Fabrication and microwave absorption properties of magnetite nanoparticle–carbon nanotube–hollow carbon fiber composites

Absorbents with “tree-like” structures, which were composed of hollow porous carbon fibers (HPCFs) acting as “trunk” structures, carbon nanotubes (CNTs) as “branch” structures and magnetite (Fe₃O₄) nanoparticles playing the role of “fruit” structures were prepared by chemical vapor deposition technique and chemical reaction. Microwave reflection loss, permittivity and permeability of Fe₃O₄–CNTs–HPCFs composites were investigated in the frequency range of 2–18 GHz. It was proven that prepared absorbents possessed the excellent electromagnetic wave absorbing performances. The bandwidth with a reflection loss less than −15 dB covers a wide frequency range from 10.2 to 18 GHz with the thickness of 1.5–3.0 mm, and the minimum reflection loss is −50.9 dB at 14.03 GHz with a 2.5 mm thick sample layer. Microwave absorbing mechanism of the Fe₃O₄–CNTs–HPCFs composites is concluded as dielectric polarization and the synergetic interactions exist between Fe₃O₄ and CNTs–HPCFs.     

Controlled synthesis of Fe3O4@SnO2/RGO nanocomposite for microwave absorption enhancement

A ternary nanocomposite of Fe₃O₄@SnO₂/reduced graphene oxide (RGO) with different contents of SnO₂ nanoparticles was synthesized by a simple and efficient three-step method. The transmission electron microscopy and field emission scanning electron microscopy characterization display that plenty of Fe₃O₄@SnO₂ core–shell structure nanoparticles are well distributed on the surface of RGO sheets. The X-ray diffractograms show that the products consist of highly crystallized cubic Fe₃O₄, tetragonal SnO₂ and disorderedly stacked RGO sheets. The magnetic hysteresis measurement reveals the ferromagnetic behavior of the products at room temperature. The microwave absorption properties of paraffin containing 50 wt% products were investigated at room temperature in the frequency range of 2–18 GHz by a vector network analyzer. The electromagnetic data show that the maximum reflection loss is −45.5 dB and −29.5 dB for Fe₃O₄@SnO₂/RGO-1 and Fe₃O₄@SnO₂/RGO-2 nanocomposite, respectively. Meanwhile, the reflection loss less than −10 dB is up to 14.4 GHz and 13.8 GHz for Fe₃O₄@SnO₂/RGO-1 and Fe₃O₄@SnO₂/RGO-2 nanocomposite, respectively. It is believed that such nanocomposite could be used as promising microwave absorbers.     

Magnetic reduced graphene oxide nanocomposite as an effective electromagnetic wave absorber and its absorbing mechanism

A magnetic reduced graphene oxide (MRGO) composite consisting of graphene oxide and Fe₃O₄ particles in the range of 5–20 nm has been prepared by the one-pot hydrothermal process. RGO nanosheets provide flexible substrates for nanoparticle decoration, while Fe₃O₄ nanoparticles can also effectively prevent nanosheets to restack each other. Compared with previously literature, the synthesized RGO-Fe₃O₄ composite exhibits excellent electromagnetic wave absorption. The minimum reflection loss (R_L) value of −49.05 dB has been observed at 14.16 GHz with a thickness of 2.08 mm. The absorption bandwidth (R_L<−10 dB) corresponding to the minimum R_L is 4.60 GHz. The electromagnetic wave absorption properties of the RGO-Fe₃O₄ composite have been interpreted through the quarter-wavelength matching model.     

The effect of GO loading on electromagnetic wave absorption properties of Fe3O4/reduced graphene oxide hybrids

Ideal electromagnetic absorbing materials with lightweight and high efficiency have broad application outlook in military and civil fields. In this work, a 3D nanostructure material by hybridizing Fe₃O₄ nanocrystals and reduced graphene oxide (Fe₃O₄/rGO) were synthesized through an environmental-friendly one-pot solvothermal method. The effect of GO loading on electromagnetic (EM) wave absorption characteristic of Fe₃O₄/rGO was investigated. The introduction of rGO sheets not only prevented Fe₃O₄ from agglomerating, also improved the absorption performance of Fe₃O₄/rGO hybrids. With an appropriate addition, Fe₃O₄/rGO obtained a minimum reflection loss (RL) of −22.7 dB and the absorption bandwidth was 3.13 GHz (90% absorption).     

