Synthesis, characterization, and microwave absorption properties of Fe-40 wt%Ni alloy prepared by mechanical alloying and annealing

Fe-40 wt%Ni alloys with granular shape and flake shape were prepared by a mechanical alloying (MA) and annealing method. The phase composition and morphology of the FeNi alloys, electromagnetic parameters, and microwave absorbing properties of the silicone rubber composite absorbers filled with the as-prepared FeNi alloy particles were characterized using X-ray diffraction (XRD), scanning electron microscope (SEM) and vector network analyzer. The XRD results indicate that the crystalline structures of the Fe-40 wt%Ni alloys prepared by both one-step and two-step MA processes are face-centered cubic (fcc) Ni (Fe) solid solutions, and the structures can be retained after annealing at 600 °C for 2 h. SEM images show that the FeNi alloy powders for one-step process have a granular shape; however the particles turned into flake form when they were sequentially milled with absolute ethyl alcohol. With the increase in thickness of composite absorber, the reflection loss (RL) decreases, and the peak for minimum reflection loss shifts towards the lower frequency range. Compared to the absorbers filled with the granular FeNi alloy, the absorbers filled with flaky FeNi alloys possess higher complex permittivities and permeabilities and have a lower RL and peak frequency under the same thickness. Microwave absorbing materials with a low reflection loss peak in the range of 1-4 GHz are obtained, and their microwave absorbing properties can be adjustable by changing their thicknesses.     

Influence of Cr content on structure and magnetic properties of Fe-Si-Al-Cr powders

As a kind of soft magnetic metallic material, flaky FeSiAl powders have been studied and used widely. Transition metal chromium can improve the magnetic properties of FeSiAl. This article prepared Fe₈₅Si_9.5-xAl_5.5Cr_x (x=0, 2, 4, 6 wt%) alloys powders by adding chromium to replace silicon in alloys. The morphology and microstructure of alloys powders were studied, electromagnetic parameters were measured and microwave absorption properties in the frequency range from 0.5 to 18 GHz were analyzed. With the increase of Cr content, α-Fe (Al, Si) superlattice phases appeared in alloys powders, and then disappeared. Excessive Cr precipitated from the alloys when its content reaches 6 wt%. The minimum reflection loss (-20 dB) among the four powders was 2 wt% Cr content at the frequency of 11.5 GHz. The peaks of reflection loss shifted to the low frequency range with increase in Cr content.     

Electromagnetic wave absorption properties of flaky Fe-Ti-Si-Al nanocrystalline composites

Nanocrystalline Fe-Ti-Si-Al flaky powders with large aspect ratio have been fabricated by high-energy planetary milling melt-spun ribbons. Magnetic composites made of thermally annealed Fe-Ti-Si-Al flaky powders embedded in epoxy resin exhibit excellent electromagnetic wave absorption properties in a wide frequency range from 100 MHz to 2.65 GHz. Ti additions can enhance the electrical resistivity of Fe-Si-Al alloy without changing the crystallographic structure, resulting in the reduction of eddy current loss at high frequencies. Moreover, the substitution of Ti for Fe enhances the cut-off frequency of flaky powder-polymer composites. Meanwhile, compared to the Ti-free composites, reflection loss of the Ti-doped composites (3 mm in thickness) is lower than −10 dB in the frequency range from 593 MHz to 1.83 GHz, indicating that the composites can effectively work in a wider frequency bandwidth.     

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.     

