Microstructure and microwave dielectric properties of Al2O3 added Li2ZnTi3O8 ceramics

Recently, the rapid development of advanced communication systems increasingly strongly demands high-performance microwave dielectric ceramics in microwave circuits. Among them, Li₂ZnTi₃O₈ ceramics have been one of the most widely investigated species, due to its high quality factor, moderate firing conditions and low cost. However, the dielectric constants of the already reported Li₂ZnTi₃O₈ ceramics are fixed in a narrow range, limiting their wider applications. To adjust the dielectric constant of the Li₂ZnTi₃O₈ based ceramics, in this work Li₂ZnTi₃O₈ ceramics added with different amounts of Al₂O₃ (0–8?wt%) were prepared by conventional solid-state reaction. The microstructure and microwave dielectric properties of the samples were investigated. Due to the addition of Al₂O₃, the sintering temperature of the ceramics would be increased somewhat. Some Al³⁺ ions could substitute for Ti⁴⁺ ions in Li₂ZnTi₃O₈, and the added Al₂O₃ would react with ZnO to produce a ZnAl₂O₄ phase accompanying with the formation of TiO₂ phase, which would inhibit the growth of Li₂ZnTi₃O₈ grains. The dielectric constant of the finally obtained ceramics would be reduced from 26.2 to 17.9, although the quality factors of the obtained ceramics would decrease somewhat and the temperature coefficient of resonant frequency would deviate further from zero.     

微波水热法制备纳米Fe3O4粉体

通过微波水热法制备了纳米Fe3O4颗粒,并对其进行了Ostwald熟化处理。研究了油酸和氢氧化钠含量对纳米Fe3O4粒径大小以及分散性的影响。利用XRD、TEM等方式对所制备颗粒的结构、形貌进行了表征,结果表明,所制备的纳米Fe3O4粒子属于反尖晶石结构,通过微波加热未经熟化的纳米Fe3O4粒子结晶度较低,平均粒径为6nm。经过在180℃下熟化8h后,转化为结晶度较高,分散性较好,平均粒径为7nm的纳米Fe3O4颗粒。     

Resistance switching in electrodeposited polycrystalline Fe3O4 films

Resistance random access memory (RRAM) is an emerging nonvolatile memory that offers advantages of scalability, fast switching, and low voltages. Magnetite, Fe₃O₄, has been shown to exhibit resistance switching in nanoscale architectures such as superlattices. Here, we show that electrodeposited polycrystalline films of Fe₃O₄ exhibit multistate resistance switching. Experiments suggest that the insulator-to-metal transition may be facilitated by the presence of a thin nano-crystalline layer which is critical for resistance switching to occur at lower bias. We also show that the switching behavior can be tuned through the applied deposition potential. The multiple resistance states accessible in these simple architectures open up new possibilities for multi-bit data storage and retrieval.     

Evidence of redox interactions between polypyrrole and Fe3O4 in polypyrrole-Fe3O4 composite films

The electrical properties of conducting polymers make them useful materials in a wide number of technological applications. In the last decade, an important effect on the properties of the conducting polymer when iron oxides particles are incorporated into the conductive matrix was shown. In the present study, films of polypyrrole were synthesized in the presence of magnetite particles. The effect of the magnetite particles on the structure of the polymer matrix was determined using Raman spectroscopy. Mass variations at different concentrations of Fe₃O₄ incorporated into the conducting matrix were also measured by means of quartz crystal microbalance. Additionally, the changes in the resistance of the films were evaluated over time by electrochemical impedance spectroscopy in solid state. These results show that the magnetite incorporation decreases polymeric film resistance and Raman experiments have evidenced that the incorporation of magnetite into polymeric matrix not only stabilizes the polaronic form of the polypyrrole, but also preserves the polymer from further oxidation.     

Adsorption of organic layers over electrodeposited magnetite (Fe3O4) thin films

The formation of monolayers of two organic compounds (oleic acid and dodecanethiol) over magnetite films was studied. Magnetite films ranging from 80 nm to 3.75 μm-thick were electrodeposited on Au on glass substrates under galvanostatic control, with deposition parameters optimized for minimum surface roughness. Films were characterised by SEM and AFM, showing granular deposits with a low rms roughness of 5–40 nm measured over an area of 1 μm². The growth rate was estimated by measuring cross-sections of the thin films. Pure magnetite with an fcc structure is observed in XRD diffractograms. The adsorption of both oleic acid and dodecanethiol on the magnetite films was tested by immersing them in ethanol solutions containing the organic molecules, for different deposition time, temperature and cleaning procedure. Monolayer formation in both cases was studied by contact angle and voltammetric measurements, as well as XPS.     