Microwave absorption study of carbon nano tubes dispersed hard/soft ferrite nanocomposite

Nickel substituted strontium hexaferrite, SrNi₂Fe₁₀O₁₉·(SrFe₁₂O₁₉/NiFe₂O₄) nanoparticles have been synthesized by low combustion method by citrate precursors using sol to gel (S–G) followed by gel to nano crystalline (G–N) conversion. The resulting ‘as-synthesized’ powder is heat treated (HT) at 800 and 1000 °C for 4 h in nitrogen atmosphere. The hysteresis loops show an increase in saturation magnetization from 27.443 to 63.706 emu/g with increasing HT temperatures. The multiwalled carbon nano tubes (CNTs) were synthesized by thermal decomposition of acetylene gas over iron-catalyst deposited on silicon wafer in the temperature range of 750–800 °C. A microwave absorbing medium is prepared by adding CNTs in the nickel substituted strontium hexaferrite nanoparticles. Addition of certain mass of CNTs improves the microwave absorption properties and wave band of SrFe₁₂O₁₉/NiFe₂O₄ absorbent. When 10 wt% CNTs is mixed with SrFe₁₂O₁₉/NiFe₂O₄ nanoparticles to fabricate a composite with 2 mm thickness, the maximum reflection loss reaches to ?36.817 dB at 9.292 GHz and ?10 dB bandwidth reaches 3.27 GHz.     

Fabrication of carbon encapsulated Co3O4 nanoparticles embedded in porous graphitic carbon nanosheets for microwave absorber

Carbon-encapsulated Co₃O₄ nanoparticles homogeneously embedded 2D (two-dimensional) porous graphitic carbon (PGC) nanosheets were prepared by a facile and scalable synthesis method. With assistance of sodium chloride, the Co₃O₄ nanoparticles (10–20 nm) with magnetic loss were well encapsulated by onion-like carbon shells homogeneously embedded porous graphitic carbon nanosheets (thickness of less than 50 nm) with dielectric loss. In the architecture, the well impedance matching for microwave absorption can be obtained by the synergetic effect between Co₃O₄ nanoparticles and encapsulated porous carbon nanosheets. The minimum reflection loss value of −32.3 dB was observed at 11.4 GHz with a matching thickness of 2.3 mm for 2D Co₃O₄@C@PGC nanosheets. The 2D Co₃O₄@C@PGC nanosheets can be used as a kind of candidate for microwave absorbing materials.     

Hollow polyaniline/Fe3O4 microsphere composites: Preparation,characterization, and applications in microwave absorption

Hollow polyaniline/Fe₃O₄ microsphere composites with electromagnetic properties were successfully prepared by decorating the surface of hollow polyaniline/sulfonated polystyrene microspheres with various amounts of Fe₃O₄ magnetic nanoparticles using sulfonated polystyrene (SPS) as hard templates and then removing the templates with tetrahydrofuran (THF). The synthesized hollow microsphere composites were characterized by FT-IR, UV/Vis spectrophotometry, SEM, XRD, elemental analysis, TGA, and measurement of their magnetic parameters. Experimental results indicated that the microspheres were well-defined in size (1.50–1.80 μm) and shape, and that they were superparamagnetic with maximum saturation magnetization values of 3.88 emu/g with a 12.37 wt% content of Fe₃O₄ magnetic nanoparticles. Measurements of the electromagnetic parameters of the samples showed that the maximum bandwidth was 8.0 GHz over ?10 dB of reflection loss in the 2–18 GHz range when the Fe₃O₄ content in the hollow polyaniline/Fe₃O₄ microsphere composites was 7.33 wt%.     

