Pt nanoparticles modified by rare earth oxides: Electronic effect and influence to catalytic hydrogenation of 3-phenoxybenzaldehyde

The rare earth elements (La, Ce, Nd, Sm, Pr, and Gd) modified Pt/Al₂O₃ catalysts were prepared by the colloidal deposition and chemical reduction methods, respectively. Pt nanoparticles with average size 3 ± 0.5 nm were uniformly dispersed on the surface of Al₂O₃ for the samples prepared by the colloidal deposition method, which exhibited higher activities in the hydrogenation of 3-phenoxybenzadehyde than the corresponding samples prepared by chemical reduction method. Moreover, except Gd, the catalysts modified by rare earth elements showed better catalytic performance than unmodified Pt/Al₂O₃. For Pt–Ce/Al₂O₃ catalyst, when the weight percent of Pt and Ce was 0.5 and 0.25, respectively, the hydrogenation conversion of 3-phenoxybenzaldehyde was 97.3% after 6 h reaction. This activity improvement is due to the electronic interaction between Pt and rare earth elements, which was investigated by X-ray photoelectron spectroscopy.     

Room temperature multiferroic properties of (Bi0.95La0.05)(Fe0.97Mn0.03)O3/NiFe2O4 double layered thin film

(Bi_0.95La_0.05)(Fe_0.97Mn_0.03)O₃/NiFe₂O₄ double layered thin film was prepared on a Pt(111)/Ti/SiO₂/Si(100) substrate by a chemical solution deposition method. X-ray diffraction and Raman scattering spectroscopy studies confirmed the formation of the distorted rhombohedral perovskite and the inverse spinel cubic structures for the (Bi_0.95La_0.05)(Fe_0.97Mn_0.03)O₃/NiFe₂O₄ double layered thin film. The (Bi_0.95La_0.05)(Fe_0.97Mn_0.03)O₃/NiFe₂O₄ double layered thin film exhibited well saturated ferromagnetic (2 M_r of 18.1 emu/cm³ and 2H_c of 0.32 kOe at 20 kOe) and ferroelectric (2P_r of 60 μC/cm² and 2E_c of 813 kV/cm at 866 kV/cm) hysteresis loops with low order of leakage current density (4.5 × 10⁻⁶ A/cm² at an applied electric field of 100 kV/cm), which suggest the ferroelectric and ferromagnetic multi-layers applications in real devices.     

Preparation and properties of sliver and nitrogen co-doped TiO2 photocatalyst

TiO₂ photocatalysts co-doped with different content of Ag and N were prepared by sol–gel method combined with microwave chemical method. The samples were analyzed by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscope (TEM), ultraviolet–visible diffuse reflectance spectrum (UV–vis) and photo-luminescence emission spectrum (PL). The photocatalytic activity was investigated by photocatalytic degradation of methylene blue (MB) under irradiation of fluorescent lamp. The results indicate that Ag and N co-doping can restrain the increase of grain size, broaden the absorption spectrum to visible light region, and inhibit the recombination of the photo-generated electron–hole pairs. Moreover, the photocatalytic activity of Ag–N–TiO₂ in MB degradation is remarkable improved. The degradation rate of the sample with Ag:TiO₂ = 0.05 at%, N:TiO₂ = 18.50 wt% in 5 h is 93.44%, which is much higher than that of Degussa P25 (39.40%).     

The cation inversion and magnetization in nanopowder zinc ferrite obtained by soft mechanochemical processing

Two zinc ferrite nanoparticle materials were prepared by the same method – soft mechanochemical synthesis, but starting from different powder mixtures: (1) Zn(OH)₂/α-Fe₂O₃ and (2) Zn(OH)₂/Fe(OH)₃. In both cases a single phase system was obtained after 18 h of milling. The progress of the synthesis was controlled by X-ray diffractometry (XRD), Raman spectroscopy, TEM and magnetic measurements. Analysis of the XRD patterns by Rietveld refinement allowed determination of the cation inversion degree for both obtained single phase ZnFe₂O₄ samples. The sample obtained from mixture (1) has the cation inversion degree 0.3482 and the sample obtained from mixture (2) 0.400. Magnetization measurements were confirmed that the degrees of the inversion were well estimated. Comparison with published data shows that used method of synthesis gives nano powder samples with extremely high values of saturation magnetizations: sample (1) 78.3 emu g⁻¹ and sample (2) 91.5 emu g⁻¹ at T = 4.5 K.     

