Preparation and microwave absorption properties of Fe-phthalocyanine oligomer/Fe3O4 hybrid microspheres

The novel nano-scale Fe-phthalocyanine oligomer/Fe₃O₄ hybrid microspheres were synthesized from bis-phthalonitrile and FeCl₃·6H₂O through a simple solvent-thermal route. The morphology and structure of the hybrid microspheres were characterized by FTIR, XRD, SEM and TEM. These results showed that the hybrids were monodispersed solid microspheres and the morphology can be adjusted by controlling the addition of bis-phthalonitrile. On the basis of these results, the formation process was discussed. Magnetization measurement indicated that saturation magnetizations decreased linearly with increasing the addition of bis-phthalonitrile, while coercivities increased. The microwave absorption properties were measured by a vector network analyzer. The dielectric loss of the hybrid microspheres was larger and a new magnetic loss peak appeared at high frequency. The microwave absorbing properties enhanced with increasing the addition of bis-phthalonitrile and a maximum reflection loss of −31.1 dB was obtained at 8.6 GHz with 1 g bis-phthalonitrile when the matching thickness was 3.0 mm. The novel hybrid materials are believed to have potential applications in the microwave absorbing performances.     

Only Ku-band microwave absorption by Fe3O4/ferrocenyl-CuPc hybrid nanospheres

A novel kind of hybrid nanospheres made of Fe₃O₄ and ferrocenyl-CuPc (FCP) was prepared via effective solvothermal method and performed microwave absorptivity only in Ku-band with minimum reflection loss of −25 dB at 16.0 GHz corresponding to absorbing about 99.7% content of microwave. Scanning electron microscopy images indicated that the nanospheres with uniform particle size distribution have the average diameter of 135 nm. Due to the synergistic reaction between magnetic ferrocenyl-CuPc and Fe₃O₄, the hybrid nanospheres showed novel electromagnetic properties. The real part of complex permittivity of hybrid nanospheres remains stable in the range of 0.5–12.0 GHz and has a large fluctuation at 16.5 GHz. Moreover, the dielectric loss of hybrid nanospheres also appeared a sharp peak at 16.3 GHz with the value of 2.7. The specific gravity of hybrid nanospheres is about 2.08. On the basis of these results, the novel hybrids are believed to have potential applications in the microwave absorbing area in Ku-band.     

One-step preparation of organometal/Fe3O4 hybrid microspheres and their electromagnetic properties

Novel organometal/Fe₃O₄ hybrid microspheres were prepared from bisphthalonitrile-benzoxine resin containing ferrocene (FPNBZ) and FeCl₃·6H₂O via a one-step solvent-thermal method. The phase structure, composition and morphology of as-prepared hybrid microspheres were characterized by X-ray powder diffraction, Fourier transform infrared spectrophotometer and scanning electron microscopy. The results revealed that crystallinity, dispersity and size of hybrid microspheres can be controlled by altering the reaction parameters. Density measurement showed that the density is decreased with increasing FPNBZ concentration in the hybrid materials. Electromagnetic properties of the FPNBZ/Fe₃O₄ hybrid microspheres were measured at 2-18 GHz. The electromagnetic measurement indicated that the resonance peaks of complex permittivity, complex permeability, dielectric loss and magnetic loss were shifted to the high frequencies, with the increasing amount of FPNBZ. The as-prepared hybrid materials are believed to have broad applications both in microwave absorption materials in a wide frequency range and in biomedical fields.     

Electromagnetic and microwave absorption properties of carbonyl iron/La0.6Sr0.4MnO3 composites

In this work carbonyl iron/La_0.6Sr_0.4MnO₃ composites were prepared to develop super-thin microwave absorbing materials. The complex permittivity, permeability and microwave absorption properties are investigated in the frequency range of 8-12 GHz. An optimal reflection loss of −12.4 dB is reached at 10.5 GHz with a matching thickness of 0.8 mm. The thickness of carbonyl iron/La_0.6Sr_0.4MnO₃ absorber is thinner, compared with conventional carbonyl iron powders with the same absorption properties. The bandwidth with a reflection loss exceeding −7.4 dB is obtained in the whole measured frequency range with the thickness of 0.8 mm. The excellent microwave absorption properties are attributed to a better electromagnetic matching established by the combination of the enhanced dielectric loss and nearly invariable magnetic loss with the addition of La_0.6Sr_0.4MnO₃ nanoparticles in the composites. Our work indicates that carbonyl iron/La_0.6Sr_0.4MnO₃ composites may have an important application in wide-band and super-thin electromagnetic absorbers in the frequency range of 8−12 GHz.     