Synthesis of core-shell structured PS/Fe3O4 microbeads and their magnetorheology

Most magnetic materials possess serious sedimentation problem due to their large density when they are adopted as magnetorheological (MR) materials. In this communication, we fabricated novel core-shell structured polystyrene(PS)/Fe₃O₄ microbeads via a facile method. Porous morphology of the PS obtained by etching silica particles and the loaded Fe₃O₄ was observed via both SEM and TEM images. XRD pattern confirms crystalline structure of the synthesized iron species. VSM data indicate the change in saturation magnetization before and after introducing organic PS core. Finally, MR performances of the PS/Fe₃O₄ based MR fluid were investigated via a rotational rheometer and sedimentation stability was found to be improved with a decreased density of the synthesized microbeads.     

Room temperature in situ chemical synthesis of Fe3O4/graphene

A simple, cost-effective, efficient, and green approach to synthesize iron oxide/graphene (Fe₃O₄/rGO) nanocomposite using in situ deposition of Fe₃O₄ nanoparticles on reduced graphene oxide (rGO) sheets is reported. In the redox reaction, the oxidation state of iron(II) is increased to iron(III) while the graphene oxide (GO) is reduced to rGO. The GO peak is not observed in the X-ray diffraction (XRD) pattern of the nanocomposite, thus providing evidence for the reduction of the GO. The XRD spectra do have peaks that can be attributed to cubic Fe₃O_4. The field emission scanning electron microscopy (FESEM) images show Fe₃O₄ nanoparticles uniformly decorating rGO sheets. At a low concentration of Fe²⁺, there is a significant increase in the intensity of the FESEM images of the resulting rGO sheets. Elemental mapping using energy dispersive X-ray (EDX) analysis shows that these areas have a significant Fe concentration, but no morphological structure could be identified in the image. When the concentration of Fe²⁺ is increased, the Fe₃O₄ nanoparticles are formed on the rGO sheets. Separation of the Fe₃O₄/rGO nanocomposite from the solution could be achieved by applying an external magnetic field, thus demonstrating the magnetic properties of the nanocomposite. The Fe₃O₄ particle size, magnetic properties, and dispersibility of the nanocomposite could be altered by adjusting the weight ratio of GO to Fe²⁺ in the starting material.     

Synthesis and strengthened microwave absorption properties of three-dimensional porous Fe3O4/graphene composite foam

The three-dimensional porous Fe₃O₄/graphene composite foam as a new kind of absorbing composite with electrical loss and magnetic loss was successfully synthesized by a facile method. Fe₃O₄ was evenly attached on structure of graphene sheets which overlapped with each other to form three-dimensional porous graphene foam. The results revealed that when the mass ratio of graphene oxide (GO) and Fe₃O₄ was 1:1, the Fe₃O₄/graphene composite foam possessed the best absorption properties: the minimum reflection loss was up to ??45.08?dB when the thickness was 2.5?mm and the bandwidth below ??10?dB was 6.7?GHz when the content of the composite foam absorbents was just 8%. The micron-sized three-dimensional porous structure provided more propagation paths, enhancing the energy conversion of incident electromagnetic waves. The addition of Fe₃O₄ contributed to improving the impedance matching performance and magnetic loss. The three-dimensional porous Fe₃O₄/graphene composite foam was a kind of high-efficiency wave absorber, providing a new idea for the development of microwave absorbing materials.     

Assembled porous Fe3O4@g-C3N4 hybrid nanocomposites with multiple interface polarization for stable microwave absorption

Magnetic/dielectric composites can offer good electromagnetic impendence. However, the strategy for embodying strong absorbing ability and broad effective absorption band simultaneously is a significant challenge. Therefore, assembled porous Fe₃O₄@g-C₃N₄ hybrid nanocomposites have been designed and synthesized, in which porous Fe₃O₄ nanospheres assembled by ~ 3?nm Fe₃O₄ nanoparticles are surrounded by g-C₃N₄. The introduction of g-C₃N₄ improves dielectric loss ability at 2–18?GHz and magnetic loss ability at 2–10?GHz, and enhances attenuation constant, and increases electromagnetic impedance degree. These merits ensure that assembled porous Fe₃O₄/g-C₃N₄ hybrid nanocomposites deliver superior microwave absorption performance, such as effective absorption bandwidth, f_E, (reflection loss less ??10?dB) exceeding 5?GHz at 2.0–2.3?mm, the maximal f_E of 5.76?GHz and minimal reflection loss of at least ??20?dB with thickness ranging from 2.3 to 10.0?mm, avoiding the sensitivity of absorption properties to absorbing layer thickness. Stable microwave absorbing performance originates from multi-interfacial polarization, multi-reflection, enhanced electromagnetic loss capability, and good electromagnetic impedance. Our study offers a new idea for stable microwave absorber at 2–18?GHz.     

