,反射率低于-10dB的吸收带宽为8.8GHz,频率范围为9.2~18GHz,反射率小于-20dB的频率范围为11.5~18GHz,带宽为6.5GHz,覆盖整个Ku波段。优化设计的双层吸波体有望作为一种轻质高效的Ku波段微波吸收材料。     

纳米Fe_3O_4及钴离子掺杂Fe_3O_4:有机碱共沉淀制备和磁性质

以有机碱四甲基氢氧化铵(TMAH)为沉淀剂合成了纳米Fe3O4和Co2+掺杂的纳米Fe3O4粒子。分别讨论了碱用量,铁盐溶液浓度,反应温度,有机碱及PEG-4000的分散性等因素对纳米Fe3O4的形貌影响。结果表明,所合成的纳米Fe3O4为30nm左右的反尖晶石型面心立方结构,有机碱除了起沉淀剂作用,还能够提高纳米Fe3O4的分散性。本文还讨论了不同Co2+掺入量的纳米Fe3O4粒子的磁性质,结果表明Co2+掺杂的纳米Fe3O4粒子的矫顽力在不同掺入量的下有较大的改变。当Co2+掺入量为10.0%时,纳米Fe3O4的矫顽力达到最大值,为1628Oe。     

聚乙二醇-四氧化三铁纳米粒子复合材料的结构、物理性质及应用

在β-环糊精作保护剂条件下, 制备了高对称的十八面体四氧化三铁(Fe₃O₄)纳米材料. 通过胶体化学方法, 合成了一系列不同起始计量比的聚乙二醇(PEG)和Fe₃O₄纳米粒子复合物(CM-1-CM-4). 这些PEG复合材料展示出重要特性: 首先, 它们的表面形貌依赖于Fe₃O₄的计量; 其次, PEG的熔化过程受Fe₃O₄的影响, 并且直接与Fe₃O₄的含量相关; 进一步研究表明, 除CM-4外, Fe₃O₄的引入导致PEG结晶度下降, 而且Fe₃O₄纳米粒子量越少, 降低幅度越大; 更为有趣的是, PEG的降解过程受制于Fe₃O₄纳米粒子的影响, 导致不同降解产物的出现; 而且, 与纯Fe₃O₄纳米粒子一样, 复合材料中的Fe₃O₄也显示典型的软铁磁性行为, 但饱和磁化强度相对较小; 此外, X射线光电子能谱(XPS)实验揭示在这些PEG复合材料中, 有从Fe到O的电子转移, Fe电子密度的降低可用来解释复合材料饱和磁化强度的减小; 最后, 这些PEG复合材料呈现出对有机染料的表面增强拉曼效应, 并且这种效应随Fe₃O₄纳米粒子含量的增加而增加. 这些结果将会对聚合物/无机纳米粒子复合材料的发展起到推进作用.     

A facile two-step modifying process for preparation of poly(SStNa)-grafted Fe3O4/SiO2 particles

This article reports the synthesis of the poly(sodium 4-styrenesulfonate)-grafted Fe₃O₄/SiO₂ particles via two steps. The first step involved magnetite nanoparticles (Fe₃O₄) homogeneously incorporated into silica spheres using the modified Stöber method. Second, the modified silica-coated Fe₃O₄ nanoparticles were covered with the outer shell of anionic polyelectrolyte by surface-initiated atom transfer radical polymerization. The resulted composites were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive microscopy (EDS), Fourier transform-infrared (FT-IR), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and vibration sample magnetometer (VSM). The XRD results indicated that the surface modified Fe₃O₄ nanoparticles did not lead to phase change compared with the pure Fe₃O₄. TEM studies revealed nanoparticles remained monodisperse. The detection of sulfur and sodium signals was a convincing evidence that sodium 4-styrenesulfonate was grafted onto the surface of the magnetic silica in XPS analysis. Finally, super-paramagnetic properties of the composite particles, and the ease of modifying the surfaces may make the composites of important use in mild separation, enzyme immobilization, etc.     

Fabricating and Tailoring Polyaniline (PANI) Nanofibers with High Aspect Ratio in a Low‐Acid Environment in a Magnetic Field

In a 0.010 m HCl solution, we successfully transformed irregular polyaniline (PANI) agglomerates into uniform PANI nanofibers with a diameter of 46–145 nm and a characteristic length on the order of several microns by the addition of superparamagnetic Fe₃O₄ microspheres in a magnetic field. The PANI morphological evolution showed that the PANI nanofibers stemmed from the PANI coating shell synthesized on the surface of the Fe₃O₄ microsphere chains. It was found that the magnetic field could optimize the PANI nanofibers with a narrow diameter size distribution, and effectively suppressed secondary growth. When compared with other microspheres (like silica and polystyrene), only the use of superparamagnetic Fe₃O₄ microspheres resulted in the appearance of PANI nanofibers. Attempts to form these high‐quality PANI nanofibers in other concentrations of HCl solution were unsuccessful. This deficiency was largely attributed to the inappropriate quantity of aniline cations.     

