Synthesis and characterization of novel flower-like CeF3 nanostructures via a rapid microwave method

Novel flower-like CeF₃ nanostructures with a mean diameter of 190 nm were successfully synthesized via a rapid and facile microwave irradiation route using ethylenediaminetetraacetic acid disodium as the complexing reagent. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and photoluminescence (PL). XRD patterns showed that the CeF₃ nanoflowers were hexagonal phase and had good crystallinity and purity. TEM and SEM images showed that the as-prepared CeF₃ samples displayed 3D flower-like nanostructures and had uniform sizes and morphologies. The experimental results revealed that the as-prepared CeF₃ nanoflowers might be assembled by nanodisks. The formation process of the CeF₃ nanoflowers was preliminarily investigated.     

The low temperature synthesis and characterization of Bi3.25La0.75Ti3O12 powder by hydroxide coprecipitation in aqueous medium

The fine powders of Bi_3.25La_0.75Ti₃O₁₂ (BLT) were prepared by coprecipitaton method in aqueous medium at low temperature. The differential thermal analysis (DTA), thermo-gravimetric analysis (TG) and X-ray diffraction (XRD) were employed to evaluate the phase formation of BLT and TEM was used to characterize and observe the particle size and morphology of BLT powder obtained. The results show that the bismuth layer perovskite phase of BLT can begin to form at as low as 500 °C by the coprecipitation method. When the precipitates obtained were calcined at 600 °C for 2 h, the mono-phase and perfect BLT powder was synthesized. The BLT powder obtained consists of irregular or plate-like particles which are less than about 100 nm and is nearly aggregate free.     

Polymer-assisted synthesis of Co2P nanocrystals

Co₂P nanocrystals were successfully synthesized by a polymer-assisted hydrothermal method. The reaction was carried out at 190 °C-220 °C using cobalt chloride hexahydrate (CoCl₂·6H₂O) as Co-source and yellow phosphorous as P-source. Polyacrylamide (PAM) was used as surfactant. By controlling the experiment parameters such as the reaction temperature and the amount of polyacrylamide (PAM), Co₂P nanocrystals with the rod-like or flower-like morphology could be prepared successfully. The phase and the morphology of the samples were characterized by X-ray diffraction (XRD), transmission electron microscopes (TEM), electron diffraction pattern (ED) and high resolution transmission electron microscope (HRTEM). Furthermore, based on the results of the TEM observation, the possible formation processes of the Co₂P nanorods or nanoflowers were also discussed.     

Synthesis and characterization of flower-like MoS2 microspheres by a facile hydrothermal route

Flower-like MoS₂ microspheres with high purity were successfully synthesized via a facile hydrothermal route by adding sodium silicate as an additive. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). XRD patterns showed that the MoS₂ microspheres had good crystallinity with well-stacked layered structure. TEM and SEM images showed that the MoS₂ microspheres had uniform sizes with mean diameter about 480 nm and were constructed with MoS₂ sheets with thickness of several nanometers. It was found that the possible precursor H₄SiMo₁₂O₄₀ obtained by sodium silicate reacting with sodium molybdate played a crucial role in the formation of the flower-like MoS₂ microspheres in our experiment. A possible formation mechanism of MoS₂ microspheres was preliminarily presented.     

A novel technique to prepare LiNbO3 at low temperature

Fresh niobium hydroxide was first precipitated from NbF₅ solution using an aqueous ammonium hydroxide under basic conditions. Then a simple procedure of mixing lithium and niobium hydroxides together and heating at a low temperature (400 °C) produced pure ultrafine single phase LiNbO₃ (LN). In the literature, this is the lowest temperature so far reported on the formation of LN. The phase content and lattice parameters are determined by X-ray diffraction (XRD). The average particle size and morphology were studied by transmission electron microscopy (TEM).     