Water-soluble,mesoporous Fe3O4: Synthesis,characterization, and properties

Water-soluble, mesoporous Fe₃O₄ nanopowder is successfully prepared by one-step thermal decomposition of an iron-urea complex ([Fe(NH₂CONH₂)₆](NO₃)₃) in triethylene glycol (TEG). The formation of Fe₃O₄ is confirmed from X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and selected area electron diffraction (SAED) measurements. The morphological and structural properties of the Fe₃O₄ nanopowder are characterized by transmission electron microscopy (TEM), nitrogen adsorption–desorption, and thermogravimetric analysis (TGA). Monodisperse, nearly spherical and highly crystalline Fe₃O₄ nanoparticles are obtained by this method. The Fe₃O₄ nanopowder is well dispersed in water and ethanol with a mesoporous structure, average pore size of 3.6 nm, and Brunauner–Emmett–Teller (BET) surface area of 122 m²/g. The room temperature magnetization hysteresis curve exhibits barely measurable values for coercivity and remanence, suggesting that the Fe₃O₄ nanopowder possesses superparamagnetic characteristics.     

Synthesis of high magnetization hydrophilic magnetite (Fe3O4) nanoparticles in single reaction—Surfactantless polyol process

High magnetization hydrophilic magnetite nanoparticles have been synthesized in two different batches with mean particle sizes of 32.3 and 9.2 nm by inexpensive and surfactant-free facile one-pot modified polyol method. In the synthesis, polyethylene glycol was used as a solvent media and it has been found to play a key role to act as a reducing agent as well as a stabilizer simultaneously. It was shown that the size of the nanoparticles can be effectively controlled by modifying the reaction parameters such as reaction temperature, time and polyol/metal precursor ratio. X-ray diffraction and energy dispersive spectroscopy studies confirm the formation of a pure magnetite phase without the presence of any other phases. Transmission electron microscopy and the Fourier transform infrared spectroscopy results reveal that the particle size and surface adsorption properties are very much dependent on reaction parameters. The magnetic properties of the samples measured by physical property measurement system have shown that the as-synthesized magnetite nanoparticles possess a high magnetization of 85.87 emu/g at 300 K and 91.7 emu/g at 5 K with negligible coercivities. The structural and magnetic characterizations of these polyol coated, hydrophilic, monodisperse, superparamagnetic nanoparticles clearly indicate that they are suitable for biomedical applications.     

Microstructure and dielectric properties control of Ba4(Nd0.7Sm0.3)9.33Ti18O54 microwave ceramics

Microwave ceramics of Ba₄(Nd_0.7Sm_0.3)_9.33Ti₁₈O₅₄ with 0–3 wt% Ag additions were synthesized by a citrate sol–gel method. The BaO–B₂O₃–SiO₂ glass was also added into the sol–gel derived BNST ceramic powders as sintering aids. The undoped, Ag- and BaBS-doped samples can be sintered at 1250 °C, 1150 °C and 1000 °C, respectively. The microstructure and dielectric properties were then controlled by doping Ag or BaBS glass. Near isoaxial grains with about 250 nm and typical columnar grains were obtained for the silver-doped and BaBS-doped samples, respectively. For the <1 wt% silver-doped samples, the dielectric constant and Q × f retained unaltered but τ_f decreased from 9 ppm/°C to 1.4 ppm/°C. With increasing silver content from 1 wt% to 3 wt%, the dielectric constant and τ_f significantly increased but Q × f decreased. For the BaBS-doped samples, both dielectric constant and Q × f decreased but τ_f increased with increasing BaBS content.     

Structure,morphology and magnetic properties of Au/Fe3O4 nanocomposites fabricated by a soft aqueous route

Magnetic Fe₃O₄ (magnetite) nanoparticles are synthesized via a chemical precipitation route in different alkaline environments (NH₃ or NaOH) and subsequently functionalized with a (propynylcarbamate)triethoxysilane moiety, with the aim of promoting the nucleation and subsequent stabilization of gold nanoparticles. The propynylcarbamate group is able to capture the gold precursor (HAuCl₄), spontaneously reduce it, and stabilize the resulting Au nanoaggregates. The obtained results show that though the dimensions of the starting magnetite substrate depend on the base used in the preparation, they remain unaltered upon the subsequent modification. Conversely, the average Au nanoparticle dimensions can be conveniently tailored as a function of the base used in Fe₃O₄ preparation and the presence/absence of the organic functionalization. The smallest dimensions (15?nm) are obtained for AuNP supported on propynylcarbamate-functionalized Fe₃O₄ prepared in the presence of ammonia. Magnetization measurements highlight that all the Au/Fe₃O₄ nanocomposites display a superparamagnetic behavior and those obtained using ammonia showed consistently smaller Hc and Mr values (av. values of 7.4?Oe and 0.8?emu/g) than those prepared with sodium hydroxide (av. values of 28?Oe and 2.8?emu/g).     

