Preparation and microwave absorbing properties of hollow glass microspheres/Fe3O4/Ag composites with core–shell structure

The low-density, conductive and magnetic hollow glass microspheres (HGM)/Fe₃O₄/Ag composites have been successfully synthesized via co-precipitation and chemical plating method. The morphology, composition, microstructure, magnetic and microwave absorbing properties of the composites were investigated based on the analyses of the results using scanning electron microscope, energy dispersive spectroscopy, X-ray diffraction, vibrating sample magnetometer and vector network analyzer. The results showed that the HGM/Fe₃O₄ composites were successfully prepared, and the coating layers on the surface of HGM are compact and continuous. Moreover, the final composites were completely covered with Ag nanoparticles. With the addition of Ag nanoparticles, the saturation magnetization of the HGM/Fe₃O₄ composites reduces from 32.08 to 14.77 emu/g, whereas its conductivity increases to 0.48 S/cm. The reflection loss (R) of HGM/Fe₃O₄/Ag composites is lower than ?10 dB at 8.2–8.7, 9.6–10.8 and 11.4–11.9 GHz, and the minimum loss value is ?19.1 dB at 9.9 GHz.     

The characterization and preparation of core–shell structure particles of carbon-sphere@NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript>@PPy as microwave absorbing materials in X band

An excellent PPy/NiFe₂O₄/CS microwave absorbing materials with a three-layer core–shell structure, was synthesized successfully by two reaction steps of solvothermal reaction and in situ polymerization. The surface morphology, phase structure and chemical components of the composite have been characterized by a scanning electron microscope, X-ray diffraction and X-ray photoelectron spectroscope. The results suggest that the surface of CS is covered by NiFe₂O₄ completely and PPy wraps the obtained NiFe₂O₄/CS successfully. The conductivity and the saturation magnetization (Ms) of the resulting PPy/NiFe₂O₄/CS composites are 0.38 S/cm and 46 emu/g, respectively. The vector network analysis shows the composite performs better microwave absorbing ability than that of CS and NiFe₂O₄/CS. The maximum reflection loss of the composite with 1.97 mm coating thickness is ?53 dB at 10.5 GHz and the bandwidth of reflection loss less than ?10 dB is 3.4 GHz (8.9–12.3 GHz). This ternary composite with light weight, thin thickness and strong absorbing capacity can be an attractive candidate in the field of microwave absorption.     

Time-sensitivity for the preparation and microwave absorption properties of core–shell structured Ni/TiO<Subscript>2</Subscript> composite microspheres

Core–shell Ni/TiO₂ composite microspheres with different crystallinity have been prepared at various reaction times by the solvothermal method. The crystal structure and morphology of the products were investigated by X-ray diffraction, field-emission scanning electron microscopy and transmission electron microscopy. The microwave absorption properties of the core–shell Ni/TiO₂ composites were investigated at 1.0–18.0 GHz. The results show that the morphology and microwave absorption performances of Ni/TiO₂ composites were largely influenced by the crystallinity of TiO₂ shells. The crystallinity of anatase TiO₂ can be increased with increasing reaction time. Minimum peaks of Ni/TiO₂ composites shift to the high frequency with increasing the crystallinity of anatase TiO₂, which are due to high thermal conductivity of high crystallinity of TiO₂. The Ni/TiO₂ prepared at 36 h exhibits the best microwave absorption properties with minimum reflection loss of ?16.9 dB at 14.1 GHz.     

Preparation,structure and microwave dielectric properties of 3MgO–Al<Subscript>2</Subscript>O<Subscript>3</Subscript>–3TiO<Subscript>2</Subscript> ceramics

3MgO–Al₂O₃–3TiO₂ (MAT) ceramics were prepared by a conventional solid-state reaction method. The crystal structure, sintering behavior and microwave dielectric properties of ceramics were investigated using X-ray diffraction, scanning electron microscopy and network analyzer. MAT ceramics contained the coexistence of three phases, including MgAl₂O₄, MgTiO₃ and MgTi₂O₅. The ceramics sintered at 1350 °C for 4 h presented excellent comprehensive performances with relative permittivity (ε _r ) of 15.4, quality factor (Q × f) of 91,000 GHz and temperature coefficient of resonant frequency (τ _f ) about ?55.1 ppm/°C.     