An easier method of preparation of mesoporous anatase TiO2 nanoparticles via ultrasonic irradiation

Mesoporous anatase TiO₂ nanopowder was synthesised by the sol–gel method using ultrasonic irradiation. This method is simple and faster for the synthesis of phase pure mesoporous anatase TiO₂ nanopowder. The product is characterised by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron spectroscopy (TEM), thermo gravimetric analysis, Brunauer–Emmett–Teller (BET) surface area, UV–visible diffuse reflectance spectroscopy and Fourier transform infrared spectroscopy. Analysis of XRD patterns, SEM and TEM image shows that the average particles size is of 19.9 nm and has an anatase structure. The mesoporous nature was determined by the BET method using the Barrett–Joyner–Halenda (BJH) model.     

Te纳米线模板法加工Bi_2Te_3-Te片式棒热电材料(英文)

以碲纳米线为模板,采用简便的回流法大规模合成了Bi2Te3-Te片式棒一维材料,产量达到90%.利用X射线衍射、扫描电镜、X射线能谱、透射电镜对样品进行了分析.系统的研究了KOH、EDTA以及反应时间对产物结构的影响,提出了这种异质结构的形成机制.本制备方法可以推广到合成其它金属和半导体的一维特殊纳米结构.     

Synthesis and shape evolution of novel cuniform-like MnO2 in aqueous solution

In this paper, the cuniform-like MnO₂ particles were first successfully synthesized with dodecylbenzenesulfonic acid (DBSA) as surfactant in aqueous solution. The samples were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD) and infrared spectroscopy (IR). The possible mechanisms of the shape evolution for the formation of MnO₂ samples were discussed.     

Facile synthesis of nanocrystalline spinel NiFe2O4 via a novel soft chemistry route

A novel soft chemistry route (rheological phase reaction method) was developed to synthesize nanocrystalline NiFe₂O₄. The as-prepared samples were characterized by powder X-ray diffractometer (XRD), transmission electron microscope (TEM) and vibrating sample magnetometer (VSM). The effects of the calcination temperature on the particle sizes and magnetic properties of the samples were investigated. The results indicated that the samples obtained by this method had the single-phase spinel. Particle sizes estimated from Scherrer's formula increased with the calcination temperature, which were consistent with the results of TEM. The magnetic properties of the samples were strongly affected by the calcination temperature. The coercivity initially increased and then decreased with increasing calcination temperature whereas the saturation magnetization continuously increased.     

Synthesis of Co3O4 nanoparticles via the CTAB-assisted method

Cobalt oxide (Co₃O₄) nanoparticles were successfully synthesized by the cetyltrimethylammonium bromide (CTAB)-assisted method at normal pressure for the first time. The structure and morphology of the as-prepared Co₃O₄ nanoparticles were characterized by powder X-ray diffracton (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and N₂-sorption analysis. XRD studies indicated that the as-prepared product was well-crystallized cubic phase of Co₃O₄ with a cell constant of α = 8.0722 Å. The EM images showed that the obtained Co₃O₄ sample consisted of dispersive quasi-spherical particles with the size ranged from 15 to 25 nm.     

Synthesis and characterization of iron aluminide nanoparticles by DC thermal plasma jet

Intermetallic iron aluminide alloy nanoparticles were synthesized by non-transferred DC plasma spray torch at atmospheric pressure. These powder particles were characterized by vibrating sample magnetometer (VSM), X-ray diffraction (XRD), environmental scanning electron microscopy (ESEM), laser scattering particle size distribution analyzer, energy dispersive X-ray spectra (EDX) and thermo gravimetric-differential thermal analysis (TG/DTA) studies and the results are discussed. Commercially available iron and aluminium powders in the size range between 40 and 100 μm were ball milled with suitable ratio (Fe-85% and Al-15%) by weight to form a iron-aluminium blende; this was used as feed stock to synthesize iron aluminide nanoparticles. These nanoparticles particles were spherical in shape and black in colour, with the size range between 30 and 70 nm observed by ESEM. It is seen that the powders processed at higher power levels (15.3 kW) have more number of single spherical nanoparticles than powders processed at lower power levels (9.8 kW). The formation of iron aluminide nanoparticles is confirmed by XRD analysis and an exothermic reaction by DTA studies.     

