Synthesis of carbon nanotube,graphene, CoFe<Subscript>2</Subscript>O<Subscript>4</Subscript>, and NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript> polypyrrole nanocomposites and study their microwave absorption

In this experimental work, different conductive polymer nanocomposites were synthesized using polypyrrole as conductive polymer and CoFe₂O₄, NiFe₂O₄, CNT and graphene as fillers. X-ray diffraction pattern was used to study the crystallinity of the products and it was found CoFe₂O₄, NiFe₂O₄, CNT, and graphene were successfully embedded in the polymer matrix. To further approve the synthesis of the nanocomposites, energy dispersive X-ray spectroscopy was served. Surface groups of the synthesized nanocomposites were studied by Fourier transform infrared and Raman spectroscopy. The morphology of the products was examined by scanning electron microscopy and transmission electron microscopy. It was found the fillers were successfully embedded in the polymer matrix and they were in nanometer scales. To investigate the magnetic properties and conductivity of the polymer nanocomposites, alternating gradient force magnetometer and four-point probe were used, respectively. Finally, the microwave absorption properties of the polymer nanocomposites were studied and it was found the fillers have different effects on the polymer microwave absorption value.     

Room temperature magnetic exchange coupling in multiferroic BaTiO<Subscript>3</Subscript>/CoFe<Subscript>2</Subscript>O<Subscript>4</Subscript> magnetoelectric superlattice

Multiferroic BaTiO₃/CoFe₂O₄ superlattice films are deposited by laser molecular beam epitaxy. The film growth modes are studied by in situ reflection high energy electron diffraction and the film structures are revealed by high resolution transmission electron microscopy study. Ferroelectric switching behavior was studied by piezoresponse force microscopy, and it shows that good ferroelectricity was retained in the superlattice. Such a multiferroic superlattice also shows a magnetic exchange coupling under room temperature. Detailed analysis reveals that different growth modes and the substrate strain effect may be responsible for the magnetic exchange coupling.     

An alternative approach of solid-state reaction to prepare nanocrystalline KNbO<Subscript>3</Subscript>

A simple preparation of KNbO₃ powders was proposed by an alternative approach of solid-state reaction. Stoichiometric niobium oxalate and potassium acetate were mixed in water and then dried. It was demonstrated that an ion-exchange reaction occurred with the formation of K[NbO(C₂O₄)₂]·nH₂O intermediate. The single-phase KNbO₃ powders were synthesized when K[NbO(C₂O₄)₂]·nH₂O intermediate was calcined between 500 and 800 °C for 3 h. KNbO₃ powders obtained at 500 °C are determined as orthorhombic structure with an average particle size of 20–50 nm by X-ray diffraction, scanning electron microscope (SEM), and transmission electron microscopy (TEM) analysis. The morphologies of KNbO₃ obtained at different temperatures were observed by SEM and TEM analysis. The average band gap energy is estimated to be 3.16 eV by UV–vis diffuse reflectance spectra.     

Preparation of magnetic composites through SrO-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-B<Subscript>2</Subscript>O<Subscript>3</Subscript> glass crystallization

Glasses with nominal compositions 11SrO · 5.5Fe₂O₃ · 4.5Al₂O₃ · 4B₂O₃ (1) and 15SrO · 5.5Fe₂O₃ · 4.5Al₂O₃ · 4B₂O₃ (2) were prepared by rapidly quenching oxide melts between counterrotating steel rollers. The glasses were then heat-treated in the range 650–950°C to produce glass-ceramic samples. The samples were characterized by X-ray diffraction, electron microscopy, and magnetic measurements. The phase composition of the glass-ceramics was determined, and their microstructure and magnetic properties were studied. The annealing temperature was shown to have a strong effect on the coercivity of the materials, which reaches 650 and 570 kA/m for compositions 1 and 2, respectively.     

Synthesis of CuO nanoflower and its application as a H<Subscript>2</Subscript>O<Subscript>2</Subscript> sensor

CuO three-dimensional (3D) flower-like nanostructures were successfully synthesized by a simple method at 100°C with Cu(NO₃)₂·3H₂O and NH₃·H₂O for 6 h in the absence of any additives. We found that NH₃·H₂O amount was critical for CuO morphology evolution. The phase analysis was carried out using X-ray diffraction (XRD) and the result confirmed that the CuO nanoflowers were single-phase. The morphological investigations by field emission scanning electron microscope (FESEM) revealed that the CuO nanoflowers were mono-dispersed in a large quantity and consisted of nanosheets. And then, CuO nanoflowers were successfully used to modify a gold electrode to detect H₂O₂ with cyclic voltammetry (CV) and amperometric (AC). It was found that CuO nanoflowers may be of great potential for H₂O₂ electrochemical sensing.     