Preparation of MnO<Subscript>2</Subscript>/porous carbon material with core–shell structure and its application in supercapacitor

Tubular manganese dioxide (MnO₂) is synthesized by hydrothermal method, and a silicon dioxide (SiO₂) used as template is wrapped on the as-synthesized MnO₂. Then poly(styrene-co-divinylbenzene) (PS) as heteropolymeric carbon precursor was wrapped on as-prepared MnO₂/SiO₂ to form intermediate product MnO₂@SiO₂@PS. The intermediate products were treated by carbon tetrachloride, stripped template and carbonized, thus the final product MnO₂/porous carbon composite (MnO₂@PC) with core–shell structure was obtained. The core–shell structural composite is used as an electrode of supercapacitors, which combines high conductivity and high surface specific area of porous carbon material and high electrochemical activity of MnO₂. The resulting core–shell MnO₂@PC exhibits a maximum specific capacitance of 196.2 F g^?1 at a discharge density of 1 A g^?1 with capacitance retention of 78.52% over 5000 discharge/charge cycles.     

Microwave adsorption of core–shell structure polyaniline/SrFe<Subscript>12</Subscript>O<Subscript>19</Subscript> composites

Polyaniline/strontium hexaferrites (PANI/SrFe₁₂O₁₉) composites were synthesized by the oxidative chemical polymerization of aniline in the presence of APS. X-ray powder diffraction of ferrites indicated that the structure of core materials is hexagonal with lattice constants around 5.886–5.885 Å. The structural in the character of the sol–gel was investigated with Fourier transform infrared spectrometer analysis. SEM and TEM photographs show that the particle size of core material is around 50–200 nm. After coating with polyaniline, the particle size of the core–shell of PANI/SrFe₁₂O₁₉ has grown up to 100~300 nm. In the magnetization for the PANI/SrFe₁₂O₁₉ composites, it was found that the saturation magnetization (M _s) and coercivity (H _c) decreased after polyaniline coating. The composite under applied magnetic field exhibited the hysteretic loops of the ferromagnetic behavior, such as high saturation magnetization (M _s = 18.9 emu/g) and coercivity (H _c = 3850.0 Oe). The conductivity of the core–shell materials increased with increasing amounts of polyaniline as the temperature increased from 0 to 50 °C, the conductivity increased by about 13%. The polymerization mechanism for the core–shell composites was also investigated. The composite specimens of core–shell PANI/SrFe₁₂O₁₉ and thermal plastic resin (TPR) had band-width microwave absorption due to reflection losses from ?27.3 to ?37.4 dB at frequencies between 10.5 and 11.8 GHz as observed by High-frequency network analyzer.     

Influence of Bi substitution on microwave dielectric properties of BaO–La<Subscript>2</Subscript>O<Subscript>3</Subscript>–Sm<Subscript>2</Subscript>O<Subscript>3</Subscript>–TiO<Subscript>2</Subscript> ceramics

The influences of Bi substitution on microwave dielectric properties of Ba₄(La_0.5Sm_0.5)_9.33Ti₁₈O₅₄ solid solutions were investigated. Dielectric ceramics with general formula Ba₄(La_(0.5−z)Sm_0.5Bi _z )_9.33Ti₁₈O₅₄, z = 0.0–0.2 were prepared by conventional solid state route. The structural analysis of all the samples was carried out by X-ray diffraction and scanning electron microscopy. The dielectric properties were investigated as a function of Bi contents using open-ended coaxial probe method in the frequency range 0.3–3.0 GHz at room temperature. Dielectric constant varies from 83 to 88 and loss tangent from 2.1 × 10⁻³ to 5.5 × 10⁻³ at 3 GHz with temperature coefficient of resonant frequency changing from 106.7 to −8.4 ppm/oC as Bi contents increases from z = 0.00–0.20. It has been found that dielectric constant and temperature coefficient of resonant frequency improve whereas loss tangent is adversely affected with increase in Bi substitution.     

