Synthesis and characterization of hollow LiNiO<Subscript>2</Subscript> fibers via sol-electrospinning method

Hollow LiNiO₂ fibers have been prepared with a capillary spinneret electrospinning technique combined with the sol–gel method, and the possible mechanism for the fabrication of the hollow fibers was discussed. The xerogel fibers and those calcined at different temperatures were characterized by thermogravimetric (TG) analysis, X-ray diffractometry (XRD), Fourier transform infrared (FT-IR) spectrum, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and etc. The Polyvinyl Pyrrolidone (PVP) has an important role in the formation of hollow LiNiO₂ fibers.     

Synthesis and characterization of ion-exchangeable titanate nanotubes

Titanate nanotubes were synthesized under hydrothermal conditions. The optimized synthesis (100-180 degrees C, longer than 48 h), thermal and hydrothermal stability, ion exchangeability and consequent magnetic and optical properties of the titanate nanotubes were systematically studied in this paper. First, nanotubes with monodisperse pore-size distribution were prepared. The formation mechanism of the titanate nanotubes was also studied. Second, the thermal and hydrothermal stability were characterized with X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), Fourier transform infrared (FTIR), and Raman spectroscopy. Results showed that sodium ions played a significant role in the stability of the frameworks. Third, the selective ion exchangeability was demonstrated with a series of ions. The ion substitution also enlarged the BET surface area of the titanate nanotubes to 240 m(2) x g(-1). Combination of these two features implied that these nanotubes might be functionalized by substitution of different transitional-metal ions and consequently used for selective catalysis. Magnetism, photoluminescence, and UV/Vis spectra of the substituted titanate nanotubes revealed that the magnetic and optical properties of the nanotubes were modifiable.     

Synthesis and thermal characterization of zirconium titanate pigments

Vezetéknév This revised version was published online in August 2006 with corrections to the Cover Date.     

Synthesis and characterization of single-crystalline alkali titanate nanowires

A simple, one-step method has been utilized to synthesize functional ternary alkali titanate nanowires of single crystallinity. Nanostructural characterization shows that the nanowires are Na2Ti6O13 with [010] growth direction and KTi8O16.5 with [001] growth direction.     

Fabrication and characterization of cerium-doped barium titanate inverse opal by sol-gel method

Cerium-doped barium titanate inverted opal was synthesized from barium acetate contained cerous acetate and tetrabutyl titanate in the interstitial spaces of a polystyrene (PS) opal. This procedure involves infiltration of precursors into the interstices of the PS opal template followed by hydrolytic polycondensation of the precursors to amorphous barium titanate and removal of the PS opal by calcination. The morphologies of opal and inverse opal were characterized by scanning electron microscope (SEM). The pores were characterized by mercury intrusion porosimetry (MIP). X-ray photoelectron spectroscopy (XPS) investigation showed the doping structure of cerium, barium and titanium. And powder X-ray diffraction allows one to observe the influence of doping degree on the grain size. The lattice parameters, crystal size and lattice strain were calculated by the Rietveld refinement method. The synthesis of cerium-doped barium titanate inverted opals provides an opportunity to electrically and optically engineer the photonic band structure and the possibility of developing tunable three-dimensional photonic crystal devices.     

Preparation and characterization of zirconium titanate fibers with good high temperature performance

Zirconium titanate (ZT) precursor fibers were prepared via sol–gel technique by dry-spinning method using polyacetylacetonatozirconium (PAZ) and tetrabutyl titanate (TBOT) as starting materials. PAZ and TBOT were added into methanol with vigorous stirring at room temperature for 2 h and mixed together homogenously. The mixture came into being a new and complicated polymerization system, and PAZ and TBOT were connected through –O– bridge forming the –O–Zr–O–Ti–O– linear chains. The evolutions from the precursor fibers to polycrystalline oxide fibers were characterized by Fourier transform infrared (FT–IR) and thermal gravimetry/differential thermal analysis (TG/DTA). The surface of the ZT fibers was smooth, dense in cross-section without cracks by scanning electronic spectroscopy (SEM) and energy dispersive X-ray spectrometry (EDS). The size of the nanocrystals was less than 50 nm and arranged compactly by atomic force microscopy (AFM). The fibriform was still kept and the size of the grains was up to 400–500 nm due to the grain growth with increasing temperature and the ZT fibers were with good high temperature performance.     

