Synthesis of magnetic Pb/Fe3O4/SiO2 and its catalytic activity for propylene carbonate synthesis via urea and 1,2-propylene glycol

To facilitate the recovery of Pb/SiO₂ catalyst, magnetic Pb/Fe₃O₄/SiO₂ samples were prepared separately by emulsification, sol-gel and incipient impregnation methods. The catalyst samples were characterized by means of X-ray diffraction and N₂ adsorption-desorption, and their catalytic activity was investigated in the reaction for synthesizing propylene carbonate from urea and 1,2-propylene glycol. When the gelatin was applied in the preparation of Fe₃O₄ at 60°C and the pH value was controlled at 4 in the preparation of Fe₃O₄/SiO₂, the Pb/Fe₃O₄/SiO₂ sample shows good catalytic activity and magnetism. Under the reaction conditions of a reaction temperature of 180°C, reaction time of 2 h, catalyst percentage of 1.7 wt-% and a molar ratio of urea to PG of 1:4, the yield of propylene carbonate attained was 87.7%.     

Graphene oxide–Fe2O3 hybrid material as highly efficient heterogeneous catalyst for degradation of organic contaminants

Graphene oxide–Fe₂O₃ (GO–Fe₂O₃) hybrid material was synthesized as a heterogeneous catalyst for photo-Fenton degradation of organic contaminants by an easy and scalable impregnation. X-ray diffraction analysis and high-resolution transmission electron microscope analysis confirm the existence of the Fe₂O₃ nanoparticles in the GO–Fe₂O₃ catalyst. Fourier transform infrared spectroscopy analysis proves that the combination of Fe₂O₃ and GO sheet is due to the metal–carbonyl coordination. The catalytic activities of the GO–Fe₂O₃ catalyst were evaluated by the degradation of Rhodamine B and 4-nitrophenol under visible light irradiation (>420 nm) in the presence of hydrogen peroxide. The results show that the catalyst exhibited excellent catalytic property at a wide pH range of 2.09–10.09 and stable catalytic activity after seven recycles, which could be attributed to the synergetic effects of the adsorptive power of GO and the hydroxyl radicals produced by heterogeneous photo-Fenton reactions. The present results suggest that the GO–Fe₂O₃ hybrid material can act as an efficient heterogeneous catalyst for degradation of organic contaminants, which may provide insight into the design and development of high-efficiency visible-light photocatalyst for water treatment.     

Structural and thermoelectric properties of hydrothermal-processed Ag-doped Fe2O3

Fe_2-xAg_xO₃ (0?≤?x?≤?0.04) nanopowders with various Ag contents were synthesized at different hydrothermal reaction temperatures (150?°C and 180?°C). Their structural properties were fully investigated through an X-ray diffraction, a Fourier transform infrared spectroscopy, and an X-ray photoelectron spectroscopy. The hydrothermal reaction temperature, time, and Ag content remarkably affected the morphological characteristics and crystal structure of the synthesized powders. The Fe_2-xAg_xO₃ (0?≤?x?≤?0.04) powders synthesized at 150?°C for 6?h and the Fe_2-xAg_xO₃ (0.02?≤?x?≤?0.04) powders synthesized at 180?°C for 12?h formed the orthorhombic α-FeOOH phase with a rod-like morphology, whereas the Fe_2-xAg_xO₃ (0?≤?x?≤?0.01) powders synthesized at 180?°C for 12?h formed the rhombohedral α-Fe₂O₃ phase with a spherical-like morphology. The Fe_1.98Ag_0.02O₃ fabricated by utilizing Fe_1.98Ag_0.02O₃ powders synthesized at 180?°C showed the largest power factor (0.64?×10^?5 Wm^?1 K^?2) and dimensionless figure-of-merit (0.0036) at 800?°C.     

Novel synthesis method and microstructure evolution of Ti3C2(OH)2/K2Ti8O17 nanocomposites as an effective surface enhanced Raman scattering substrate

In this paper, we have developed a mild and facile approach using KOH solution as etchants to corrode Ti₃SiC₂ at room temperature, fabricating novel Ti₃C₂(OH)₂/K₂Ti₈O₁₇ nanocomposites with open network structures and abundant surface functional groups. The as-produced products obtain the excellent surface enhanced Raman scattering (SERS) performance in the determination of crystal violet (CV), rhodamine 6G (R6G) and methylene blue (MB) dye molecules. The enhancement factors of the three can be calculated to be 3.98 × 10⁵, 1.78 × 10⁵ and 5.27 × 10⁵, and the Raman signals can be detected at the concentrations as low as 10^?6 M, 10^?8 M and 10^?6 M, respectively, suggesting the potential for reliable SERS substrates. In this regard, this work provides a new strategy for exploring and synthesizing MAX phase-derived nanomaterials as promising SERS substrates for high-sensitive molecular detection.     