Splitting behavior and structural transformation process of K<Subscript>2</Subscript>Ti<Subscript>6</Subscript>O<Subscript>13</Subscript> whiskers under hydrothermal conditions

The splitting behavior and structural transformation process of K₂Ti₆O₁₃ whiskers in various hydrothermal solutions were investigated by the X-ray diffraction technique, scanning electron microscopy, transmission electron microscopy, and atomic force microscopy. TiO₂ (B) particle aggregates and rutile twinned crystals were produced respectively in diluted and concentrated HCl solutions via “dissolution-precipitation” mechanism, while no changes were observed in deionized water. In contrary to the chemical inertia of K₂Ti₆O₁₃ whiskers in KOH solution, trititanate nanowires were synthesized by splitting the bulk K₂Ti₆O₁₃ whiskers in NaOH solution. The driving force for the formation of nanowires originated from the intrinsic strain induced by the phase transition from K₂Ti₆O₁₃ with a tunnel structure to layered trititanate. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Structural and Magnetic Properties of La<Subscript>2/3</Subscript>Sr<Subscript>1/3</Subscript>MnO<Subscript>3</Subscript>/SrTiO<Subscript>3</Subscript>/CoFe<Subscript>2</Subscript> Hard-Soft Magnetic Systems

We report on the growth and magnetic properties of La_2/3Sr_1/3MnO₃/SrTiO₃/CoFe₂ hard-soft magnetic systems prepared by pulsed laser deposition on SrTiO₃(001) substrates. In situ reflection high-energy electron diffraction along the [100]SrTiO₃ substrate azimuth and atomic force microscopy measurements reveal that La_2/3Sr_1/3MnO₃ and SrTiO₃ grow both in a three dimensional mode and that the roughness of the lower and upper magnetic/non-magnetic interfaces ranges between 2 and 4 Å. Cross-section transmission electron microscopy observations show that the layers are continuous, with an homogeneous thickness, and that the interfaces are mostly sharp and correlated. The magnetization curves show a two step reversal of the magnetization, with very distinct coercive fields. A small anisotropy is observed for the CoFe₂ layer with an in plane easy magnetization axis along the [110]SrTiO₃ direction. Minor magnetization loops indicate that the coupling between the magnetic layers is negligible.     

Preparation and characterization of Y<Subscript>2</Subscript>O<Subscript>3</Subscript>:Eu phosphors by combustion process

Europium-doped yttrium phosphors were successfully synthesized by combustion process using yttrium nitrate hexahydrate [Y(NO₃)₃·6H₂O], europium nitrate [Eu(NO₃)₃·6H₂O], and carbohydrazide [CO(N₂H₃)₂]. The process takes only a few minutes to obtain Y₂O₃:Eu phosphors. The resultant powders annealed at different temperature and were investigated by X-ray diffractometer (XRD), differential thermal analyzer/thermogravimeter (DTA/TG), Fourier transform infrared spectroscopy (FTIR), photoluminescence excitation and emission spectra (PL), and transmission electron microscopy (TEM). The results showed that the formation temperature of Y₂O₃ phase is significant low, compared to solid-state reaction route of constituent oxides. For luminescence property, the emission intensity of Y₂O₃:Eu phosphors synthesized by combustion process increases steadily with increasing europium amount from 1 mol% to 5 mol%.     

Preparation and magnetic properties of the CoFe<Subscript>2</Subscript>O<Subscript>4</Subscript> thin films on Si substrate by sol-gel technique

A stable precursor for CoFe₂O₄ thin film was prepared by sol-gel technique from the aqueous solution of FeCl₃·6H₂O and CoCl₂·6H₂O. Sol was deposited on a naturally oxidized silicon-substrate by spinning technique (2000 rpm) and heat treated at different temperatures ranging from 700 to 1100 °C. Thickness of the films was controlled in the range of 400–500 nm and all the films were characterized by using XRD and SEM. The effects of temperature and the composition on the formation of CoFe₂O₄ thin film were also studied. Films obtained at relatively lower temperature showed multi-phases of α-Fe₂O₃, CoFe₂O₄ and CoO while the formation of CoFe₂O₄ phase increases with increasing temperature. Furthermore, the composition of the solution in mol% has great role on the formation of CoFe₂O₄ films and the film containing 50 mol% of Co²⁺ exhibited CoFe₂O₄ mono-phase. Surface morphology of the films was studied by scanning electron microscope (SEM). Magnetic properties of the films, studied by using vibrating sample magnetometer (VSM), showed relatively high saturation magnetization (8.04–22.21 kWb/m²) as well as high coercivity (44.59–63.30 kA/m). Saturation magnetization also increases with increasing heat treatment temperature.     