Controlled synthesis and electromagnetic wave absorption properties of core-shell Fe3O4@SiO2 nanospheres decorated graphene

Fe₃O₄/reduced graphene oxide (RGO) nanocomposite was synthesized by a simple hydrothermal method and then SiO₂ coated onto Fe₃O₄ by a modified Stӧber method. The transmission electron microscopy and field emission scanning electron microscopy characterization indicate that masses of Fe₃O₄@SiO₂ core-shell structure nanospheres attached to the RGO sheets, and that the thicknesses of SiO₂ shells are about 20–40 nm. The X-ray diffractograms and Raman spectra illustrate that the synthesized samples consist of highly crystallized cubic Fe₃O₄, amorphous SiO₂ and disorderedly stacked RGO sheets. The magnetic hysteresis loops reveal the ferromagnetic behavior of the samples at room temperature. In addition, the Fe₃O₄@SiO₂/RGO paraffin composite exhibit excellent electromagnetic wave absorption properties at room temperature in the frequency range of 2–18 GHz, which are attributed to the effective complementarities between the dielectric loss and magnetic loss. For Fe₃O₄@SiO₂/RGO-1 and Fe₃O₄@SiO₂/RGO-2 nanocomposite, the minimum reflection loss can reach −26.4 dB and −16.3 dB with the thickness of 1.5 mm, respectively. The effective absorption bandwidth of the samples can reach more than 10.0 GHz with the thickness in the range of 1.5–3.0 mm. It is demonstrated that such nanocomposite could be used as a promising candidate in electromagnetic wave absorption area.     

Magnetic and microwave properties of BaFe12O19 substituted with magnetic,non-magnetic and dielectric ions

Barium hexaferrite particles were synthesized with conventional solid state reaction route. 1% boron (B₂O₃) was added to the initial mixture of oxides to inhibit crystal growth at lower temperatures. Magnetic (Mn²⁺, Co²⁺, Ni²⁺and Cu²⁺), non-magnetic (Zn²⁺) and dielectric (Ti⁴⁺) ions were replaced by one Fe³⁺ ion of barium hexaferrite to shift the ferromagnetic resonance frequency to low frequencies and to increase the magnetic and dielectric losses. The structural and morphological characterization of samples was done by X-ray powder diffractometer and scanning electron microscopy. Magnetic and microwave properties were determined by vibrating sample magnetometer and vector network analyzer, respectively. The maximum saturation magnetization and the highest reflection losses of −34 dB at 10 GHz, with absoption bandwidth of 1.6 GHz at −20 dB, were observed in Cu²⁺–Ti⁴⁺ and Zn²⁺–Ti⁴⁺ substituted samples. The mechanism of microwave energy dissipation is due to the impedance matching at matching thickness. It was also observed that as the sample thickness increases, the resonance frequency decreases exponentially.     

Microwave-assisted solution combustion synthesis of Fe3O4 powders

Magnetite (Fe₃O₄) powders were synthesized by solution combustion method at different fuel to oxidant ratios (ϕ = 0.5, 0.75, 1 and 1.5) using conventional and microwave ignition. The ignition method and fuel content affected the phase evolution, microstructure and magnetic properties of Fe₃O₄ powders as characterized by X-ray diffractometry, infrared spectroscopy, N₂ adsorption–desorption, electron microscopy and vibrating sample magnetometry techniques. Single phase Fe₃O₄ powders were only obtained using conventional ignition at ϕ value of 1, while the impurity phases such as α-Fe₂O₃ and FeO together with Fe₃O₄ phase were formed by microwave ignition. The bulky microstructure of conventionally combusted powders with specific surface area of 71.5 m²/g was transformed to disintegrated structure (76.5 m²/g) by microwave heating. The microwave combusted powders showed the highest saturation magnetization of 86.5 emu/g at ϕ value of 0.5 and the lower coercivity than that of conventionally combusted powders at all ϕ values, due to their larger particles.     

Effect of La-Ni substitution on structural,magnetic and microwave absorption properties of barium ferrite

In this paper, La-Ni substituted barium ferrite nanoparticles were prepared by a co-precipitation method. The morphology, structure, magnetic and microwave absorption properties of samples were accomplished by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscope (TEM), vibrating sample magnetometer (VSM) and vector network analysis. From the results evaluation, it can be seen that the magnetoplumbite structure for all of the samples have been formed and the average crystallite sizes of Ba_1−xLa_xFe_12−xNi_xO₁₉ nanoparticles within in the range of 50.9–65.5 nm. Ba_0.9La_0.1Fe_11.9Ni_0.1O₁₉ exhibits a remarkable reflection loss of −13.5 dB at 13.05 GHz with a matching thickness of 1.5 mm. The reflection loss results indicate that Ba_0.9La_0.1Fe_11.9Ni_0.1O₁₉ nanoparticles may be used as a potential for thin microwave absorbers.     