One-pot sequential synthesis of magnetically separable Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>/AgCl photocatalysts with enhanced activity and stability

Magnetically separable Fe₃O₄/AgCl photocatalysts were prepared by a one-pot sequential method. A series of techniques proved the hybrid structure of Fe₃O₄/AgCl composites. Fe₃O₄/AgCl composites had a much higher photocatalytic activity toward Rhodamine B (RhB) degradation than pure AgCl under the simulated solar light irradiation. The existence of metal Ag resulted in high photocatalytic activity of Fe₃O₄/AgCl, which was related with the amount of metallic Ag. The scavenging experiments showed that the degradation reaction most probably was initiated by the photoinduced single-electron transfer, and the generation of superoxide anion (O ₂ ^-· ) played a significant role. The composite photocatalysts could be recycled by applying an external magnetic field, and the reused composites maintained their original photocatalytic activity. Fe₃O₄/AgCl composites were highly efficient, magnetically separable, and recoverable. This proves their potential applications in the photodegradation of organic pollutants.     

Development of Fe3O4-poly(l-lactide) magnetic microparticles in supercritical CO2

The Fe₃O₄-poly(l-lactide) (Fe₃O₄-PLLA) magnetic microparticles were successfully prepared in a process of solution-enhanced dispersion by supercritical CO₂ (SEDS), and their morphology, particle size, magnetic mass content, surface atom distribution and magnetic properties were characterized. Indomethacin (Indo) was used as a drug model to produce drug-polymer magnetic composite microparticles. The resulting Fe₃O₄-PLLA microparticles with mean size of 803 nm had good magnetic property and a saturation magnetization of 24.99 emu/g. The X-ray photoelectron spectroscopy (XPS) test indicated that most of the Fe₃O₄ were encapsulated by PLLA, which indicated that the Fe₃O₄-PLLA magnetic microparticles had a core–shell structure. After further loading with drug, the Indo-Fe₃O₄-PLLA microparticles had a bigger mean size of 901 nm, and the Fourier transform infrared spectrometer (FTIR) analysis demonstrated that the SEDS process was a typical physical coating process to produce drug-polymer magnetic composite microparticles, which is favorable for drugs since there is no change in chemistry. The in vitro cytotoxicity test showed that the Fe₃O₄-PLLA magnetic microparticles had no cytotoxicity and were biocompatible, which means there is potential for biomedical application.     

Constructing magnetic Fe3O4‐Au@CeO2 hybrid nanofibers for selective catalytic degradation of organic dyes

Au nanoparticles (Au NPs) play a vital role in heterogeneous catalytic reactions. However, pristine Au NPs usually suffer from poor selectivity and difficult recyclability. In this work, Fe₃O₄‐Au@CeO₂ hybrid nanofibers were prepared via a simple one‐pot redox reaction between HAuCl₄ and Ce (NO₃)₃ in the presence of Fe₃O₄ nanofibers. CeO₂ shell was uniformly coated on the surface of Fe₃O₄ nanofibers to form a unique core‐shell structure, while Au NPs were encapsulated inside the CeO₂ shell. The as‐prepared Fe₃O₄‐Au@CeO₂ hybrid nanofibers have been proved to be positively surface charged due to the formation of CeO₂ shell, enabling them to be good candidates for predominant selective catalytic activity towards the degradation of negatively charged organic dyes. In addition, the Fe₃O₄‐Au@CeO₂ hybrid nanofibers showed magnetic properties, offering them excellent recyclable usability. This work presents a facile and effective solution to prepare magnetic noble metal/metal oxide hybrid nanomaterials with unique chemical structure and surface characteristic for promising applications in heterogeneous catalysis.     

Superparamagnetic Polymer Emulsion Particles from a Soap-Free Seeded Emulsion Polymerization and their Application for Lipase Immobilization

Using emulsion copolymer of styrene (St), glycidyl methacrylate (GMA) and 2-hydroxyethyl methacrylate (HEMA) as seed latexes, the superparamagnetic polymer emulsion particles were prepared by seeded emulsion copolymerization of butyl methacrylate (BMA), vinyl acetate (VAc) and ethylene glycol dimethacrylate in the presence of the seed latexes and superparamagnetic Fe₃O₄/SiOx nanoparticles (or Fe₃O₄-APTS nanoparticles) through a two-step process, without addition of any emulsifier. The magnetic emulsion particles named P(St-GMA-HEMA)/P(BMA-VAc) were characterized by transmission electron microscope and vibrating sample magnetometry. The results showed that the magnetic emulsion particles held a structure with a thinner shell (around 100 nm) and a bigger cavity (around 200 nm), and possessed a certain level of magnetic response. The resulting magnetic emulsion particles were employed in the immobilization of lipase by two strategies to immobilized lipase onto the resulting magnetic composites directly (S-1) or using glutaraldehyde as a coupling agent (S-2), thus, experimental data showed that the thermal stability and reusability of immobilized lipase based on S-2 were higher than that of S-1.