Sol–gel auto-combustion synthesis of PVP/CoFe2O4 nanocomposite and its magnetic characterization

Poly(vinyl pyrrolidone)/CoFe₂O₄ nanocomposite has been fabricated by a sol–gel auto-combustion method. Poly(vinyl pyrrolidone) was used as a reducing agent as well as a surface capping agent to prevent particle aggregation and stabilize the particles. The average crystallite size estimated from X-ray line profile fitting was found to be 20 ± 7 nm. The high field irreversibility and unsaturated magnetization behaviours indicate the presence of the core–shell structure in the sample. The exchange bias effect observed at 10 K suggests the existence of the magnetically aligned core surrounded by spin-disordered surface layer. The reduced remanent magnetization value of 0.6 at 10 K (higher than the theoretical value of 0.5) shows the PVP/CoFe₂O₄ nanocomposite to have cubic magnetocrystalline anisotropy according to the Stoner–Wohlfarth model.     

Synthesis,characterization and microwave absorption properties of Fe3O4/Co core/shell-type nanoparticles

Co coated Fe₃O₄ core/shell-type nanoparticles were fabricated by hydrothermal technique and electroless plating process. X-ray powder diffraction (XRD), X-ray fluorescence spectrometer (XRF) and transmission electron microscope (TEM) were employed to investigate the crystal structure, element composition and morphology of the prepared nanoparticles. Vibrating sample magnetometer (VSM) and vector network analyzer were used to measure the magnetic properties and electromagnetic parameters of pure Fe₃O₄ and Fe₃O₄/Co core/shell-type nanoparticles, then reflection losses (RL(dB)) were calculated in the frequency range of 2–18 GHz. Magnetic studies revealed typical ferromagnetic behavior for the pure Fe₃O₄ and Fe₃O₄/Co core/shell-type nanoparticles with their saturation magnetization (M_s = 63.1 and 72.4 emu/g) and coercivity (H_c = 99.5, and 165.4 Oe), respectively. Due to the existence of the core/shell structure, the electromagnetic characteristic of the Fe₃O₄/Co nanoparticles exhibit better microwave absorption performance than the pure Fe₃O₄ in the range of 2–18 GHz, such as more powerful absorbing property and wider frequency band of microwave absorption.     

Preparation,characterization and application of Fe3O4/ZnO core/shell magnetic nanoparticles

Fe₃O₄ magnetic nanoparticles (MNPs) were synthesized by a co-precipitation method. The phase purity was confirmed by X-ray powder diffraction (XRD) analysis. The crystal size was found to be 10 nm from transmission electron microscopy (TEM). It is evidenced that the surface of Fe₃O₄ MNPs was modified by sodium citrate. The Fe₃O₄/ZnO core/shell MNPs were obtained by coating the MNPs with direct precipitation using zinc acetate and ammonium carbonate. The precursor was firstly dried and then calcined at 350 °C. The antioxidation tests indicated that the core/shell MNPs give better antioxidation than that of the Fe₃O₄ MNPs. The photocatalytic degradation of methyl orange revealed that the core/shell MNPs have higher photocatalytic activity than that of the ZnO nanoparticles. Separation of the core/shell MNPs from the aqueous suspension using a magnet provides an easy way to recycle the core/shell MNPs. After four-time recycling, the photocatalytic degradation percentage of the core/shell MNPs is about 70%.     