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.     

Multiferroic and magnetoelectric properties of lead-free Ba0.8Sr0.2Ti0.9Zr0.1O3-Ni0.8Zn0.2Fe2O4 composite films with different deposition sequence

Ba_0.8Sr_0.2Ti_0.9Zr_0.1O₃/Ni_0.8Zn_0.2Fe₂O₄(BN) and Ni_0.8Zn_0.2Fe₂O₄/Ba_0.8Sr_0.2Ti_0.9Zr_0.1O₃ (NB) composite film were deposited on Pt/Ti/SiO₂/Si substrates by the sol-gel method and spin-coating method. The results show that the deposition sequences of the composite films have significant influence on the ferroelectric, ferromagnetic and magnetoelectric properties of the composite films. Two composite films possess not only good ferroelectric and ferromagnetic properties but good magnetoelectric properties as well. The NB composite film has clear interface between the ferroelectric film and ferromagnetic film and possesses greater magnetoelectric coupling effect than the BN composite film under the same H_bias. The maximum value of α_E is 70.14?mV?cm^?1 Oe^?1 was obtained in the NB composite film when H_bias is 638?Oe.     

Effect of substrate on the microstructure and thermoelectric performances of Sr-doped Ca3Co4O9 thick films

Ca₃Co₄O₉ thermoelectric materials in form of thick films are very promising in practical applications due to their low costs and relatively high performance. In this work, two different suspensions have been used to produce different coatings on Al₂O₃ polycrystalline substrates with theoretical green thickness of 360 and 2000?µm. Moreover, the effect of substrate has also been investigated using Al₂O₃ monocrystalline substrates and a 360?µm green thickness. Sintering procedure at 900?°C for 24?h has drastically decreased coating thickness. XRD performed on the coatings surface has shown the formation of small amounts of Ca₃Co₂O₆ secondary phase on the polycrystalline substrates, while it was more abundant, and accompanied by Ca₂Co₂O₅ on the monocrystalline substrates. In spite of the higher secondary phases content, monocrystalline substrates produced a slight grain orientation which led to the highest thermoelectric properties between the samples (0.38?mW/K²m at 800?°C), and very close to the best reported values in the literature.     

Construction of Z-scheme type CdS–Au–TiO2 hollow nanorod arrays with enhanced photocatalytic activity

The Z-scheme type CdS–Au–TiO₂ hollow nanorod arrays have been constructed on glass substrates by following these simple steps: firstly, highly ordered TiO₂ hollow nanorod arrays (THNAs) were synthesized by liquid phase deposition (LPD) using ZnO nanorod arrays as templates; then both Au core and CdS shell nanoparticles were achieved on the THNAs by in situ photodeposition. The prepared three-component films were characterized by field-emission scanning electron microscopy (FSEM), high-resolution transmission electron microscope (HRTEM), Raman scattering and ultraviolet–visible absorption spectrum. The results showed that Au–CdS core–shell nanoparticles were well dispersed on wall of anatase THNAs from top to bottom. The three-component nanojunction system was evaluated for their photocatalytic activity through the degradation of methylene blue (MB) in aqueous solution. It was found that the CdS–Au–TiO₂ three-component hollow nanorod arrays exhibited significantly enhanced photocatalytic activity compared with single (THNAs) and two components (Au-THNAs or CdS-THNAs) systems. Reasons for this enhanced photocatalytic activity were revealed by photoluminescence (PL) results of our samples.     

Effects of pore diameter and catalyst loading in hydroliquefaction of coal with CoO/MoO3/Al2O3 catalysts