Preparation and characterization of carbonyl iron/glass composite absorber as matched load for isolator

Composite absorbers made from 66 wt% carbonyl iron and 34 wt% low melting point glass powder were prepared by a pressureless sintering technique in a nitrogen atmosphere. Apparent porosity and bending strength of the as-prepared composites were investigated. The microstructure, heat resisting properties and electromagnetic properties were characterized by scanning electron microscopy, thermal gravimetric analysis–differential scanning calorimetry and vector network analyzer. The results show that the carbonyl iron/glass composite absorbers were difficult to densify. As the sintering temperature and soaking time increased, the apparent porosity first decreased and then increased, whereas the bending strength showed the opposite change. The composite absorber sintered at 520 °C for 40 min achieved the minimum apparent porosity of 13.08% and the highest bending strength of 52 MPa. Compared to the carbonyl iron/silicone rubber absorber, the carbonyl iron/glass composite absorber exhibited better heat resisting properties, and the initial oxidation temperature was increased about 200 °C. The composite absorber with a thickness of 1.25 mm showed a good microwave absorbing property in 8–12 GHz.     

High frequency properties of composite membrane with in-plane aligned Sendust flake prepared by infiltration method

Composite membranes (with thickness around 100–200 μm) containing highly in-plane aligned Sendust flakes embedded in polyvinyl alcohol matrix were prepared with a novel infiltration method. As compared with tape-casting method, infiltration method results in enhanced magnetic permeability, which could be caused by better alignment and less porosity. Annealing process could modify the grain size, improve saturation magnetization and coercivity of Sendust flakes. Hence, the radio and quasi-microwave frequency permeability (between 10 MHz to 3 GHz) of composites membranes with annealed Sendust flakes could be enhanced significantly as compared with that of the as-prepared flakes. Infiltration method is especially suitable for composites with high concentration of flaky fillers. The composite membranes prepared have potential applications, including electromagnetic shielding, noise reduction and wave absorption.     

Investigating the magnetic properties of soft magnetic composites based on mechanically alloyed nanocrystalline Fe-5 wt% Ni powders

In this work, the soft magnetic composites (SMCs) of the nanocrystalline Fe-5 wt% Ni powders coated with phenolic resin were studied. The nanocrystalline powders with an average diameter of 10 nm were obtained by mechanical alloying up to 96 h milling in a high-energy planetary ball mill. The microstructure and magnetic properties of the milled powders were characterized by X-ray diffraction, energy dispersive X-ray spectroscopy and a vibrating sample magnetometer. The results of X-ray diffraction showed that the bcc Fe(Ni) solid solution is formed after 24 h milling. Magnetic measurements indicated that the 96 h milled powders with a steady-state grain size of 10 nm have the highest saturation magnetization and the lowest coercivity. The SMCs based on nanocrystalline powders showed higher electrical resistivity and magnetic permeability up to 1 MHz, as compared with the pure iron-based composites. Besides, the nanocrystalline-based SMCs exhibited higher relaxation frequency and a significantly lower loss factor up to 1 MHz.     

Microwave absorption properties of one thin sheet employing carbonyl-iron powder and chlorinated polyethylene

To solve more and more serious electromagnetic interference problem, one thin microwave absorbing sheet employing carbonyl-iron powder (CIP) and chlorinated polyethylene (CPE) was prepared. The pattern, static magnetic properties and phase of CIP were characterized by scanning electron microscope (SEM), vibrating sample magnetometer (VSM) and X-ray diffraction (XRD), respectively. The electromagnetic parameters of CIP were measured in the frequency range of 2-18 GHz, and the electromagnetic loss mechanisms of the powder were discussed. The microwave absorption properties of composite sheets with different thicknesses and CIP ratios in matrix were investigated by measuring reflection loss (RL) in 2-18 GHz frequency range using the arch method. The results showed that appropriate CIP content and thickness could greatly improve microwave absorption properties in lower frequency range. For the sample with the weight ratio (CIP:CPE) of 16:1 and 1.5 mm thickness, the bandwidth (RL below −10 dB) achieved 1.1 GHz (2-3.1 GHz), and the minimum reflection loss value was obtained −13.2 dB at 2.2 GHz. This suggested that CIP/CPE composites could be applied as thin microwave absorbers in S-band (2-4 GHz).     

