Iron phthalocyanine oligomer/Fe3O4 hybrid microspheres and their microwave absorption property

The novel nano-scale iron phthalocyanine oligomer/Fe₃O₄ (FePc/Fe₃O₄) hybrid microspheres were synthesized from iron phthalocyanine oligomer and FeCl₃·6H₂O via a solvent-thermal crystallization route. The morphology and structure of the hybrid microspheres were characterized by Fourier transform infrared spectrophotometer, X-ray diffraction, scanning electron microscopy and transmission electron microscopy. These results showed that the hybrids were monodisperse microspheres and the morphology can be adjusted by controlling pre-polymerization time. The saturation magnetization increased with increase in the pre-polymerization time, while the coercivities decreased. The FePc/Fe₃O₄ hybrid microspheres exhibited novel microwave electromagnetic properties: the dielectric loss was enhanced when the pre-polymerization time increased and a new microwave loss peak appeared at high frequency. The microwave absorbing properties enhanced with increase in the pre-polymerization time and a maximum reflection loss of −29.7 dB was obtained at 11.7 GHz with 6 h of pre-polymerization time when the matching thickness was 3.0 mm. The novel hybrid materials are believed to have potential applications as microwave absorbing materials.     

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.     

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.     

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.     

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.     

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.     

Adjustable microwave absorption properties of flake shaped (Ni0.5Zn0.5)Fe2O4/Co nanocomposites with stress induced orientation

Flake shaped (Ni_0.5Zn_0.5)Fe₂O₄/Co nanocomposites were successfully fabricated by co-precipitating of Ni-Zn ferrite on the surface of cobalt nanoflakes. The electromagnetic characteristics of the samples were studied at the frequency of 0.1–14 GHz. The results showed that the cobalt nanoflakes in compacted nanocomposites were well orientated, and the nanocomposites were characterized with low optimal reflection loss (RL) of −33.8 dB at 11.5 GHz and broad RL bandwidth for <−20 dB in the frequency range of 7.6–12.1 GHz. At the same time, the position of the absorptive band can be adjusted by changing the mass ratio of ferrite to cobalt in the nanocomposites. It is proposed that the excellent microwave absorption properties are related to the combination of strong shape anisotropy of cobalt nanoflakes and adjustable dielectric loss.     

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.     

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.     

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.     

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.     

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.     

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.     

The electrochemical preparation and microwave absorption properties of magnetic carbon fibers coated with Fe3O4 films

Electrodeposition was employed to fabricate magnetite (Fe₃O₄) coated carbon fibers (MCCFs). Temperature and fiber surface pretreatment had a significant influence on the composition and morphology of Fe₃O₄ films. Uniform and compact Fe₃O₄ films were fabricated at 75 °C on both nitric acid treated and untreated carbon fibers, while the films prepared at 60 °C were continuous and rough. Microwave measurements of MCCF/paraffin composites (50 wt.% of MCCFs, pretreated carbon fibers as deposition substrates) were carried out in the 2-18 GHz frequency range. MCCFs prepared at 60 °C obtained a much higher loss factor than that prepared at 75 °C. However, the calculation results of reflection loss were very abnormal that MCCFs prepared at 60 °C almost had no absorption property. While MCCFs prepared at 75 °C exhibited a good absorption property and obtained −10 dB and −20 dB refection loss in wide matching thickness ranges (1.0-6.0 mm and 1.7-6.0 mm range, respectively). A secondary attenuation peak could also be observed when the thickness of MCCF/paraffin composite exceeded 4.0 mm. The minimum reflection loss was lower.     

Magnetic and Microwave Absorbing Properties of Electrospun Ba(1−x)LaxFe12O19 Nanofibers

Ba_(1−x)La_xFe₁₂O₁₉ (0.00≤x≤0.10) nanofibers were fabricated via the electrospinning technique followed by heat treatment at different temperatures for 2 h. Various characterization methods including scanning electron microscopy (SEM), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), and microwave vector network analyzer were employed to investigate the morphologies, crystalline phases, magnetic properties, and complex electromagnetic parameters of nanofibers. The SEM images indicate that samples with various values of x are of a continuous fiber-like morphology with an average diameter of 110±20 nm. The XRD patterns show that the main phase is M-type barium hexaferrite without other impurity phases when calcined at 1100 °C. The VSM results show that coercive force (H_c) decreases first and then increases, while saturation magnetization (M_s) reveals an increase at first and then decreases with La³⁺ ions content increase. Both the magnetic and dielectric losses are significantly enhanced by partial substitution of La³⁺ for Ba²⁺ in the M-type barium hexaferrites. The microwave absorption performance of Ba_0.95La_0.05Fe₁₂O₁₉ nanofibers gets significant improvement: The bandwidth below −10 dB expands from 0 GHz to 12.6 GHz, and the peak value of reflection loss decreases from −9.65 dB to −23.02 dB with the layer thickness of 2.0 mm.     

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.     

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.     

Static and dynamic magnetic characteristics of BaCo0.5Mn0.5Ti1.0Fe10O19

The effect of Mn²⁺Co²⁺Ti⁴⁺ substitution on microwave absorption has been studied for BaCo_0.5Mn_0.5Ti_1.0Fe₁₀O₁₉ ferrite-acrylic resin composites in frequency range from 12 to 20 GHz. X-ray diffraction (XRD), scanning electron microscope (SEM), vibrating sample magnetometer, AC susceptometer and vector network analyzer were used to analyze the structural, magnetic and microwave absorption properties. The results showed that the magnetoplumbite structures for all samples have been formed. Based on microwave measurement on reflectivity, BaCo_0.5Mn_0.5Ti_1.0Fe₁₀O₁₉ may be a good candidate for electromagnetic compatibility and other practical applications at high frequency.     

Magnetic and microwave absorption properties of BaFe12−x (Mn0.5Cu0.5Zr)x/2O19 synthesized by sol–gel processing

BaFe_12−x (Mn_0.5Cu_0.5Zr)_x/2O₁₉ hexaferrites with x=1, 2 and 3 were prepared by sol–gel process. The ferrite powders possess hexagonal shape and are well separated from one another. The powders of these ferrites were mixed with polyvinylchloride (PVC) plasticizer to be converted into a microwave absorbing composite ferrite with a thickness of 1.8 mm. X-ray diffractometer (XRD), scanning electron microscope (SEM), ac susceptometer, vibrating sample magnetometer and vector network analyzer were used to analyze its structure, electromagnetic and microwave absorption properties. The results showed that magnetoplumbite structures for all samples were formed. The sample with higher magnetic susceptibility and coercivity exhibits a larger microwave absorbing ability. Also the present investigation demonstrates that a microwave absorber using BaFe_12−x(Mn_0.5Cu_0.5Zr)_x/2O₁₉ (x=2 and 3)/PVC with a matching thickness of 1.8 mm can be fabricated for applications over 15 GHz, with reflection loss more than −25 dB for specific frequencies, by controlling the molar ratio of the substituted ions.     

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.