The effect of catalyst pore size has been studied for the hydroliquefaction of a West Virginia coal in the presence of Co/Mo/Al₂O₃ catalyst. The alumina supports used for catalyst preparation had relatively sharp, unimodal pore size distribution with average pore diameters in the range of 100 Å to almost 1000 Å. Loading of MoO₃ and CoO on the Al₂O₃ supports was in the constant weight ratio of 5:1, but the absolute loading was in direct proportion to the surface area of the support. Two series of catalyst were studied: “High loading”, with 9.7 × 10^?4 g MoO₃/m² Al₂O₃, and “low loading”, with 4.5 × 10^?4 g MoO₃/m² Al₂O₃; both loadings were less than the amount necessary for monolayer distribution of MoO₃ on Al₂O₃. The weight of catalyst charged in each autoclave run was varied so that the same weight of MoO₃ and CoO was present for each experiment.The principal results were: (1) Al₂O₃ alone is not catalytic, even in large amount; (2) conversion of coal increases as catalyst pore diameter increases; from 100 Å to at least 500 Å; (3) the increased conversion with increasing pore size is manifested mainly as increased yield of asphaltenes at 400°C, so the ratio of oil to oil-plus-asphaltenes decreases as pore diameter increases; and (4) catalysts with “low loading” of MoO₃ and CoO on the Al₂O₃ surface give higher liquefactions than their counterparts with “high loading”. Most of the results are consistent with an expected low diffusion rate of large, coal-derived molecules through the catalyst pore system. The higher liquefaction with “low loading” of the Al₂O₃ surface might result from slow desorption of large product molecules (asphaltenes) exhibiting multiple-site adsorption to Mo neighbors on the surface.     

Novel iron-rich mullite solid solution synthesis using fused-silica and α-Al2O3 powders

An iron-rich mullite solid solution was synthesized by using α-Al₂O₃, fused-silica and Fe₂O₃ powders at elevated temperatures. The phase compositions and microstructures of the synthesized samples were characterized by X-ray diffraction (XRD), energy dispersive spectrometer (EDS) and field emission scanning electron microscope (FESEM). The occurrence states of Fe²⁺ and Fe³⁺ at different temperatures were analysed by X-ray photoelectron spectroscopy (XPS). The influence and the reaction mechanism of Fe₂O₃ addition on the synthesis of the mullite solid solution were clarified. The results showed that with the addition of Fe₂O₃, a liquid-solid sintered state was formed at 1300–1400?°C, which leaded to a reduction in the mullitization temperature. After sintering at 1600?°C, the quantitative analysis showed that the mullite phase content was 100%. Meanwhile, the Fe^3+/2+ ions entered completely into the mullite to form a stable solid solution, which exhibited the crystal morphology of a spherical shape and a short columnar shape with a low aspect ratio. The crystal grains were interwoven and squeezed each other, showing good structural stability. The refractoriness under load (RUL) property of the sample sintered at 1700?°C was slightly higher than that of the sample sintered at 1600?°C.     

Efficient degradation of methylene blue dye by catalytic oxidation using the Na8Nb6O19·13H2O/H2O2 system

Na₈Nb₆O₁₉·13H₂O particles were synthesized by a simple hydrothermal method. The catalysts were characterized by X-ray diffraction (XRD), scanning electronic microscopy (SEM) and thermogravimetric and differential scanning (TG-DSC). The XRD and TG-DSC analyses indicated that Na₈Nb₆O₁₉·13H₂O was an intermediate hexaniobate during the preparation of NaNbO₃ powders. Methylene blue (MB) dye degradation using Na₈Nb₆O₁₉·13H₂O/H₂O₂, Nb₂O₅/H₂O₂ and NaNbO₃/H₂O₂ systems were investigated, respectively. Among the catalytic oxidation systems, Na₈Nb₆O₁₉· 13H₂O showed the highest activity for degradation of MB in the presence of H₂O₂. The results indicated that the dye degradation efficiency could be 93.5% at 30 °C after 60 min in the presence of the Na₈Nb₆O₁₉·13H₂O/H₂O₂ system. It was also found that the degradation of MB over the catalytic systems followed pseudo-first-order kinetics, and the degradation rate was 0.02376 min⁻¹ in the Na₈Nb₆O₁₉·13H₂O/H₂O₂ system, which was higher than that in the Nb₂O₅/H₂O₂ and NaNbO₃/H₂O₂ systems. A possible mechanism for MB catalytic oxidation degradation using the Na₈Nb₆O₁₉·13H₂O/H₂O₂ system was proposed.     

Photocatalytic reactions of imazamox at TiO2, H2O2 and TiO2/H2O2 in water interfaces: Kinetic and photoproducts study

The photocatalytic transformation of imazamox, a herbicide of imidazolinone family, is investigated in aqueous solution containing titanium dioxide, hydrogen peroxide or the combination of TiO₂/H₂O₂ under simulated sunlight irradiation. The effect of parameters such as the amount of catalysts, the concentration of herbicide, and the pH were investigated by measurement of the rate constant of degradation. Experimental data obtained under different conditions describe the dependency of degradation rate on the above mentioned parameters. Consequently, kinetic parameters were experimentally determined and a pseudo-first-order kinetic was observed. Mulliken charge distributions calculated by the DFT method B3LYP/6–31+G(d) level of theory for key cationic, anionic and neutral structures of imazamox give interpretation for the dependency of photodegradation rate constant on pH. The degradation rate constants were always higher for the heterogeneous catalysis in reactions (TiO₂/UV, TiO₂/UV/H₂O₂) compared to the homogeneous systems (UV alone, H₂O₂/UV). In parallel, five photoproducts could be tentatively identified using Electrospray ionization Fourier transform ion cyclotron resonance mass spectroscopy based on precise chemical formula assignments.     