Crystallization kinetics and magnetic properties of iron oxide contained 25Li2O–8MnO2–20CaO–2P2O5–45SiO2 glasses

With crystallization at 850 °C for 4 h, LiMn₂O₄, β-wollastonite (β-CaSiO₃), lithium silicate (Li₂SiO₃), Ca(Ca, Mn)Si₂O₆ and Li₂Ca₄Si₄O₁₃ phases were found in 25Li₂O–8MnO₂–20CaO–2P₂O₅–45SiO₂ (LMCPS) glass ceramics. The (Li, Mn)ferrite phase was obtained in the iron oxide contained LMFCPS glass ceramic and Li₂FeMn₃O₈ phase was found in that containing 8 at.% Fe₂O₃. TEM investigations showed that (Li, Mn)ferrite particles dispersed in the β-wollastonite matrix (Li, Mn)ferrite particles, with an average size of 40 nm, were found in the glass ceramics containing 4 at.% Fe₂O₃. The (Li, Mn)ferrite particle sizes in the glass ceramics containing 8 at.% Fe₂O₃ varied from a few μm to 5 nm. The SQUID result showed that only the glass ceramic containing 4 at.% Fe₂O₃ exhibited super-paramagnetic behavior at temperature 300 K and ferromagnetic behavior at 4 K. The LMCPS glass ceramic containing 8 at.% Fe₂O₃ exhibited ferromagnetic behavior at both temperatures.     

Development of novel magnetic-dielectric ceramics for enhancement of reflection loss in X band

The purpose of this research was to develop BaFe_9.5Al_1.5CrO₁₉-xCaCu₃Ti₄O₁₂ nanocomposites (x=10%, 20%, 30%, 40%, 50%) and investigate their structural and magnetic features. The substituted barium hexaferrite (BaFe_9.5Al_1.5CrO₁₉) nanoparticles and calcium copper titanate (CaCu₃Ti₄O₁₂) particles were synthesized by the auto-combustion sol-gel method. The structural, chemical composition and morphology of CaCu₃Ti₄O₁₂ (CCTO) and the nanocomposites were investigated by X-ray diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy, respectively. The magnetic and microwave properties of nanocomposites were also investigated by vibrating sample magnetometer and vector network analyzer, respectively. The results confirmed that 1100 °C is the optimum synthesis temperature for CCTO, the mean particles size of the CCTO particles changing from 220 nm (at 850 °C) to 2.18 µm (1250 °C). The SEM micrograph revealed that in all of the BaM-xCCTO nanocomposites (x=10%, 20%, 30%, 40%, 50%), the CCTO dielectric particles were attached to the substituted barium hexaferrite nanoparticles, indicating the effectiveness of the adopted synthesis method. Due to the presence of a dielectric phase in the nanocomposites the saturation magnetization decreases from 22 emu/g to 12 emu/g. The coercive field was a slightly larger than substituted barium hexaferrite and increased from 5.558 kOe for substituted barium hexaferrite to 5.813 kOe for BaM-50CCTO due to hindered motion of the domain walls by the dielectric phase and also to the collective behavior of agglomerated barium ferrite nanoparticles. The BaM-30CCTO nanocomposite shows the highest value of reflection loss compared to other nanocomposites. The reflection dip frequency of BaM-30CCTO nanocomposite was −48.85 dB at 10.93 GHz.     

A comparative study of the magnetic and microwave properties of Al3+ and In3+ substituted Mg–Mn ferrites