Complexing reagent-assisted microwave synthesis of uniform and monodisperse disk-like CeF3 particles

Highly uniform and monodisperse disk-like CeF₃ particles with diameter about 230 nm and thickness about 76 nm were successfully synthesized via a mild and facile microwave irradiation assisted by a complexing reagent, ethylenediamine tetraacetic acid disodium salt (Na₂H₂EDTA). The morphologies and crystal structure of the products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and scanning electron microscopy (SEM). XRD patterns showed that the as-prepared CeF₃ products have hexagonal structure and high crystallinity. SEM images showed that these disk-like CeF₃ nanocrystals had rough surfaces which were covered with many sheet-like structures. It was found that the reaction time and the complexing reagent played crucial roles on formation of uniform disk-like CeF₃ particles. A possible formation mechanism of the disk-like CeF₃ particles was preliminarily presented.     

Mesoporous structure of praseodymium-stabilized zirconia

Mesoporous PrO_y-ZrO₂ materials were obtained by coprecipitation process. XRD patterns and TEM images reveal pore size growth with increase in the calcining temperature. N₂ adsorption-desorption isotherms of the PrO_y-ZrO₂ samples are indicative of type IV behavior characteristic of mesoporous materials (as evidenced by low-angle XRD patterns). PrO_y-ZrO₂ calcined at 500 and 650 °C show well-developed H2 type hysteresis loops, indicating the existence of ink-bottle-like pores with a narrow entrance and a large cavity. PrO_y-ZrO₂ calcined at 800 and 950 °C show H1 type hysteresis loops, which is often associated with porous materials known to consist of agglomerates of approximately uniform spheres, and hence to have narrow distributions of pore size. The phase analysis by Rietveld refinement method clearly shows the formation of cubic PrO_y-ZrO₂ solid solution from 500 to 950 °C.     

The multi-staged formation process of titanium oxide nanotubes and its thermal stability

The multi-staged formation process of titanium oxide nanotubes was investigated in detail under a hydrothermal treatment. During the synthesis procedure, an intermediate stage (tree-like structures) was observed before the formation of the titanium oxide layered structures. The layered structure of titanium oxide generally was considered to exfoliate directly from raw TiO₂ materials through the alkaline hydrothermal treatment. The rolling process of the layered structures of titanium oxide was confirmed by TEM observation after the alkaline hydrothermal treatment for the raw TiO₂ materials, followed by washing with 4 M HNO₃ aqueous solution. The thermal stability of the tube products was investigated by X-ray diffraction (XRD) and scanning electron microscope (SEM). The result showed that both the morphology and crystal phase of titanium oxide nanotubes could be retained even after calcination at 650 °C.     

Hydrothermal synthesis of single-crystalline Bi2Te3 nanoplates

Novel Bi₂Te₃ nanoplates with about 0.2-1 μm in diagonal and 100 nm in thickness have been facilely synthesized via hydrothermal routes in the presence of polyvinylpyrrolidone (PVP). Various techniques such as X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), and Fourier transform infrared spectrometry (FT-IR) have been used to characterize the obtained products. The results show that the existence of PVP is vital to the formation of the plate-like morphology. Other factors, such as the reaction temperature and the different surfactants also have influence on the morphology of the final products to some extent.     

Microstructure of a-plane ZnO grown on LaAlO3 (001)

The microstructure of a-plane ZnO grown on LaAlO₃ (LAO) (001) has been systematically investigated by employing X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Based on the results of XRD and TEM, only a-plane ZnO has been found to grow on LAO (001), and it consists of two types of domains perpendicular to each other. The crystal orientation relationships of a-plane ZnO domains with LAO have been verified to be [0001]_ZnO//[110]_LAO and [11?00]_ZnO//[11?0]_LAO. The domain boundaries in the a-plane ZnO are along the direction in a rotation angle of about 45° from the c-axes of ZnO. The surface morphology of ZnO films in SEM exhibits domain structure in stripe-like shape. The formation of two domains can be attributed to the cubic symmetry of the surface configuration of LAO (001).     