Synthesis of MFe2O4 (M=Mg2+, Zn2+, Mn2+) spinel ferrites and their structural,elastic and electron magnetic resonance properties

Structural, elastic and electron magnetic resonance investigations of spinel ferrites with the formula MFe₂O₄ (M = Mg²⁺, Zn²⁺, Mn²⁺) synthesized by the sol-gel auto-combustion method are reported here. XRD patterns revealed the co-existence of secondary phases along with the ferrite phase. The lattice parameter (8.301?Å, 8.366?Å and 8.434?Å) was found to be varying according to the ionic radii of cations. As determined by scanning electron microscopy (SEM), ZnFe₂O₄ has a comparatively narrow distribution of grain sizes (1.3–3.8?µm) compared to those in MnFe₂O₄ (0.8–4.3?µm) and MgFe₂O₄ (0.3–4.8?µm). The estimated values of average crystallite sizes (17.5?nm, 21.3?nm and 23.3?nm) determined from the X-ray diffraction peaks are considerably less than the average grain sizes (1.3?µm, 1.6?µm and 2.7?µm) estimated from the SEM histograms. The vibrational frequencies in FTIR spectra are in the conformity with the cubic spinel structure and their variation supports the variation of lattice parameter. Equal values of Poission's ratio (0.35) were obtained for the three systems which represent the isotropic behaviour of spinel ferrite systems. The exceptional low value of Lande's g-parameter for ZnFe₂O₄ indicates the dominance of Fe³⁺–O–Fe³⁺ superexchange interaction. Though cation redistribution is possible in the present ferrite systems, the secondary phases existed in these ferrite systems are predominantly influencing the structural, elastic and electron magnetic resonance properties.     

The system CaOAl2O3Fe2O3 with added fluoride flux

Effects of fluoride fluxes, especially CaSiF₆·2H₂O upon phase equilibria in the system CaOAl₂O₃Fe₂O₃ are described, presenting liquidus data, new phase field boundaries and invariant points and solid solution areas. The primary phase field for C_12?xA₇·CaF₂ is increased substantially in size, and liquidus or invariant temperatures are depressed by amounts ranging from 20 to 80°C.     

Preparation of Al2O3 and MgAl2O4-based samples with tailored macroporous structures

In this work we successfully obtained freeze-cast alumina (Al₂O₃) and magnesium aluminate spinel (MgAl₂O₄) samples. Camphene was used as the freezing vehicle in this study. The specimens prepared herein were examined by Archimedes tests, scanning electron microscopy, and X-ray powder diffraction. Cold crushing tests were also carried out at room temperature. It was observed that the pore structure of Al₂O₃ samples can be tailored by changing the solid loading and freezing rate; the higher the solid loading and freezing rate, the finer the pore structure of the freeze-cast sample. MgAl₂O₄-based specimens were fabricated by keeping the solid loading in the starting slurry at 30 vol% and using liquid nitrogen as the cooling agent. The material obtained from a 60 Al₂O₃?40 MgO slurry showed a spinel amount of about 90%, an expressive total porosity (63 ± 3%), and a significant cold crushing strength (58 ± 6 MPa). In addition, this material exhibited the finest pore structure among the composition studied herein, showing a mean pore size of about 4 µm.     

Electromagnetic properties of electrospun Fe3O4/carbon composite nanofibers

In order to develop multifunctional nanofibers, the electrical conductivity and magnetic properties of Fe₃O₄/carbon composite nanofibers have been examined. Polyacrylonitrile (PAN) is used as a matrix to produce magnetic composite nanofibers containing different amounts of magnetite (Fe₃O₄) nanoparticles. Electrospun composite nanofibers were thermally treated to produce electrically conductive and magnetically permeable composite carbon nanofibers. The composite nanofibers were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffractometry (XRD), Raman spectroscopy, four-point probe and Superconducting Quantum Interference Device (SQUID). Uniform nanofibers were obtained with successful transferring of magnetic properties of Fe₃O₄ into the as-spun composite nanofibers. The electromagnetic properties were tuned by adjusting the amount of Fe₃O₄ in the matrix and carbonization process. The electrical conductivity, magnetic moment and also magnetic hysteresis rise up by adding Fe₃O₄ and increasing carbonization temperature. The high surface area provided by the ultrafine fibrous structures, the flexibility and tuneable electromagnetic properties are expected to enable the expansion of the design options for a wide rage of electronic devices.     