Electromagnetic wave-absorption properties of rapidly quenched of Nd–Fe–B nanocomposites with low Nd content

The electromagnetic wave-absorption properties of Nd₃Fe_68−xMn_xCo₁₈B₁₁ (x=0, 1, 2) alloys obtained by rapid quenching from the melt was studied. The complex permittivity-frequency and permeability-frequency properties were determined in the microwave frequency regime of 2–18 GHz by vector network analysis. XRD spectra showed that only α-Fe diffraction peak was observed in the as-spun alloys. It is found that the acquired complex permittivity and permeability values match the microwave frequency when the 1 at% Mn content was doped. A minimum reflection loss of −6.9 dB is obtained at 2.7 GHz for composite Nd₃Fe₆₆Mn₂Co₁₈B₁₁ with absorber thickness of 1.5 mm. The exchange interaction was attributed to the microwave absorption properties. The results suggest a new design of microwave absorbers based on electromagnetic wave-absorbing materials.     

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.     

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.     

X-ray diffraction,microstructure, Mössbauer and magnetization studies of nanostructured Fe50Ni50 alloy prepared by mechanical alloying

Nanocrystalline Fe₅₀Ni₅₀ alloy samples were prepared by the mechanical alloying process using planetary high-energy ball mill. The alloy formation and different physical properties were investigated as a function of milling time, t, (in the 0–50 h range) by means of the X-ray diffraction (XRD) technique, scanning electron microscopy (SEM), energy dispersive X-ray (EDAX), Mössbauer spectroscopy and the vibrating sample magnetometer (VSM). The complete formation of γ-FeNi is observed after 24 h milling. When milling time increases from 0 to 50 h, the lattice parameter increases towards the Fe₅₀Ni₅₀ bulk value, the grain size decreases from 67 to 13 nm, while the strain increases from 0.09% to 0.41%. Grain morphologies at different formation stages were observed by SEM. Saturation magnetization and coercive fields derived from the hysteresis curves are discussed as a function of milling time.     

Magnetic and structural studies of mechanically alloyed nanostructured Fe49Co49V2 powders

Nanostructured Fe₄₉Co₄₉V₂ powders were produced by high energy milling at different milling times and then examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The saturation magnetization and coercivity of samples were measured at room temperature by a vibration sample magnetometer (VSM). Structural studies show that as the milling time increases from 0 to 125 h, the average grain size reduces from 130 to about 8-10 nm, while the microstrain increases up to 1.7%. The lattice parameter decreases from 0 to 36 h and then increases up to 125 h. According to the XRD patterns, the formation of intermetallic compound of (Fe, Co)V after about 16 h affects the magnetic properties. The coercivity totally increases up to 61 Oe due to the introduction of microstrain during the milling process. Magnetic measurements reveal that the saturation magnetization has some fluctuations during the milling treatment and finally at 125 h reaches about 180 emu/g     

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.     

The effect of multi-step milling and annealing treatments on microstructure and magnetic properties of nanostructured Fe-Si powders

Nanostructured Fe_1−xSi_x (x=0.05, 0.1, 0.15 and 0.2) powders are prepared by different multi-step milling and annealing treatments. The microstructure and magnetic properties are investigated for all alloys. The minimum crystallite size of as-annealed powders (∼40 nm) is found to be larger than in as-milled ones (∼15 nm). It is found that microstrains of 2- and 4-step processes are close to those of the as-received powders. The lattice parameter decreased ∼0.5% and 0.9% for the powders that experienced milling and annealing at the last step, respectively. The Fe₈₀Si₂₀ powders prepared by 1- and 4-step treatments show the maximum (40-125 Oe) and minimum (20-26 Oe) coercivity, respectively. With increase in milling time, mass magnetization increased for all processes. This can be ascribed to diminution in magneto-crystalline anisotropy due to grain refinement. The maximum mass magnetization (160-199 Am²/kg) is achieved for the 4-step process.     