Sn<Superscript>4+</Superscript> and La<Superscript>3+</Superscript> co doped TiO<Subscript>2</Subscript> nanoparticles and their optical,photocatalytic and antibacterial properties under visible light

Sn⁴⁺ and La³⁺ co-doped TiO₂ photocatalytic material with nanoparticle structure have been successfully prepared using SnCl₂·2H₂O and La(NO₃)₃·6H₂O as precursors. Scanning electron microscopy, X-ray diffraction, transmission electron microscopy and UV–visible spectroscopy have been used to for the characterization of the morphology, crystal structure, particle size and optical properties of the samples. The photocatalytic properties of sample with various amount of La doped TiO₂ have been studied by photo degradation of methyl orange (MO) in water under visible light. XRD patterns showed both rutile and anatase phases for 5 mol% of Sn and 5–10 mol% of La. But anatase phase with a little rutile phase was formed for 5 mol%Sn and 10 mol%La. The prepared Sn and La co doped TiO₂ photo-catalyst showed optical absorption edge in the visible light area and exhibited excellent photo-catalytic ability for degradation of MO solution under visible irradiation. Antibacterial behavior towards E. coli was then studied under visible irradiation. The synthesized T-5%Sn-10%La powder exhibited superior antibacterial activity under visible irradiation compared to the pure TiO₂.     

Synthesis and conductivity studies of Li<Subscript>1.5</Subscript>Al<Subscript>0.5</Subscript>Ge<Subscript>1.5</Subscript>(PO<Subscript>4</Subscript>)<Subscript>3</Subscript> solid electrolyte

This paper describes the preparation of a lithium ion conducting solid electrolyte with the composition Li_1.5Al_0.5Ge_1.5(PO₄)₃ by a new liquid-phase method with the use of the water-soluble salts Al(NO₃)₃ · 9H₂O, LiNO₃ · 3H₂O, and (NH₄)₂HPO₄ and the germano-oxalic acid H₂[Ge(C₂O₄)₃]. The synthesized materials have been characterized by X-ray diffraction, differential scanning calorimetry, thermogravimetry, and impedance spectroscopy. The results demonstrate that sintering of the synthesized amorphous powders at a temperature of 650°C leads to the formation of phase-pure Li_1.5Al_0.5Ge_1.5(PO₄)₃. The ionic conductivity of the electrolyte measured at frequencies from 10 Hz to 2 MHz using pellets with an 86% relative density was 4.2 × 10^–4 S/cm.     

Hydrothermal synthesis and magnetic properties of NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles and nanorods

NiFe₂O₄ nanoparticles and nanorods were synthesized by a facile hydrothermal treatment of Ni(DS)₂ (Nickel dodecyl sulfate), FeCl₃, and NaOH aqueous solution at 120 °C. The products were characterized by powder X-ray diffraction, transmission electron microscopy, and selected area electron diffraction. The magnetic properties were evaluated using a vibrating sample magnetometer. The probable mechanism of the formation of NiFe₂O₄ nanoparticles and nanorods was discussed.     

Synthesis and microwave absorption property of ternary composites: polyaniline/CoFe<Subscript>2</Subscript>O<Subscript>4</Subscript>/Ba<Subscript>3</Subscript>Co<Subscript>2</Subscript>Fe<Subscript>24</Subscript>O<Subscript>41</Subscript>

Polyaniline (PANI)/CoFe₂O₄/Ba₃Co₂Fe₂₄O₄₁ composite was prepared by an in-situ polymerization method. The phase structure, morphology and magnetic properties of the as-prepared PANI/CoFe₂O₄/Ba₃Co₂Fe₂₄O₄₁ composite were characterized by XRD, FT-IR, SEM, TEM, and VSM, respectively. The microwave absorption properties of the composite were investigated by using a vector network analyzer in the 2–18 GHz frequency range. The results show that the maximum reflection loss value of the PANI/CoFe₂O₄/Ba₃Co₂Fe₂₄O₄₁ composite reaches ?30.5 dB at 10.5 GHz with a thickness of 3 mm and the bandwidth of reflection loss below ?10 dB reaches up to 1.2 GHz. The excellent microwave absorption properties of the as-prepared PANI/CoFe₂O₄/Ba₃Co₂Fe₂₄O₄₁ composite due to the enhanced impedance match between dielectric loss and magnetic loss.     