Ordered CoFe2O4 nanowire arrays with preferred crystal orientation and magnetic anisotropy

CoFe₂O₄ nanowire arrays were fabricated by electrodeposition of Fe²⁺ and Co²⁺ into anodic aluminum oxide (AAO) templates and further oxidization. The phase structure of the nanowires is cubic spinel-type, and the XRD result exhibits perfect preferred crystallite orientation along the nanowire axes. Compared with CoFe₂O₄ nanowire arrays synthesized by other methods, the magnetic hysteresis loops demonstrate that the arrays of nanowires exhibit uniaxial magnetic anisotropy with easy magnetization direction along the nanowire axes owing to the large shape anisotropy. This approach provides a facile technology to fabricate oxide nanowires with uniaxial magnetic anisotropy.     

Effect of surface-modified Al2O3 on the thermomechanical properties of polybutylene succinate/Al2O3 composites

This study investigates the effect of the incorporation of alumina particles on the thermomechanical properties of polybutylene succinate (PBS)/Al₂O₃ composites. The alumina surface was modified with the carboxylic groups of maleic acid through simple acid-base and in situ polymerization reactions. Scanning electron microscope (SEM) results revealed the introduction of maleic acid treated alumina significantly affect the morphology of the PBS/Al₂O₃ composites as compared to the neat PBS. The thermal conductivity of the composite (0.411?W?m^?1 K^?1) was more than twice that of neat PBS. The composite containing polymerization-modified alumina showed a 50% increase in storage modulus compared with that of neat PBS. In addition, universal testing machine (UTM) and differential scanning calorimetry (DSC) measurements indicated an increase in the tensile strength and degree of crystallinity after the incorporation of modified alumina in the PBS/Al₂O₃ composite.     

In-situ synthesis of Ge/Ti4O7 composite with enhanced electrochemical properties

Germanium (Ge) is a high-capacity material that has been extensively studied due to its relatively high theoretical capacity, excellent electrical conductivity, and high Li diffusion coefficient. However, to overcome the severe volumetric expansion of Ge caused by the alloy/dealloy process during cycling, composite structures consisting of Ge and a highly stable 2nd material need to be developed. In this study, a composite structure consisting of Ge and Ti₄O₇ (Ge/Ti₄O₇) is prepared using a facile, in-situ process with GeO₂ and TiO₂ under an H₂ atmosphere at 900 °C. Ge/Ti₄O₇ exhibits a relatively small particle size of < 1 µm compared to pure Ge (> 10 µm) prepared in the absence of TiO₂. Ge/Ti₄O₇ as an anode for LIB shows a highly reversible capacity and enhanced cycling performance compared to pure Ge electrode. The enhanced electrochemical properties of Ge/Ti₄O₇ might be attributed to Ti₄O₇ acting as an electronically conductive matrix in the composite, which could buffer the pulverization of Ge during the cycle.     

Processing,microstructure and performance of Al2O3/Er3Al5O12/ZrO2 ternary eutectic ceramics prepared by laser floating zone melting with ultra-high temperature gradient

Directionally solidified Al₂O₃/Er₃Al₅O₁₂(EAG)/ZrO₂ ternary eutectic/off-eutectic composite ceramics with high density, homogeneous microstructures, well-oriented growth have been prepared by laser floating zone melting at different solidification rates from 4 to 400 µm/s. Uniform and stable melting zone is obtained by optimizing temperature field distribution to keep continuous and stable eutectic growth and prevent from cracks and defects. The as-solidified composite ceramic exhibits complexly irregular eutectic structure, in which the eutectic spacing is rapidly refined but dotted ZrO₂ number inside Al₂O₃ phase is decreased as increasing the solidification rate. The formation mechanism of ZrO₂ distributed inside Al₂O₃ matrix is revealed by examining the depression of solid/liquid interface. Furthermore, after heat exposure 1500 °C for 200 h, the eutectic microstructure only shows tiny coarsening, which indicates it has excellent microstructural stability. As increasing the ZrO₂ content, the fracture toughness can be improved up to 3.5 MPa m^1/2 at 20.6 mol% ZrO₂.