Preparation and dual microwave-absorption properties of carboxylic poly(arylene ether nitrile)/Fe3O4 hybrid microspheres

The carboxylic poly(arylene ether nitrile)/Fe₃O₄ hybrid microspheres were prepared via solvothermal method. The carboxylic poly(arylene ether nitrile) (PEN-COOH) was introduced into the Fe₃O₄ microspheres by chemisorption with mass content up to 15% as defined by infrared spectra and thermal gravimetric analysis. The hybrid sphere is of hierarchical polymer-inorganic microstructure as observed by transmission electron microscopy. The microwave-absorption of the sample owns a shifting peak and a special immobilized peak with the variation of absorber thickness from 3 to 5 mm. Maximum microwave-absorption of the product is capable of over −30 dB in the range of 10-12 GHz. By proposed equivalent filter circuit model, the immobilized peak was attributed to the ordered nanostructure where the Fe₃O₄ nanocrystals were isolated by PEN-COOH. The product has the potential to be applied as microwave absorber with high microwave-absorption, good dispersibility and robust polymer-inorganic interfacial adherence.     

Magnetic and rheological properties of monodisperse Fe3O4 nanoparticle/organic hybrid

Fe₃O₄ nanoparticle/organic hybrids were synthesized via hydrolysis using iron (III) acetylacetonate at ∼80 °C. The synthesis of Fe₃O₄ was confirmed by X-ray diffraction, selected-area diffraction, and X-ray photoelectron spectroscopy. Fe₃O₄ nanoparticles in the organic matrix had diameters ranging from 7 to 13 nm depending on the conditions of hydrolysis. The saturation magnetization of the hybrid increased with an increase in the particle size. When the hybrid contained Fe₃O₄ particles with a size of less than 10 nm, it exhibited superparamagnetic behavior. The blocking temperature of the hybrid containing Fe₃O₄ particles with a size of 7.3 nm was 200 K, and it increased to 310 K as the particle size increased to 9.1 nm. A hybrid containing Fe₃O₄ particles of size greater than 10 nm was ferrimagnetic, and underwent Verwey transition at 130 K. Under a magnetic field, a suspension of the hybrid in silicone oil revealed the magnetorheological effect. The yield stress of the fluid was dependent on the saturation magnetization of Fe₃O₄ nanoparticles in the hybrid, the strength of the magnetic field, and the amount of the hybrid.     

Synthesis of Co-Cu-Zn doped Fe3O4 nanoparticles with tunable morphology and magnetic properties

Co-Cu-Zn doped Fe₃O₄ nanoparticles can be successfully synthesized using a simple method. The particles in the size range 20−400 nm with different regular shapes i.e. sphere-like, regular hexane and tetrahedron are controllably achieved by changing the metal ion concentration. Compared to pure Fe₃O₄ without dopants, Co-Cu-Zn doped Fe₃O₄ nanoparticles exhibit better microwave absorbing properties at 2−18 GHz. Among three Co-Cu-Zn doped Fe₃O₄ nanoparticles with different morphologies, tetrahedral Co-Cu-Zn doped Fe₃O₄ nanoparticles represent a better dielectric loss in high frequency range. This work is believed the first known report of Co-Cu-Zn doped Fe₃O₄ nanoparticles with tunable morphology and magnetic properties through the hydrothermal process without using any organic solvents, organic metal salts or surfactants.     

Preparation of pyrrole with iron oxide precipitated on the surface of graphite nanosheet