On the mechanical and biological properties of bredigite-magnetite (Ca7MgSi4O16-Fe3O4) nanocomposite scaffolds

The aim of the present study was to study the mechanical and biologocal properties of the bredigite-magnetite (Ca₇MgSi₄O₁₆-Fe₃O₄) nanocomposite with various amounts of magnetite (0, 10, 20 and 30 wt%). According to the obtained results, the properties of the constructed scaffolds have an extreme dependence on the magnetite content. In this research, the bredigite-30 wt% magnetite as the optimum sample showed a fracture toughness of 2.69 MPa m^1/2 and a Young's modulus of 29 GPa. Increasing bredigite content led to the increase of pH values in the SBF solution. This was originated from the interchange/interaction of Ca²⁺ ion on the scaffold surface. The sample containing 10 wt% magnetite presented a rocky and irregular surface while that of 30 wt% illustrated a smooth and flat outer layer with coarse projections. The results confirmed that the biodegradation rate of the pure bredigite is more than that of 20 wt% sample. The event is originated from the dissolution of the Si ions of the bridigite particles in the absence of magnetite.     

Evolution of microstructure and electrical properties of Aurivillius phase (CaBi4Ti4O15)1-x(Bi4Ti3O12)x ceramics

(CaBi₄Ti₄O₁₅)_1-x(Bi₄Ti₃O₁₂)_x (CBT-xBIT) Aurivillius phase ceramics were synthesized by the conventional solid reaction method. The evolution of the structure and the electrical properties of CBT-xBIT ceramics were systematically investigated. Due to the enhanced spontaneous polarization induced by internal stresses on the Bi₂O₂ layers in the CBT-xBIT structure, the optimal piezoelectric coefficient (d₃₃ ~ 13?pC/N) was obtained in the ceramics with x?=?0.3 while exhibiting a relatively good thermal stability in the temperature range of 20–700?°C. The dc resistivity (ρ_dc) of the CBT-xBIT ceramics exhibited a higher value (≥?10⁹ Ω?cm) at room temperature, and the tan δ value of CBT-xBIT (x= 0, 0.1 and 0.3) within the temperature range of 20–500?°C maintained stability as a result of the domain structure and point defect concentration in the ceramics. In addition, a distinctive double dielectric peak anomaly was observed in the ε_r-T curves of the CBT-xBIT (x= 0.3, 0.5 and 0.7) ceramics, and it plays a remarkable role in the thermal stability of the piezoelectricity of CBT-xBIT ceramics. As a result, such research can benefit high temperature practical piezoelectric devices.     

Corrosion mechanisms of Al2O3/MgAl2O4 by V2O5, NiO, Fe2O3 and vanadium slag

The effects of V₂O₅, NiO, Fe₂O₃ and vanadium slag on the corrosion of Al₂O₃ and MgAl₂O₄ have been investigated. The specimens of Al₂O₃ and MgAl₂O₄ with the respective oxides above mentioned were heated at 10 °C/min from room temperature up to three different temperatures: 1400, 1450 and 1500 °C. The corrosion mechanisms of each system were followed by XRD and SEM analyses. The results obtained showed that Al₂O₃ was less affected by the studied oxides than MgAl₂O₄. Alumina was only attacked by NiO forming NiAl₂O₄ spinel, while the MgAl₂O₄ spinel was attacked by V₂O₅ forming MgV₂O₆. It was also observed that Fe₂O₃ and Mg, Ni, V and Fe present in the vanadium slag diffused into Al₂O₃. On the other hand, the Fe₂O₃ and Ca, S, Si, Na, Mg, V and Fe diffused into the MgAl₂O₄ structure. Finally, the results obtained were compared with those predicted by the FactSage software.     