Synthesis and microwave absorption enhancement of yolk–shell Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@C microspheres

Rational design on the microstructure of microwave-absorbing materials is paving the way for upgrading their performances in electromagnetic pollution prevention. In this study, a Fe₃O₄/C composite with unique yolk–shell microstructure (YS-Fe₃O₄@C) is successfully fabricated by a silica-assisted route. It is found that carbon shells in this composite can make up the shortages of Fe₃O₄ microspheres in dielectric loss ability, while they may more or less attenuate the intrinsically magnetic loss of Fe₃O₄ microspheres. The microwave absorption properties of YS-Fe₃O₄@C are evaluated in the frequency range of 2.0–18.0 GHz in terms of the measured complex permittivity and complex permeability. The results demonstrate that YS-Fe₃O₄@C can exhibit much better performance than bare Fe₃O₄ microspheres and individual carbon materials, as well as core–shell Fe₃O₄/C composite (CS-Fe₃O₄@C), where strong reflection loss and wide response bandwidth can be achieved simultaneously. With an absorber thickness of 2.0 mm, the maximum reflection loss is ?73.1 dB at 14.6 GHz and a bandwidth over ?10.0 dB is in the range of 12.3–18.0 GHz. It can be proved that the unique yolk–shell microstructure is helpful to reinforce the dielectric loss ability and create an optimized matching of characteristic impedance in the composite.     

Enhanced antibacterial performance of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>–Ag and MnFe<Subscript>2</Subscript>O<Subscript>4</Subscript>–Ag nanocomposites

In this work, we have described the antibacterial activities of Fe₃O₄ nanoparticles with different organic parts, including Humic acid (HA), Nicotinic acid (Nico) and Histidine (His), and the antibacterial activity of MnFe₂O₄ nanoparticles coated with PANI and SiO₂ against different bacteria and some standard antibacterial drugs. The present study revealed that the newly fabricated various Fe₃O₄ and MnFe₂O₄ nanocomposites, when combined with some different organic parts, are superiour antibacterial agents. Also, the synthesized nanocomposites can be easily separated from aqueous solution by magnetic filtration without any contamination of the medium.     

Synthesis and photocatalytic behaviors of Cr<Subscript>2</Subscript>O<Subscript>3</Subscript>–CNT/TiO<Subscript>2</Subscript> composite materials under visible light

Cr₂O₃–CNT/TiO₂ composites derived from chromium acetylacetonate, multi-walled carbon nanotubes (MWCNT) and titanium n-butoxide (TNB) were prepared, and the photocatalytic activity of the Cr₂O₃–CNT and CNT/TiO₂ composites was examined. The Cr₂O₃–CNT/TiO₂ composites were characterized by BET surface area measurement, X-ray diffraction, transmission electron microscopy, and energy dispersive X-ray analysis. The photocatalytic activity was determined from the decomposition of methylene blue (MB) under visible light irradiation. Methylene blue was photodegraded successfully in the presence of the Cr₂O₃–CNT/TiO₂ composite under visible light irradiation.     

Crystallization and microstructural evolution of MgO–Al<Subscript>2</Subscript>O<Subscript>3</Subscript>–SiO<Subscript>2</Subscript>–TiO<Subscript>2</Subscript>–La<Subscript>2</Subscript>O<Subscript>3</Subscript> glass-ceramics