The measurement of the adhesion force between ceramic particles and metal matrix in ceramic reinforced-metal matrix composites

This paper presents the method for measurement of the adhesion force and fracture strength of the interface between ceramic particles and metal matrix in ceramic reinforced-metal matrix composites. Three samples with the following Cu to Al₂O₃ ratio (in vol.%) were prepared: 98.0Cu/2.0Al₂O₃, 95.0Cu/5.0Al₂O₃ and 90Cu/10Al₂O₃. Furthermore, microwires which contain a few ceramic particles were produced by means of electro etching. The microwires with clearly exposed interface were tested with use of the microtensile tester. The microwires usually break exactly at the interface between the metal matrix and ceramic particle. The force and the interface area were carefully measured and then the fracture strength of the interface was determined. The strength of the interface between ceramic particle and metal matrix was equal to 59 ± 8 MPa and 59 ± 11 MPa in the case of 2% and 5% Al₂O₃ to Cu ratio, respectively. On the other hand, it was significantly lower (38 ± 5 MPa) for the wires made of composite with 10% Al₂O₃.     

Graphene-enhanced microwave absorption properties of Fe3O4/SiO2 nanorods

Fe₃O₄/SiO₂/graphene composite composed of Fe₃O₄/SiO₂ core–shell nanorods and graphene nanosheets were synthesized by a facile wet chemical method. Structure and morphology studies reveal that the Fe₃O₄/SiO₂ nanorods with porous structure and large aspect ratio are densely wrapped by the graphene nanosheets. By changing the graphene content, the electromagnetic properties of the Fe₃O₄/SiO₂/graphene composite can be well tuned. When the weight ratio of Fe₃O₄/SiO₂ to graphene reaches an appropriate value, excellent microwave absorption performance is achieved due to the large electromagnetic losses and good impedance matching. The Fe₃O₄/SiO₂/graphene composite with graphene content of 5 wt.% shows the minimum reflection loss of −27.1 dB at 12.2 GHz when the coating layer thickness is only 1.5 mm.     

Fracture behaviour of α-Al2O3 ceramics reinforced with a mixture of single-wall and multi-wall carbon nanotubes

The extraordinary mechanical properties of single-wall carbon nanotubes (SWCNTs) and multi-wall carbon nanotubes (MWCNTs) have generated interest in incorporating them as toughening agents in ceramics. This work describes the fracture behaviour of an alumina (Al₂O₃) ceramic reinforced with a mixture of 0.05 wt% MWCNTs + 0.05 wt% SWCNTs. The CNT/Al₂O₃ nanocomposite was pressureless sintered in air using graphite powder as bed powder at 1520 °C for 1 h. The hardnesses and fracture toughnesses were lower than for pure Al₂O₃ and Al₂O₃ + 0.1 wt% SWCNTs and Al₂O₃ + 0.1 wt% MWCNTs. A predominantly transgranular fracture mode with a decrease in crack deflection and no pull-out was observed in the SWCNT + MWCNT–Al₂O₃ nanocomposite. MWCNTs had to the best reinforcing effect in Al₂O₃ nanocomposite.     

La-doped ZnO nanoparticles: Simple solution-combusting preparation and applications in the wastewater treatment

La-doped ZnO nanoparticles have been successfully synthesized by a simple solution combustion method via employing a mixture of ethanol and ethyleneglycol (v/v = 60/40) as the solvent. Zinc acetate and oxygen gas in the atmosphere were used as zinc and oxygen sources, and La(NO₃)₃ as the doping reagent. The as-obtained product was characterized by means of powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray spectrometry and X-ray photoelectron spectroscopy. Experiments showed that La-doped ZnO nanoparticles exhibited the higher capacities for the removal of Pb²⁺ and Cu²⁺ ions in water resource than undoped ZnO nanoparticles.     