Fe₃O₄/NanoG was firstly prepared by precipitation reaction of iron oxide (Fe₃O₄) on the surface of graphite nanosheet (NanoG). Then composites PPy/NanoG, PPy/Fe₃O₄ and PPy/Fe₃O₄/NanoG were prepared by in-situ polymerization of the monomer pyrrole polymerized on the surface of NanoG, Fe₃O₄ and Fe₃O₄/NanoG. The structures of Fe₃O₄/NanoG, PPy, PPy/NanoG, PPy/Fe₃O₄ and PPy/Fe₃O₄/NanoG were characterized by scanning electron microscopy, energy dispersive spectroscopy, fourier transmission infrared spectroscopy and X-ray diffraction . Results show that NanoG and Fe₃O₄/NanoG are encapsulated by PPy for the layered structure and their high aspect ratio (300–500). From the thermogravimetric analysis it can be seen that the introductions of NanoG, Fe₃O₄ and Fe₃O₄/NanoG into PPy based composites lead them to exhibit better thermal stabilities than pure PPy. The measurements of electromagnetic parameters show that the reflection loss of PPy/Fe₃O₄/NanoG is below −15 dB at the X band (8.2–12.4 GHz) and the minimum loss value is −18.30 dB at 9.84 GHz, while the reflection loss of PPy/Fe₃O₄ is below −10 dB at 8.2–12.4 GHz and the minimum loss value is −14.02 dB at 10.26 GHz. The reflection loss of PPy/NanoG is below −10 dB at 8.2–12.4 GHz and the minimum loss value is −13.44 dB at 10.28 GHz. The microwave absorbing properties of PPy/Fe₃O₄/NanoG, PPy/Fe₃O₄ and PPy/NanoG are superior to that of PPy.     

The microwave absorption properties of La0.8Sr0.2Mn1−yFeyO3 nanocrystalline powders in the frequency range 2-18 GHz

La_1−xSr_xMn_1−yFe_yO₃ nanocrystalline powders were prepared by the sol-gel method as a microwave absorption material. The reflectance, the dielectric loss tan δ_e and the magnetic loss tan δ_m of the samples were calculated according to the data of electromagnetism parameters measured by a microwave vector network analyzer in the frequency range 2-18 GHz. The dielectric loss tan δ_e and the magnetic loss tan δ_m had a step-change at a certain frequency so that the superiority of dielectric loss change into the superiority of magnetic loss, which indicated that anti-ferromagnetic clusters in the material change into ferromagnetic clusters by absorbing quantum of microwave electromagnetic field when the frequency of incident microwave reaches a certain value. The effective absorption bandwidth higher than 10 dB reached 6.2 GHz. As a result, the La_0.8Sr_0.2Mn_1−yFe_yO₃ has shown useful applications as a microwave absorption material.     

Microwave dielectric and magnetic properties of superparamagnetic 8-nm Fe3O4 nanoparticles

The superparamagnetic 8-nm Fe₃O₄ nanoparticles were successfully prepared by chemical oxidation process. For the complex permittivity, the dual dielectric relaxation processes have been proved by two overlapped Cole–Cole semicircles, and the natural resonance frequency is 3.03 GHz for the complex permeability. The maximum reflection loss value reaches −55.5 dB at 6.11 GHz with 3.85 mm in the thickness of the absorbers for the superparamagnetic 8-nm Fe₃O₄ nanoparticles which is better than that of 150 nm and 30 nm Fe₃O₄ nanoparticles. It is believed that the superparamagnetic 8-nm Fe₃O₄ nanoparticles can be used as a kind of candidate for microwave absorber.     

Preparation and microwave absorption properties of loose nanoscale Fe3O4 spheres

Magnetite nanoparticles are found to assemble into randomly dispersed loose nanoscale spheres with diameters ∼300 nm in ethylene glycol in the presence of polyethylene and a small quantity of polyethyleneimine. Modern analysis methods are employed to provide structure information of the magnetic loose spheres. The ferromagnetic saturation magnetization is ∼80.0 emu g⁻¹, and the coercive force is 209 Oe. The microwave electromagnetic parameters are measured by a vector network analyzer. The synthesized loose spheres exhibit novel microwave properties compared with the conventional Fe₃O₄ nanoparticles. An additional microwave loss peak appears in the Ku band, which is attributed to the loose structure.     

Synthesis, infrared and microwave absorbing properties of (BaFe12O19+BaTiO3)/polyaniline composite

The (BaFe₁₂O₁₉+BaTiO₃)/polyaniline composite was synthesized by in situ polymerization and introduced into epoxy resin and polyethylene to be a microwave and infrared absorber. The spectroscopic characterizations of the formation processes of (BaFe₁₂O₁₉+BaTiO₃)/polyaniline composite were examined using Fourier transform infrared, ultraviolet-visible spectrophotometer, X-ray diffraction, scanning electron microscopy, transmission electron microscopy and electron spin resonance. Microwave absorbing properties were investigated by measuring reflection loss in 2-18 and 18-40 GHz microwave frequency range using the free space method. Thermal extinction measurements in the 3-5 and 8-12 μm were done to evaluate the shielding effectivity of infrared. The results showed that a significant absorption frequency range shifting and thermal extinction could be obtained by adding polyaniline to the BaFe₁₂O₁₉+BaTiO₃ blend.     