Crystallization and microstructure of glasses with the molar compositions 1MgO·1.2Al₂O₃·2.8SiO₂·1.2TiO₂·xLa₂O₃ (x = 0.1 and 0.4) were thermally treated at different temperatures in the range from 950 to 1250 °C and then analyzed by X-ray diffraction and scanning electron microscopy, in combination with energy-dispersive X-ray spectroscopy and electron backscatter diffraction. It was found that the microstructure is first homogeneous with the precipitation of randomly distributed crystals and then indialite domains with embedded perrierite and rutile crystals are formed. For higher temperatures or prolonged times, more domains appear and expand into the bulk of the sample. Finally, the entire sample consists of the indialite domains and the boundaries that are enriched in rutile, perrierite, and magnesium aluminotitanate. Nevertheless, very distinct differences are observed between the samples with different La₂O₃ concentrations. For the sample with x = 0.4, the domains were detected at lower temperatures, while the quantity and size of the domains increase faster due to the promoted precipitation of indialite. For the sample with x = 0.1, in addition to the domain boundaries, secondary boundaries between the “regions” (assemblages of the domains) are observed in a larger length scale. The average size of the crystalline phases found between the “regions” is larger than that typically observed at the domain boundaries. The sizes of the crystals at the boundaries decrease with higher concentrations of La₂O₃, and the crystals (especially perrierite) within the domains become larger, resulting in a more homogeneous microstructure. This results in better dielectric properties, i.e., much higher quality factor for the sample with x = 0.4 in comparison to that with x = 0.1 after heat-treatment at 1150 or 1250 °C.     

Synthesis and characterization of TiO<Subscript>2</Subscript>–NiO and TiO<Subscript>2</Subscript>–WO<Subscript>3</Subscript> nanocomposites

TiO₂–NiO and TiO₂–WO₃ nanocomposites were prepared by hydrothermal and surface modification methods. The samples were analyzed using X-ray diffraction, Scanning Electron Microscope images, Transmission Electron Microscope, Energy dispersive analysis, Zeta potential, Electrophoretic mobility and Photocatalysis activity measurement. XRD data sets of TiO₂–NiO, TiO₂–WO₃ powder nanocomposite have been studied for the inclusion of NiO, WO₃ on the anatase-rutile mixture phase of TiO₂ by Rietveld refinement. The cell parameters, phase fraction, the average grain size, strain and bond lengths between atoms of individual phases have been reported in the present work. Shifted positional co-ordinates of individual atoms in each phase have also been observed.     

Enhanced microwave dielectric properties of Ba<Subscript>0.40</Subscript>Sr<Subscript>0.60</Subscript>TiO<Subscript>3</Subscript>–Zr<Subscript>0.80</Subscript>Sn<Subscript>0.20</Subscript>TiO<Subscript>4</Subscript> composite ceramics

The (1−x) Ba_0.40Sr_0.60TiO₃ (BST)−xZr_0.80Sn_0.20TiO₄ (ZST) composite ceramics with x = 10, 20, 30, and 40 wt% were fabricated by conventional solid-state reaction method. With increasing of ZST content, the dielectric constant of composite ceramics was decreased and dielectric loss increases. The effect of ZnO addition to 70 wt% BST–30 wt% ZST composition on the microstructure and dielectric properties was investigated. The improvements in dielectric constant, dielectric loss, and microwave dielectric properties of composite ceramics can be achieved by ZnO addition. The sample with 98 wt% (70 wt% BST–30 wt% ZST)–2 wt%ZnO composition exhibits promising dielectric properties, with dielectric constant, loss tangent and tunability at 4 kV/mm, of 125, 0.0016 and 12%, at 10 kHz and room temperature. At ~2 GHz, it possesses a dielectric constant of 101 and a Q factor of 187, which makes it a good candidate for tunable microwave device applications.     

Spectroscopic characterisation of local structure in Y<Subscript>2</Subscript>O<Subscript>3</Subscript>–B<Subscript>2</Subscript>O<Subscript>3</Subscript>–Bi<Subscript>2</Subscript>O<Subscript>3</Subscript> glasses doped with gadolinium

Gadolinium doped bismuth borate glasses containing up to 30 mol% Y₂O₃ were prepared by fast melt quenching method. The effect of yttrium on the local order in 3B₂O₃ · Bi₂O₃ and B₂O₃ · Bi₂O₃ glass matrices, particularly on the bismuth sites, was investigated by infrared (IR) spectroscopy and electron paramagnetic resonance (EPR) of Gd³⁺ ions. The IR results show that the local structure is more ordered in the glass system with higher bismuth content and the progressive addition of yttrium increases the local disorder in both bismuth–borate glass matrices. The EPR results indicate that Gd³⁺ ions occupy both bismuth and yttrium sites and reflect the same structural disorder like that suggested by IR results.     