Synthesis of heterostructured In2O3/BiOCl powders and their visible-light-driven photocatalytic activity for the degradation of Rhodamine B

Heterostructured In₂O₃/BiOCl powders were synthesized by chemical coprecipitation method at room temperature followed by thermal treatment at 400 °C for 2 h. The TEM results confirmed the formation of sheet-like BiOCl nanostructures with the thickness of ca. 5–7 nm. In order to investigate the effect of In₂O₃ on the photocatalytic activity of heterostructured powders, the amount of In₂O₃ was varied from 0 wt% to 14 wt%. Adsorption and photocatalytic activity of the samples were evaluated for the degradation of Rhodamine B (RhB) in the dark and under visible light irradiation, respectively. The heterostructured In₂O₃/BiOCl powders showed high adsorption capacity and enhanced photocatalytic activity compared to P25 and pure BiOCl. Based on the results obtained in this study, the mechanism for the enhancement of photocatalytic activity of heterostructured In₂O₃/BiOCl powders is discussed. 10 wt% In₂O₃/BiOCl composite also exhibited good cycle performance for the degradation of RhB under visible light irradiation.     

Co-electrospinning fabrication and photocatalytic performance of TiO2/SiO2 core/sheath nanofibers with tunable sheath thickness

In this paper, core/sheath TiO₂/SiO₂ nanofibers with tunable sheath thickness were directly fabricated via a facile co-electrospinning technique with subsequent calcination at 500 °C. The morphologies and structures of core/sheath TiO₂/SiO₂ nanofibers were characterized by TGA, FESEM, TEM, FTIR, XPS and BET. It was found that the 1D core/sheath nanofibers are made up of anatase–rutile TiO₂ core and amorphous SiO₂ sheath. The influences of SiO₂ sheath and its thickness on the photoreactivity were evaluated by observing photo-degradation of methylene blue aqueous solution under the irradiation of UV light. Compared with pure TiO₂ nanofibers, the core/sheath TiO₂/SiO₂ nanofibers performed a better catalytic performance. That was attributed to not only efficient separation of hole–electron pairs resulting from the formation of heterojunction but also larger surface area and surface silanol group which will be useful to provide higher capacity for oxygen adsorption to generate more hydroxyl radicals. And the optimized core/sheath TiO₂/SiO₂ nanofibers with a sheath thickness of 37 nm exhibited the best photocatalytic performance.     

Enhanced photodegradation activity of Rhodamine B by Co3O4/Ag3VO4 under visible light irriadiation

Co₃O₄/Ag₃VO₄ composite photocatalysts were synthesized by the wetness impregnation method and characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and diffuse reflectance spectroscopy (DRS). The photoactivity testing result shows that the Co₃O₄/Ag₃VO₄ composite exhibits enhanced photodegradation activity for Rhodamine B (RhB) under visible-light irradiation. The Co₃O₄ content and calcination temperature have a significant impact on the photocatalytic activities of the samples. The highest efficiency was observed on the 1.0 wt.% Co₃O₄/Ag₃VO₄ sample calcined at 653 K. Moreover, the photoelectrochemical performance with the method of transient photocurrent–time was investigated. Based on the results of the characterizations, the mechanism of enhanced photocatalytic activity is discussed.     

Nb2O5 hollow nanospheres as anode material for enhanced performance in lithium ion batteries

Nb₂O₅ hollow nanospheres of average diameter ca. ～29 nm and hollow cavity size ca. 17 nm were synthesized using polymeric micelles with core–shell–corona architecture under mild conditions. The hollow particles were thoroughly characterized by transmission electron microscope (TEM), X-ray diffraction (XRD), infrared spectroscopy (FTIR), thermal (TG/DTA) and nitrogen adsorption analyses. Thus obtained Nb₂O₅ hollow nanospheres were investigated as anode materials for lithium ion rechargeable batteries for the first time. The nanostructured electrode delivers high capacity of 172 mAh g^?1 after 250 cycles of charge/discharge at a rate of 0.5 C. More importantly, the hollow particles based electrodes maintains the structural integrity and excellent cycling stability even after exposing to high current density 6.25 A g^?1. The enhanced electrochemical behavior is ascribed to hollow cavity coupled with nanosized Nb₂O₅ shell domain that facilitates fast lithium intercalation/deintercalation kinetics.     