Microwave Synthesis of Cu/Cu<Subscript>2</Subscript>O/SnO<Subscript>2</Subscript> Composite with Improved Photocatalytic Ability Using SnCl<Subscript>4</Subscript> as a Protector

Cu/Cu₂O/SnO₂ composites were successfully prepared with a facile microwave synthesis method. The structure of Cu/Cu₂O/SnO₂ composite was studied by morphology characterizations, such as X-ray diffraction, transmission electron microscopy and high-resolution transmission electron microscopy, which showed that the size of the Cu/Cu₂O/SnO₂ particles is 20–50 nm. The synthesis mechanism revealed that SnCl₄ obstructed between Cu(OH) and ethylene glycol, preventing Cu(OH) being reduced into Cu at high temperature. The photocatalytic property of Cu/Cu₂O/SnO₂ composite was investigated by degrading the mixed dyestuff under the irradiation of visible light at room temperature. Benefiting from the effect of electron transfer, the photocatalytic performance of the microwave-prepared Cu/Cu₂O/SnO₂ composite was much better than that of pure Cu₂O. The possible photocatalytic mechanism of the Cu/Cu₂O/SnO₂ composite catalysts was proposed and elaborated in this study. This synthesis of Cu/Cu₂O/SnO₂ composite may provide a method for other Cu₂O/semiconductor composites microwave preparation.     

Li-storage and cycling properties of spinel,CdFe<Subscript>2</Subscript>O<Subscript>4</Subscript>, as an anode for lithium ion batteries

Cadmium ferrite, CdFe₂O₄, is synthesized by urea combustion method followed by calcination at 900°C and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM) and selected area electron diffraction (SAED) techniques. The Li-storage and cycling behaviour are examined by galvanostatic cycling, cyclic voltammetry (CV) and impedance spectroscopy in the voltage range, 0·005–3·0 V vs Li at room temperature. CdFe₂O₄ shows a first cycle reversible capacity of 870 (± 10) mAhg⁻¹ at 0·07C-rate, but the capacity degrades at 4 mAhg⁻¹ per cycle and retains only 680 (± 10) mAhg⁻¹ after 50 cycles. Heat-treated electrode of CdFe₂O₄ (300°C; 12 h, Ar) shows a significantly improved cycling performance under the above cycling conditions and a stable capacity of 810 (± 10) mAhg⁻¹ corresponding to 8·7 moles of Li per mole of CdFe₂O₄ (vs theoretical, 9·0 moles of Li) is maintained up to 60 cycles, with a coulombic efficiency, 96–98%. Rate capability of heat-treated CdFe₂O₄ is also good: reversible capacities of 650 (± 10) and 450 (± 10) mAhg⁻¹ at 0·5 C and 1·4 C (1 C = 840 mAg⁻¹) are observed, respectively. The reasons for the improved cycling performance are discussed. From the CV data in 2–15 cycles, the average discharge potential is measured to be ∼0·9 V, whereas the charge potential is ∼2·1 V. Based on the galvanostatic and CV data, ex situ-XRD, -TEM and -SAED studies, a reaction mechanism is proposed. The impedance parameters as a function of voltage during the 1st cycle have been evaluated and interpreted. Dedicated to Prof. C N R Rao on his 75th birthday, and his contributions to science for the past 56 years     

Preparation of lamellar-stacked TS-1 and its catalytic performance for the ammoximation of butanone with H<Subscript>2</Subscript>O<Subscript>2</Subscript>

A SiO₂ particle was prepared with different alkali sources, and then lamellar-stacked TS-1 catalysts were hydrothermally synthesized using the SiO₂ particle as a silica source. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectra, nitrogen adsorption–desorption and UV–vis absorption spectra were used to characterize the TS-1 catalysts. The effect of the alkali source during the preparation of the SiO₂ particle on the textural properties and catalytic performance of the TS-1 catalyst was thoroughly investigated. The TS-1 catalyst that was prepared with a SiO₂ particle using tetrapropylammonium hydroxide (TPAOH) as an alkali source (TS-1-TPAOH) possessed more meso- and macro-pores and a higher framework Ti content than the catalyst that was prepared with a SiO₂ particle using NH₃·H₂O as an alkali source (TS-1-NH₃·H₂O). As a result, the TS-1-TPAOH catalyst had a better catalytic performance for butanone ammoximation with H₂O₂ than conventional TS-1 and TS-1-NH₃·H₂O catalysts. Furthermore, the influences of reaction conditions, including reaction temperature, reaction time, the amount of catalyst and the molar ratio between H₂O₂ and butyl ketone oxime on the catalytic performance of the TS-1-TPAOH catalyst were evaluated. The unique structure of the lamellar-stacked TS-1 catalyst can effectively avoid the diffusing of large reactant molecules into zeolite channels and has potential applications in other oxidation reactions.     