Microwave-assisted green synthesis of MnO2 nanoplates with environmental catalytic activity

In this paper, MnO₂ nanoplates were synthesized in aqueous solution under the microwave irradiation, without using any templates, catalysts, and organic reagents. The as-prepared MnO₂ nanoplates were systematically characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM), high-resolution TEM (HRTEM), Fourier transform infrared (FT-IR) spectroscopy, differential scanning calorimetry (DSC) and thermo-gravimetric (TG) analysis, and nitrogen sorption measurements. Microwave irradiation could produce MnO₂ with uniform size and well-defined shape as well as high crystallinity. On the basis of experimental results, a possible formation mechanism of MnO₂ nanoplates was proposed. Furthermore, the resulting MnO₂ nanoplates were found to exhibit remarkable environmental catalytic performance in degradation of Rhodamine B (RhB) in aqueous solution, indicating these MnO₂ nanoplates is very promising for wastewater treatment.     

Synthesis of nanostructure rutile TiO2 in a carboxyl-containing ionic liquid

Nanostructure rutile TiO₂ was prepared in a carboxyl-containing ionic liquid, 1-methylimidazolium-3-acetate chlorine ([AcMIm]Cl), by using TiOCl₂ solution as a precursor at low temperature. The obtained nanostructure TiO₂ was analyzed with fourier transform infrared (FTIR), X-ray powder diffraction (XRD) and transmission electron microscopy (TEM). The as-prepared TiO₂ present only rutile crystal phase and a novel flower-like morphology. The as-prepared rutile TiO₂ shows better photocatalytic performance in the degradation of methyl orange. The template-directing performance of ionic liquid is due to the bidentate chelating complexation between the carboxylic functional group of ionic liquid and titania.     

Cold-Sprayed TiO2 Coatings from Nanostructured Ceramic Agglomerated Powders

In this work, synthesis of agglomerated TiO₂, which is ready to be used after synthesis via a simple hydrolysis process, is described. The as-synthesized TiO₂ powders were characterized by X-ray diffraction (XRD), Scanning Electron Microscope (SEM), Field Emission Scanning Electron Microscope (FE-SEM), Transmission Electron Microscope (TEM) and DTA. DTA curve indicated that addition of (NH₄)₂SO₄ into the starting precursor has accelerated the hydrolysis of titanyl sulfate. The XRD patterns showed that single-phase anatase TiO₂ was produced using low-temperature hydrolysis at 80°C. SEM confirmed that the as-synthesized powders were in agglomerated form and in micro size. Addition of a structure-directing agent (SDA), (NH₄)₂SO₄, promotes agglomeration, with a denser closed packing of particle arrangement, which reduces the number of existing porosities in the synthesized powder. The TEM image showed that the primary particles were nanoparticles. The preliminary study of coating formation depicted that the powder obtained could be used as the feedstock powder for the cold spray (CS) process to make the coating as it can be deposited onto the ceramic tile substrate.     

Solution route synthesis of dendrite Cu6Sn5 powders, anode material for lithium-ion batteries

Intermetallic dendrite particles, such as Cu₆Sn₅ compound, possible anode materials for high power lithium-ion batteries, can be synthesized by using solution technique. Solution route method can induce the formation of the compound by performing a redox reaction between metal chloride salts and metallic reducing powder in a suitable solvent. The morphological features and single-phase formation corresponding to different processing conditions including solvent type, reducing agent particle size, and reaction temperature, were determined. The X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) results illustrate the dendritic morphology of Cu₆Sn₅ particles with small amount of impurities, which can be synthesized by using ethylene glycol as solvent and zinc powder as reducing agent. Reducing agent particle size and reaction temperature have a very small effect on the formation of the Cu₆Sn₅ dendrite powder.