Synthesis and characterization of a new organic sulphate, [2,3-(CH3)2C6H3NH3]HSO4·H2O

Crystals of a new hybrid compound C₈H₁₂N⁺, HSO₄^?·H₂O were synthesized in aqueous solution and characterized by X-ray diffraction and IR absorption spectroscopy. This compound crystallizes in the orthorhombic non-centrosymmetrical space group P2₁2₁2₁ and an unit cell with a = 5.74(2) Å, b = 9.17(2) Å, c = 21.34(4) Å, V = 1124(6) Å³, and Z = 4. Its crystal structure is a packing of alternated inorganic and organic layers parallel to (a,b) planes. The different components are connected by a bi-dimensional network of strong OH…O and NH…O hydrogen bonds. Then, in order to detect phase transitions and watch changes in the conductivity behaviour, investigations by DTA–TG and differential scanning calorimetry (DSC) and electrical conductivity measurements were carried out.     

Structural,optical and morphological properties of La,Cu co-doped SnO2 nanocrystals by co-precipitation method

Sn_0.96−xLa_0.04Cu_xO₂ (0 ⩽ x ⩽ 0.03) nanocrystals have been successfully synthesized by employing a simple co-precipitation method. The crystal structure of the synthesized nanocrystals was found to be tetragonal rutile of tin oxide by using X-ray diffraction technique and was not affected by doping. The change in lattice parameters was discussed based on the secondary phase formation and presence of Cu²⁺/Cu³⁺ in LaSnO₂ lattice. The variation in size and shape of the nanocrystals by Cu-doping was discussed using scanning electron microscope. The chemical stoichiometry of Sn, Cu, La and O was confirmed by energy dispersive X-ray spectra. The best optical transparency and lower absorption observed at Sn_0.97La_0.02Cu_0.01O₂ nanocrystals seems to be optimal for industrial applications especially as transparent electrode. The initial blue shift of energy gap from 3.65 eV (Cu = 0%) to 3.78 eV (Cu = 1%) (ΔE_g ≈ 0.13 eV) is due to the distortion in the crystal structure of the host compound and generation of defects. The red shift of energy gap after Cu = 1% is due to the charge-transfer transitions between the metal ions d-electrons and the SnO₂ conduction or valence band. Lattice mode of SnO₂ at 686 cm⁻¹ in Sn_0.98La_0.02O₂ nanocrystals and anti-symmetric SnOSn stretching mode of the surface bridging oxide around 634–642 cm⁻¹ in Cu doped Sn_0.98La_0.02O₂ nanocrystals was confirmed by Fourier transform infrared spectra.     

A facile assembly of polyimide/graphene core–shell structured nanocomposites with both high electrical and thermal conductivities

Polyimide/reduced graphene oxide (PI/r-GO) core–shell structured microspheres were fabricated by in-situ reduction of graphene oxide (GO), which was coated on the surface of PI microspheres via hydrogen bonding and π–π stacking interaction. The highly ordered 3D core–shell structure of PI/r-GO microspheres with graphene shell thickness of 3 nm was well characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM) and Raman spectra. The glass transition temperature (T_g) of PI/r-GO microspheres was slightly increased because of the interaction of r-GO and PI matrix while the temperature at 5% weight loss (T_5%) of PI/r-GO microspheres was decreased due to the side effect of reductant hydrazine hydrate. The PI/r-GO nanocomposites exhibited highly electrical conductivity with percolation threshold of 0.15 vol% and ultimate conductivity of 1.4 × 10⁻² S/m. Besides, the thermal conductivity of PI/r-GO nanocomposites with 2% weight content of r-GO could reach up to 0.26 W/m K.