Electromagnetic and microwave absorption properties of Fe3O4 magnetic films plated on hollow glass spheres

Magnetic hollow spheres of low density were prepared by plating Fe₃O₄ magnetic films on hollow glass spheres using ferrite plating. The complex permeability and permittivity of spheres–wax composites were measured in the range of 2–18 GHz. The complex permeability and permittivity increased, and the dielectric and magnetic losses were improved as the volume fraction of the magnetic spheres in the composites increased from 60% to 80%, which also resulted in a great improvement of microwave absorption properties. For composites with volume fraction 80%, its magnetic resonance frequency was at about 13 GHz and it appeared three loss peaks in the calculated reflection loss curves; the bandwidth less than −10 dB was almost 4 GHz which was just in the Ku-band frequencies (12–18 GHz) and a minimum reflection loss of −20 dB was obtained when the thickness was 2.6 mm; the microwave absorbing properties were mainly due to the magnetic loss. The results showed that the magnetic spheres composites were good and light microwave absorbers in the Ku-band frequencies.     

Microwave sintering of high-permeability (Ni0.20Zn0.60Cu0.20)Fe1.98O4 ferrite at low sintering temperatures

The (Ni_0.20Zn_0.60Cu_0.20)Fe_1.98O₄ ferrite was sintered using microwave sintering and conventional sintering technique, respectively. It was found that microwave sintering technique can effectively promote the forward diffusion of ions and thus accelerate the sintering process, resulting in the grain growth and the densification of matrix. At the low frequency of 100 kHz, the magnetizing contribution of domain wall motion is predominant, and compact and coarse matrixes are favorable for domain wall motion, giving rise to improvement of relative initial permeability and loss of ferrites. Using microwave sintering technique, for the (Ni_0.20Zn_0.60Cu_0.20)Fe_1.98O₄ ferrite, the relative initial permeability μ_i of about 2000 and the relative loss factor tanδ/μ_i of about 8.7×10⁻⁶ at 100 kHz were achieved at only 980 °C sintering temperature. In addition, the sintering time of ferrites was reduced from 5 to 0.5 h by using microwave sintering technique.     

Magnetism and thermal induced characteristics of Fe2O3 content bioceramics

Magnetic properties of Li₂O–MnO₂–CaO–P₂O₅–SiO₂ (LMCPS) glasses doped with various amounts of Fe₂O₃ were investigated. There is a dramatic change in the magnetic property of pristine LMCPS after the addition of Fe₂O₃ and crystallized at 850 °C for 4 h. Both the electron paramagnetic resonance and magnetic susceptibility measurements showed that the glass ceramic with 4 at% Fe₂O₃ exhibited the coexistence of superparamagnetism and ferromagnetism at room temperature. When the Fe₂O₃ content was higher than 8 at%, the LMCPS glasses showed ferromagnetism behavior. The complex magnetic behavior is due to the distribution of (Li, Mn)ferrite particle sizes driven by the Fe₂O₃ content. The thermal induced hysteresis loss of the crystallized LMCPS glass ceramics was characterized under an alternating magnetic field. The energy dissipations of the crystallized LMCPS glass ceramics were determined by the concentration and Mn/Fe ratios of Li(Mn, Fe)ferrite phase formed in the glass ceramics.     

Microwave anneal effect on magnetic properties of Ni0.6Zn0.4Fe2O4 nano-particles prepared by conventional hydrothermal method

Ni_0.6Zn_0.4Fe₂O₄ ferrite nano-particles with a crystallite size of about 20 nm were prepared by the conventional hydrothermal method, followed by annealing in a microwave oven for 7.5-15 min. The microstructure and magnetic properties of the samples were characterized by scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy and vibrating sample magnetometry. The microwave annealing process has slight effect on the morphology and size of Ni_0.6Zn_0.4Fe₂O₄ ferrite nano-particles. However it reduces the lattice parameter and enhances the densification of the particles, and then greatly increases the saturation magnetization (50-56 emu/g) and coercive force of the samples as compared to the non-annealing condition. The microwave annealing process is an effective way to rapidly synthesize high performance ferrite nano-particle.     