Fast microwave synthesis of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> and Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>/Ag magnetic nanoparticles using Fe<Superscript>2+</Superscript> as precursor

A simple and quick microwave method to prepare high performance magnetite nanoparticles (Fe₃O₄ NPs) directly from Fe has been developed. The as-prepared Fe₃O₄ NPs product was fully characterized by X-ray diffraction, transmission electron microscopy and scanning electron microscopy. The results show that the as-prepared Fe₃O₄ NPs are quite monodisperse with an average core size of 80 × 5 nm. The microwave synthesis technique can be easily modified to prepare Fe₃O₄/Ag NPs and these NPs possess good magnetic properties. The formation mechanisms of the NPs are also discussed. Our proposed synthesis procedure is quick and simple, and shows potential for large-scale production and applications for catalysis and biomedical/biological uses.     

One-step hydrothermal synthesis of ZnFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nano-octahedrons as a high capacity anode material for Li-ion batteries

Binary transition metal oxides are considered as promising anode materials for lithium-ion batteries (LIB), because they can effectively overcome the drawbacks of simple oxides. Here, a one-step hydrothermal method is described for the synthesis of regular ZnFe₂O₄ octahedrons about 200 nm in size at a low temperature without further annealing being required. The ZnFe₂O₄ octahedrons were characterized by powder X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy and X-ray photoelectron spectroscopy. The electrochemical performance of the ZnFe₂O₄ octahedrons was examined in terms of cyclic voltammetry and discharge/charge profiles. The ZnFe₂O₄ octahedrons exhibit a high capacity of 910 mA·h/g at 60 mA/g between 0.01 and 3.0 V after 80 cycles. They also deliver a reversible specific capacity of 730 mA·h/g even after 300 cycles at 1000 mA/g, a much better performance than those in previous reports. A set of reactions involved in the discharge/charge processes are proposed on the basis of ex situ high-resolution transmission electron microscopy (HRTEM) images and selected area electron diffraction (SAED) patterns of the electrode materials. The insights obtained will be of benefit in the design of future anode materials for lithium ion batteries.      

Synthesis of CaTiO<Subscript>3</Subscript> from calcium titanyl oxalate hexahydrate (CTO) as precursor employing microwave heating technique

Calcium titanate, CaTiO₃, an important microwave dielectric material and one of major phases in synroc (synthetic rock), a titanate ceramic with potential application for fixation of high level nuclear waste was synthesized from calcium titanyl oxalate [CaTiO (C₂O₄)₂·6H₂O] (CTO) by employing microwave heating technique. CTO heated in microwave heating system in air at 500°C for 1 h gave a perovskite, CaTiO₃. The product obtained by heating of CTO in the same system at 700°C for the same duration was however, much more crystalline. CaTiO₃ obtained by the present method was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and BET surface area measurement.     

Synthesis and characterization of Cd-doped ZnMn<Subscript>2</Subscript>O<Subscript>4</Subscript> microspheres as supercapacitor electrodes

In this paper, we demonstrate the effects of Cd-doping ZnMn₂O₄ on structural and electrochemical performance. Cd-doped ZnMn₂O₄ spheres with diameters of about 2 μm were successfully synthesized by a facile hydrothermal method at 200 °C for 18 h. The fabricated Cd-doped ZnMn₂O₄ samples were characterized by X-ray diffraction, scanning electron microscopy, Brunauer Emmett Teller surface area analyzer and X-ray photoelectron spectroscopy. The electrochemical performance was investigated by cyclic voltammetry and electrochemical impedance spectrometry. The experimental results show that the synthesized spherical Cd-doped ZnMn₂O₄ exhibit far better rate capability and cyclic stability than that of pure spinel porous ZnMn₂O₄ microspheres. The result of cyclic voltammetry measurement indicates that the obtained Cd-doped ZnMn₂O₄ microspheres exhibited the high specific capacitance of 364 Fg^?1 at 2 mV/s.