The crystallographic orientation relationship between Al<Subscript>2</Subscript>O<Subscript>3</Subscript> and MgAl<Subscript>2</Subscript>O<Subscript>4</Subscript> in the composite material Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/Al–Mg–Si alloy

The formation mechanism of spinels on Al₂O₃ particles in the Al₂O₃/Al–1.0 mass% Mg₂Si alloy composite material has been investigated by transmission electron microscopy (TEM) in order to determine the crystallographic orientation relationship. A thin sample of the Al₂O₃/Al–Mg–Si alloy composite material was obtained by the FIB method, and the orientation relationship between Al₂O₃ and MgAl₂O₄, which was formed on the surface of Al₂O₃ particles, was discovered by the TEM technique as follows:

Structural investigation of V<Subscript>2</Subscript>O<Subscript>5</Subscript>–P<Subscript>2</Subscript>O<Subscript>5</Subscript>–K<Subscript>2</Subscript>O glass system with antibacterial potential

The xV₂O(1?x)[0.8 P₂O₅ ? 0.2 K₂O] glass system with 0 ≤ x ≤ 50 mol% was prepared and the structural changes induced in these glasses by increasing the vanadium oxide content were investigated by IR and ESR spectroscopies. The dual behaviour role of V₂O₅ oxide, as network modifier (for x ≤ 10 mol%) and the network former (x ≥ 20 mol%), as a consequence of phosphate network depolymerization and P–O–V and V–O–V linkages appearance was also highlighted. The antibacterial effect of the glasses with x ≤ 20 mol% V₂O₅ content was tested by optical density (OD) measurements. A linear correlation between the amount of vanadium and the antibacterial effect was evidenced.     

Extraction,detection, and profiling of serum biomarkers using designed Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@SiO<Subscript>2</Subscript>@HA core–shell particles

Serum biomarkers in the form of proteins (e.g. cluster of differentiation-44 (CD44)) have been demonstrated to have high clinical sensitivity and specificity for disease diagnosis and prognosis. Owing to the high sample complexity and low molecular abundance in serum, the detection and profiling of biomarkers rely on efficient extraction by materials and devices, mostly using immunoassays via antibody-antigen recognition. Antibody-free approaches are promising and need to be developed for real-case applications in serum to address the limitations of antibody-based techniques in terms of robustness, expense, and throughput. In this work, we demonstrated a novel approach using hyaluronic acid (HA)-modified materials/devices for the extraction, detection, and profiling of serum biomarkers via ligand-protein interactions. We constructed Fe₃O₄@SiO₂@HA particles with different sizes through layer-by-layer assembly and for the first time applied HA-functionalized particles in the facile extraction and sequence identification of CD44 in serum by mass spectrometry. We also first validated HA-CD44 binding through electrochemical sensing using HA-modified electrodes in both standard solutions and diluted serum samples, achieving a detection limit of ～0.6 ng/mL and a linear response range from 1 ng/mL to 10 μg/mL. Furthermore, we performed profiling of HA-binding serum proteome, providing a new preliminary benchmark for the construction of future databases, and we investigated selected surface chemistries of particles for the capture of proteins in serum. Our work not only resulted in the development of a platform technology for CD44 extraction/detection and HA-binding proteome identification, but also guided the design of ligand affinity-based approaches for antibody-free analysis of serum biomarkers towards diagnostic applications.