Crystal structure and electrochemical performance of Li3V2(PO4)3 synthesized by optimized microwave solid-state synthesis route

To investigate the crystal structure and electrochemical performance of samples synthesized under different microwave solid-state synthesis condition, a series of Li₃V₂(PO₄)₃ samples has been synthesized at five different temperatures for 3-5 min and at 750 °C for various time. The as-synthesized Li₃V₂(PO₄)₃ samples are characterized and studied by ICP-AES analysis, X-ray diffraction (XRD), Rietveld analysis, scanning and transmission electron microcopy (SEM and TEM). At relatively lower temperature (650 °C) and very short reaction time (3 min), pure phase of Li₃V₂(PO₄)₃ could be synthesized in microwave irradiation field. The crystal structure and Li atomic fractional coordinate present a significant deviation upon the change of microwave irradiation temperature and time. Relatively, the diffusion ability of lithium cations and the electrochemical performance are affected. Under the proper reaction temperature and time, the carbon-free samples MW750C5m and MW850C3m show the best specific discharge capacity 126.4 and 132 mAh g⁻¹ at the voltage range of 3.0-4.3 V, near the reversible cycling of two lithium ions per Li₃V₂(PO₄)₃ formula unit (133 mAh g⁻¹). At the voltage range of 3-4.8 V, the sample MW750C5m presents the best initial specific charge capacity of 197 mAh g⁻¹, equivalent to the reversible cycling of three lithium ions per Li₃V₂(PO₄)₃ formula unit (197 mAh g⁻¹). The initial discharge capacity, the samples MW750C5m and MW850C3m present high specific discharge capacity 183.4 and 175.7 mAh g⁻¹, respectively. The relationship among microwave irradiation condition, crystal structure, lithium atomic fractional coordinates and the electrochemical performance have been discussed in detail.     

Fe3O4磁粉的合成与结构表征

采用化学共沉淀法制备纳米磁性Fe3O4粒子。选用NH3.H2O作为沉淀剂,加入到Fe2+和Fe3+的混合盐溶液中,制得了纳米磁性Fe3O4粒子。考察了影响产物粒径的一些实验因素。通过X-Ray谱图证实了产物结构特征,平均粒径在37 nm左右,平均晶粒度只有28 nm左右的均分散。     

Mixtures of carbon and Ni/Al2O3 as catalysts for the microwave-assisted CO2 reforming of CH4

In this work, the microwave-assisted CO₂ reforming of CH₄ over mixtures of carbonaceous materials and an in-lab prepared Ni/Al₂O₃ was studied. Ni/Al₂O₃ is not heated by microwave radiation, and for this reason, microwave receptors, such as carbonaceous materials, must be mixed with this catalyst. In order to evaluate the role of the carbonaceous component of the blend, two different carbonaceous materials were used: an activated carbon, FY5, and a metallurgical coke, CQ. The carbonaceous component acted not only as microwave receptor but also as catalyst and, consequently, it influenced the catalytic activity of the mixture. FY5 + Ni/Al₂O₃ was found to be a better catalyst than CQ + Ni/Al₂O₃, since FY5 on its own showed a better catalytic activity than CQ. Ni/FY5, which consists of Ni impregnated directly onto the microwave receptor, was also evaluated as a catalyst. It was found that the catalytic activity of the mixture FY5 + Ni/Al₂O₃ was better than that of Ni/FY5. Finally, the influence of the heating device on the catalytic activity of FY5 + Ni/Al₂O₃ was studied. Conversions over FY5 + Ni/Al₂O₃ and microwave heating were found to be similar to conversions over Ni/Al₂O₃ and conventional heating.     

Microwave assisted hydrothermal synthesis of (Fe,Co)3O4 nanoparticles in the presence of surfactants and effects of Co/Fe ratio on microstructure and magnetism

Microstructure and magnetic properties of nanoparticles can be tailored by optimising the synthesis procedure and changing chemical composition. In this study, a two-step procedure, i.e., coprecipitation in the presence of PEG 300 followed by microwave assisted (MW) hydrothermal synthesis, was introduced to obtain Co_xFe_3-xO₄ (x?=?0, 0.1 and 0.2) nanoparticles. It was found that with the increase of Co content, particle/crystallite size increased, with significant change of coercivity (H_c). The mixed samples of Co_xFe_3-xO₄ (x?=?0.1 and 0.2) were magnetically harder in comparison with Fe₃O₄. Тhe H_c of Fe₃O₄ was 91?Oe, while for Co_0.10Fe_2.90O₄ and Co_0.20Fe_2.80O₄, H_c was 256?Oe and 1070?Oe, respectively. Saturation magnetisation (M_s) of mixed samples also increased up to 6% compared to Fe₃O₄. A special effort was devoted to study the effects of introducing different surfactants (PEG 300, PEG 4000 or SDS) during the synthesis procedure in order to improve morphological and microstructural properties of CoFe₂O₄ nanoparticles. The influence of surfactants on physical/chemical properties of nanoparticles is discussed.