Magnetic and microwave absorbing properties of polyaniline/γ-Fe2O3 nanocomposite

The conducting protonated polyaniline (ES)/γ-Fe₂O₃ nanocomposite with the different γ-Fe₂O₃ content were synthesized by in-situ polymerization. Its morphology, microstructure, DC conductivity and magnetic properties of samples were characterized by transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), four-wire-technique, and vibrating sample magnetometer (VSM), respectively. The microwave absorbing properties of the nanocomposite powders dispersing in wax coating with the coating thickness of 2 mm were investigated using a vector network analyzers in the frequency range of 7–18 GHz. The pure ES has shown the absorption band with a maximum absorption at approximately 16 GHz and a width (defined as frequency difference between points where the absorption is more than 8 dB) of 3.24 GHz, when 10% γ-Fe₂O₃ by weight is incorporated , the width is broadened to 4.13 GHz and some other absorption bands appear in the range of 7–13 GHz. The parameter dielectric loss tan δ_e (=ε″/ε′) in the 7–18 GHz is found to decrease with increasing γ-Fe₂O₃ contents with 10%, 20%, 30%, respectively, but magnetic loss tan δ_m (=μ″/μ′) increases with increasing γ-Fe₂O₃ contents. The results show that moderate content of γ-Fe₂O₃ nanoparticles embedded in protonated polyaniline matrix may create advanced microwave absorption properties due to simultaneous adjusting of dielectric loss and magnetic loss.     

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.     

Microwave-absorbing properties of shape-optimized carbonyl iron particles with maximum microwave permeability

The microwave-absorbing properties for different shapes of carbonyl-iron particles prepared by the high-energy planetary ball milling with 40 vol% in epoxy resin matrix have been investigated. Higher value of magnetic permeability and permittivity can be obtained in the composites for thin flake carbonyl iron than spherical powders. The results are attributed to reduction of eddy current loss, orientation of magnetic moment and space-charge polarization with the shape change from spherical powders to thin flake particles. As the iron flakes with 0.4 μm in thickness as the absorbent fillers, the minimum RL value of −6.20 dB was observed at 4.57 GHz with thickness of 1 mm. The minimum reflection loss (RL) shifts to lower frequency and the value declines with change from spherical powders to thin flakes. It results from the considerable dielectric loss in the absorbing materials.     

Preparation of nanocrystalline Fe–Ni powders by mechanical alloying used in soft magnetic composites

This paper focuses on the preparation of nanocrystalline Fe–Ni powders by mechanical alloying method, which can be used in soft magnetic composites. Fe–10 wt% Ni and Fe–20  wt % Ni alloys were prepared using a high-energy ball mill. The magnetic properties of samples were measured by a B–H curve analyzer and microstructures of the samples were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The bcc Fe(Ni) phase formation was identified by XRD and completed after 45 h of milling. It was found that higher milling time resulted in, larger lattice parameter, higher microstrains and smaller crystallite sizes. Also, results showed that with increasing the milling time, coercivity increased and saturation intrinsic flux density firstly increased noticeably and then decreased in higher milling times (>70 h).     

Magnetic binary nanofillers

Magnetic binary nanofillers containing multiwall carbon nanotubes (MWCNT) and hercynite were synthesized by Chemical Vapor Deposition (CVD) on Fe/AlOOH prepared by the sol–gel method. The catalyst precursor was fired at 450 °C, ground and sifted through different meshes. Two powders were obtained with different particle sizes: sample A (50–75 μm) and sample B (smaller than 50 μm). These powders are composed of iron oxide particles widely dispersed in the non-crystalline matrix of aluminum oxide and they are not ferromagnetic. After reduction process the powders are composed of α-Fe nanoparticles inside hercynite matrix. These nanofillers are composed of hercynite containing α-Fe nanoparticles and MWCNT. The binary magnetic nanofillers were slightly ferromagnetic. The saturation magnetization of the nanofillers depended on the powder particle size. The nanofiller obtained from powder particles in the range 50–75 μm showed a saturation magnetization 36% higher than the one formed from powder particles smaller than 50 μm. The phenomenon is explained in terms of changes in the magnetic environment of the particles as consequence of the presence of MWCNT.