The effect of substitution of diamagnetic Al³⁺ and In³⁺ ions for partial Fe³⁺ ions in a spinel lattice on the magnetic and microwave properties of magnesium–manganese (Mg–Mn) ferrites has been studied. Three kinds of Mg–Mn based ferrites with compositions of Mg_0.9Mn_0.1Fe₂O₄, Mg_0.9Mn_0.1Al_0.1Fe_1.9O₄, and Mg_0.9Mn_0.1In_0.1Fe_1.9O₄ were prepared by the solid-state reaction route. Each mixture of high-purity starting materials (oxide powders) in stoichiometric amounts was calcined at 1100 °C for 4 h, and the debinded green compacts were sintered at 1350 °C for 4 h. XRD examination confirmed that the sintered ferrite samples had a single-phase cubic spinel structure. The incorporation of Al³⁺ or In³⁺ ions in place of Fe³⁺ ions in Mg–Mn ferrites increased the average particle size, decreased the Curie temperature, and resulted in a broader resonance linewidth as compared to un-substituted Mg–Mn ferrites in the X-band. In this study, the In³⁺ substituted Mg–Mn ferrites exhibited the highest saturation magnetization of 35.7 emu/g, the lowest coercivity of 4.1 Oe, and the highest Q×f value of 1050 GHz at a frequency of 6.5 GHz.     

Fabrication of graphene nanosheet (GNS)–Fe3O4 hybrids and GNS–Fe3O4/syndiotactic polystyrene composites with high dielectric permittivity

Graphene nanosheet–Fe₃O₄ (GNS–Fe₃O₄) hybrids were obtained by a one-step solvothermal reduction of iron (III) acetylacetonate [Fe(acac)₃] and graphene oxide (GO) simultaneously, which had several advantages: (1) the Fe₃O₄ nanoparticles were firmly anchored on GNS surface even after mild ultrasonication; (2) the loading amount of Fe₃O₄ nanoparticles could be effectively controlled by changing the initial feeding weight ratio of Fe(acac)₃ to GO; (3) the Fe₃O₄ nanoparticles were homogeneously distributed on the GNS surface without much aggregation. Composites based on syndiotactic polystyrene (sPS) and GNS–Fe₃O₄ were prepared by a solution-blending method and the electric and dielectric properties of the resultant GNS–Fe₃O₄/sPS composites were investigated. The percolation threshold of GNS–Fe₃O₄ in the sPS matrix was determined to be 9.41 vol.%. Slightly above the percolation threshold with 9.59 vol.% of GNS–Fe₃O₄, the GNS–Fe₃O₄/sPS composite showed a high dielectric permittivity of 123 at 1000 Hz, which was 42 times higher than that of pure sPS. The AC electrical conductivity at 1000 Hz increased from 3.6 × 10⁻¹⁰ S/m for pure sPS to 2.82 × 10⁻⁴ S/m for GNS–Fe₃O₄/sPS composite containing 10.69 vol.% of GNS–Fe₃O₄, showing an obvious insulator-semiconductor transition.     

Solution combustion synthesis of La1−xSrxFe1−yCuyO3±w (x=0, 0.2; y=0, 0.2) perovskite nanoparticles: Conventional vs. microwaves ignition

La_1−xSr_xFe_1−yCu_yO_3±w (x=0, 0.2; y=0, 0.2) nanoparticles have been prepared by solution combustion synthesis exploiting both conventional and microwave heating in the ignition of the self-sustaining reactions. Interaction of microwaves with the reaction mixture allowed significant reduction of the ignition time according to the dielectric properties of the precursor gels, which have been measured at room temperature in the 0.5–3 GHz frequency range. Both the ignition strategies led to the preparation of crystalline single-phase products without affecting particles morphology. The ignition technique influenced only the average particles size with those prepared by microwaves-ignition, possessing typically larger dimension, as a probable consequence of the higher temperatures reached due to microwave absorbing products. Perfectly crystallised nanoparticles were obtained after combustion syntheses and calcination at 600 °C for 3 h in the particle size range between 20 and 80 nm dependently upon the heating source and the dopant level.     