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Structural investigations of V<Subscript>2</Subscript>O<Subscript>5</Subscript>–P<Subscript>2</Subscript>O<Subscript>5</Subscript>–CaO glass system by FT-IR and EPR spectroscopies

xV₂O₅·(100 − x)[0.7P₂O₅·0.3CaO] glass system was obtained for 0 ≤ x ≤ 35 mol% V₂O₅. In order to obtain information regarding their structure, several techniques such as X-Ray diffraction, FT-IR, and EPR spectroscopies were used. X-Ray diffraction patterns of investigated samples are characteristic of vitreous solids. FT-IR spectra of 0.7P₂O₅·0.3CaO glass matrix and its deconvolution show the presence in the glass structure of all structural units characteristic to P₂O₅. Their number are increasing for x ≤ 3 mol% V₂O₅ then, for higher content of vanadium ions, the number of phosphate structural units are decreasing leading to a depolymerization of the structure. The structural units characteristic to V₂O₅ were not evidenced but their contribution to the glass structure can be clearly observed. EPR revealed a well resolved hyperfine structure (hfs) typical for vanadyl ions in a C_4v symmetry for x ≤ 3 mol% V₂O₅. For 5 < x < 20 mol% V₂O₅ the spectra show a superposition of two EPR signals one due to a hfs structure and another consisting of a broad line typical for associated V⁴⁺–V⁴⁺ ions. For x ≥ 20 mol% V₂O₅ only the broad line can be observed. The composition dependence of the line-width suggests the presence of dipole–dipole interaction between vanadium ions up to x ≤ 5 mol% V₂O₅ and superexchange interactions between vanadium ions for x > 5 mol% V₂O₅.     

Atomistic structure and energetics of interface between Mn-doped γ-Ga<Subscript>2</Subscript>O<Subscript>3</Subscript> and MgAl<Subscript>2</Subscript>O<Subscript>4</Subscript>

The interface between an Mn-doped γ-gallium oxide (Ga₂O₃) thin film and an MgAl₂O₄ (001) substrate has been investigated using high-resolution transmission electron microscopy (HRTEM), high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM), and first-principles calculations. A high-quality Mn-doped γ-Ga₂O₃ film with a defective spinel structure has been epitaxially grown by pulsed laser deposition. The γ-Ga₂O₃ crystal shows an uniform tetragonal distortion with a tetragonality of 1.05 throughout the film thickness of 75 nm. HRTEM and HAADF-STEM observations reveal that the γ-Ga₂O₃ and MgAl₂O₄ crystals form a coherent interface without any interfacial layers or precipitates. The atomistic structure and energies are theoretically evaluated for the interfaces with two types of termination plane, i.e., Mg- and Al₂O₄-termination of MgAl₂O₄. The cation sublattice is found to be continuous for both interfaces despite the defective spinel structure of Mn-doped γ-Ga₂O₃ with some vacant cation sites. The Al₂O₄-termination shows a lower interfacial energy than the Mg-termination under most conditions of the chemical potentials. This behavior is attributed to the energetic preference of the Mn–Al₂O₄ local configuration at the interface.     

Comparative study of multilayered ZnO/TiO<Subscript>2</Subscript>/ZnO and TiO<Subscript>2</Subscript>/ZnO/TiO<Subscript>2</Subscript> thin films prepared by sol–gel dip coating method

The aim of this research work is to represent the comparative study of ZnO/TiO₂/ZnO (ZTZ) and TiO₂/ZnO/TiO₂ (TZT) thin films deposited by sol–gel dip coating on FTO substrates. After deposition, the films were annealed at 500 °C for 1 h. Structural, surface morphology, optical and electrical properties of these films were studied by X-ray diffractrometer (XRD), Raman spectra, atomic force microscope (AFM), photoluminescence spectra (PL) and four point probe technique respectively. XRD and Raman spectra confirmed the anatase, brookite phases of TiO₂ and cubic phase of ZnO. AFM confirmed the formation of nano particles with average sizes of 18.4 and 47.2 nm of TZT and ZTZ films respectively. According to PL spectra, both the multilayer films slowdown the electron hole recombination rate and enhances the optoelectronic properties of the materials. Also it showed the peaks in the visible region of spectrum. The four point probe results showed that the average sheet resistivity of the films is 450 and 120 (ohm-m) respectively.