Synthesis of (Mg0.476Mn0.448Zn0.007)(Fe1.997Ti0.002)O4 powder and sintered ferrites by high energy ball-milling process

(Mg_0.476Mn_0.448Zn_0.007)(Fe_1.997Ti_0.002)O₄ nanocrystalline powder prepared by high energy ball-milling process were consolidated by microwave and conventional sintering processes. Phases, microstructure and magnetic properties of the ferrites prepared by different processes were investigated. The (Mg_0.476Mn_0.448Zn_0.007)(Fe_1.997Ti_0.002)O₄ nanocrystalline powder could be prepared by high energy ball-milling process of raw Fe₃O₄, MnO₂, ZnO, TiO₂ and MgO powders. Prefired and microwave sintered ferrites could achieve the maximum density (4.86 g/cm⁻³), the average grain size (15 μm) was larger than that (10 μm) prepared by prefired and conventionally sintered ferrites with pure ferrite phase, and the saturation magnetization (66.77 emu/g) was lower than that of prefired and conventionally sintered ferrites (88.25 emu/g), the remanent magnetization (0.7367 emu/g) was higher than that of prefired and conventionally sintered ferrites (0.0731 emu/g). Although the microwave sintering process could increase the density of ferrites, the saturation magnetization of ferrites was decreased and the remanent magnetization of ferrites was also increased.     

Synthesis of magnetic and lightweight hollow microspheres/polyaniline/Fe3O4 composite in one-step method

After hollow microspheres (HM) were surface modified, a layer of electromagnetic polyaniline/Fe₃O₄ composite (PAN/Fe₃O₄) was successfully grafted onto the surface of the self-assembled monolayer coated HM, resulting in HM/PAN/Fe₃O₄ composites. In this approach, γ-aminopropyltriethoxy silane was adopted to form a well-coating monolayer with amino groups for the graft polymerization of aniline, which played an important role in fabricating the core-shell structure. FeCl₃ was used as the oxidant not only for aniline to form PAN, but also for FeCl₂ to prepare the magnets. The structure, morphologies, and magnetic properties of the as-prepared samples were characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction and vibrating sample magnetometer. The results indicated that the HM/PAN/Fe₃O₄ composites possess low density (ρ < 1.0 g/cm³), controllable morphology, and good magnetic properties at room temperature (saturation magnetization Ms = 8.32 emu g⁻¹ and coercive force Hc ≈ 0).     

Electromagnetic and microwave absorption properties of Fe–Sr0.8La0.2Fe11.8Co0.2O19 shell-core composites

Shell-core Fe–Sr_0.8La_0.2Fe_11.8Co_0.2O₁₉ composites are prepared by chemical vapor deposition (CVD) for use as microwave absorbing materials. Scanning electron microscopy and X-ray diffraction analyses show that the CVD method yields Sr_0.8La_0.2Fe_11.8Co_0.2O₁₉ powders with a uniform coating of Fe. Compared with Sr_0.8La_0.2Fe_11.8Co_0.2O₁₉, Fe–Sr_0.8La_0.2Fe_11.8Co_0.2O₁₉ composites have higher electrical conductivity, permittivity, and dielectric loss, which gradually increase with increasing Fe content. When Sr_0.8La_0.2Fe_11.8Co_0.2O₁₉/Fe=7:3, a reflection loss (RL) exceeding −10 dB is obtained in the frequency range of 10–14 GHz at a coating thickness of 2.0 mm. A minimum RL of −30 dB was found at 8.0 GHz, corresponding to a matching thickness of 2.8 mm.     

Synthesis and characterization of a novel magnetic carrier with its composition of Fe3O4/carbon using hydrothermal reaction

In this study, a simple method to prepare a novel magnetic carrier based on carbon matrix has been built by heating the aqueous solution of glucose and oleic acid-stabilized Fe₃O₄ nanoparticle at 170 °C for 3 h. The results show that the surface hydrophobic modification of Fe₃O₄ nanoparticle is necessary for the successful synthesis of Fe₃O₄/C nanocomposition, and a possible formation mechanism of Fe₃O₄/C nanocomposition was presented. The influence of the reaction parameters such as the concentration of oleic acid-stabilized Fe₃O₄ nanoparticle, the reaction time, etc. on the product was also investigated. In the typical reaction (2.5 g/L of oleic acid-stabilized Fe₃O₄ nanoparticle, 0.5 M of glucose), Fe₃O₄/C nanocompositions with the average diameter in the range 100–200 nm were obtained and its saturation is 12.4 emu/g. In order to characterize Fe₃O₄/C nanocompositions, XPS, XRD, FT–IR, and Mössbauer spectra were employed.