Study on orientation in EVA/Fe3O4 composite hot-melt adhesives

EVA hot melt adhesives have tackiness to both external anticorrosion coating made by cross-linked polyethylene and iron-base petroleum pipeline. But, traditional EVA hot melt adhesives cannot meet the requirement of external anticorrosion coating for weaker tackiness. Two types of Fe₃O₄ particles with different particle sizes and magnetic strengths were added in adhesives. One is of 3.665 μm^{Laser particle size analyzer (LPSA)} and 8.403×10¹ emu/g^{vibrating sample magnetometer (VSM)} and the other one is of 0.426 μm^LPSA and 3.997×10¹ emu/g^VSM. The result of peel test indicated that peel strength of composite adhesives increased as Fe₃O₄ content increased when particles size was 3.665 μm^LPSA but the tackiness of composite adhesive decreased as Fe₃O₄ content increased when particles size was 0.426 μm^LPSA. Also, microphotos of SEM revealed that the composite adhesive with 3.665 μm^LPSA Fe₃O₄ was more likely to distribute in a region near the tackiness surface between the adhesive and iron layers, but the one with 0.426 μm^LPSA Fe₃O₄ was more likely to aggregate in the middle region of adhesive. The movement of 3.665 μm^LPSA Fe₃O₄ particles could induce EVA molar chain orientation and this orientation was confirmed by infrared dichroism and XRD. Results of infrared dichroism and XRD showed that the orientation degree of EVA increased as 3.665 μm^LPSA Fe₃O₄ content increased. Furthermore, crystallinity tests by XRD and DSC indicated that crystallinity of PE segment of EVA also increased as 3.665 μm^LPSA Fe₃O₄ content increased, which could support increase of orientation tested by infrared dichroism and XRD.     

Synthesis of hierarchical core-shell NiFe2O4@MnO2 composite microspheres decorated graphene nanosheet for enhanced microwave absorption performance

A ternary functional composite NiFe₂O₄@MnO₂@graphene was synthesized successfully via a facile method. The phase constitution, microstructures, morphologies and chemical compositions of the samples were investigated by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), Brunauer-Emmett-Teller (BET) and X-ray photoelectron spectroscopy (XPS). It was observed that the NiFe₂O₄ nanoparticles were coated by hierarchically MnO₂ shells and distributed on the surface of graphene. Investigations of EM wave absorption indicated that NiFe₂O₄@MnO₂@ graphene composite has the strongest reflection loss of −47.4 dB at 7.4 GHz at the matching thickness of 3 mm, compared to NiFe₂O₄ and NiFe₂O₄@MnO₂, and its maximum absorption bandwidth (<−10 dB) is 4.3 GHz (from 5.1 to 9.4 GHz). The enhanced microwave absorption performance can be attributed to the hierarchical structure of MnO₂, void space between MnO₂ and graphene, and better impedance matching of ternary composite. The above results indicate that the novel hierarchical NiFe₂O₄@MnO₂@graphene composite, with intense absorption and wide absorption bandwidth, would be a promising absorber with less EM wave interference.     

Fabrication of microwave absorbing CoFe2O4 coatings with robust superhydrophobicity on natural wood surfaces

A superhydrophobic wood surface with microwave absorption property was prepared based on the formation of CoFe₂O₄ nanoparticles and subsequent hydrophobization using fluorinated alkylsilane (FAS). Meanwhile, sticky epoxy resin was worked as a caking agent by adhering abundant of CoFe₂O₄ nanoparticles to wood surface. The as-prepared superhydrophobic coatings on wood maintain stable superhydrophobicity after suffering a significant abrasion. Moreover, the complex permeability and permittivity of the coated wood composites were measured in the frequency range of 2–18 GHz by vector network analysis. The microwave absorption properties were elucidated by the traditional coaxial line method. The results show that the as-prepared wood composites have excellent microwave absorption properties at the frequency of 16 GHz, and the minimum reflection loss can reach −12.3 dB. The approach presented may provide further routes for designing outdoor wood wave absorbers with a specified absorption frequency.     

Flexible polymer composites with enhanced wave absorption properties based on beta-manganese dioxide nanorods and PVDF

Beta-manganese dioxide (β-MnO₂) nanorods have been fabricated on a large scale by a simple hydrothermal process in a wild condition. Several characterizations such as XRD, SEM, TEM and FESEM have been employed. The wave absorption properties of β-MnO₂/PVDF nanocomposites have been investigated. The results indicated that the β-MnO₂/PVDF nanocomposites exhibit enhanced wave absorption properties. The minimum reflection loss of the β-MnO₂/PVDF nanocomposite reaches − 30.1 dB (> 99.9% attenuation) at 8.16 GHz with a filler loading of 40 wt.%, and the frequency bandwidth less than –10 dB is from 7.12 to 9.20 GHz. The main microwave absorbing mechanism has been also discussed.