Fabrication of lead titanate single crystalline nanowires by hydrothermal method and their characterization

Single crystalline nanowires of lead titanate (PbTiO₃) were fabricated by hydrothermal method at 200°C using lead acetate and n-tetrabutyl titanate as starting materials, where sodium hydroxide was served as a mineralizer. Crystalline phases, microstructure and optical properties of PbTiO₃ nanowires were investigated. The PbTiO₃ nanowires were uniform and continuous along the long axis, and were composed of single crystalline PbTiO₃ with a tetragonal perovskite structure. The diameter of a single nanowire was around 12 nm and the length reached up to 3 μm. The chemical composition of the samples and the valence states of elements were determined by X-ray photoelectron spectroscopy (XPS). The ultraviolet/visible absorption spectroscopic investigation suggested that the absorption edge of optical transition of the first excitonic state occurred at around 320 nm. A blue-green light emission peaking at about 471 nm (2.63 eV) is observed at room temperature, and the intensity of this emission increased with increasing excitation wavelength. Oxygen vacancies are responsible for the light emission of PbTiO₃ nanowires.     

Synthesis and characterization of zinc oxide nanoparticles

The research is aimed at synthesis and characterization of nanoscaled zinc oxide particles and their application on linen fibrous supports, for thermal properties. To impart thermal activity to the fibrous nanocomposites, nanoparticles as well as fibrous nanocomposites were produced in different hydrothermal conditions of temperature (90 °C). To characterize the nanoparticles composition, their shape, size, and crystallinity, investigations technique, such as Fourier transformed infrared spectroscopy, scanning electron microscopy, and X-ray powder diffractometry were used. Differential scanning calorimetry analysis profiles were also revealed. The thermal treatment of linen fabrics with nanosized ZnO does not modify significantly their thermal stability.     

Synthesis and characterization of layered zinc hydroxychlorides

Layered material of zinc hydroxychlorides (Zn₅(OH)₈Cl₂·nH₂O: ZHC), which is one of the basic zinc salts (BZS), was synthesized from ZnO nano-particles aged with aqueous ZnCl₂ solutions at different temperatures ranging from 6 to 140 °C for 48 h. X-ray diffraction (XRD) results indicated that the diffraction peaks of ZnO completely disappeared by aging at 6 °C and the ZHC peaks were developed. By increasing the aging temperature, crystallinity of the layered structure was improved. At 6 °C, the ZHC particles were thin hexagonal plate particles with sizes ranging from 1 to 3 μm. The particle size of ZHC was independent of aging temperature. The atomic Cl/Zn ratios of all the ZHC materials were almost 0.2 less than 0.4 of the theoretical ratio, indicating that the synthetic ZHC is Cl-deficient. It seemed that half of Cl atoms in the layer were replaced with HCO₃⁻ and/or OH⁻. The specific surface areas of ZHC estimated from N₂ adsorption isotherms were ca. 10 m² g⁻¹ and were independent of the aging temperature. However, the H₂O monolayer adsorption capacity per unit surface area (n_w) for all the samples was higher than that of ZnO particles, revealing the high affinity of ZHC to H₂O molecules. The n_w values were increased by reducing the crystallinity of ZHC. This enhancement of H₂O adsorption selectivity was thought to be related with less-crystallized parts of the particles.     

钛酸钙的电沉积法制备及表征

采用硝酸钙为钙源,钛酸丁酯为钛源,通过电极沉淀法制备钛酸钙.利用红外光谱仪对制备所得的钛酸钙进行表征.结果显示,在室温条件下,于外加5 V的电场中反应3 h,所得前驱体在800℃下焙烧2 h可得到纯度较高的钛酸钙产品.     

Synthesis and characterization of N-doped zinc oxide nanotetrapods

Nitrogen-doped (N-doped) self-assembled nanotetrapods ZnO were synthesized via chemical vapor deposition process using N₂O as a dopant source via vapor-solid (VS) growth. The decomposition of N₂O gas giving NO and NO₂ during the synthesis provided successful N-doping of the sample. All samples (N-doped and undoped) were characterized by XRD, SEM, TEM, EDX, photoluminescence (PL), Fourier transform infrared (FT-IR), and diffuse reflection spectra. After nitrogen-doping process, N-doped ZnO samples show the change in structural and optical properties. The detailed structure and the growth mechanism of individual ZnO tetrapod is characterized by TEM and SEM investigations. The TEM study gives the direct assumption about the formation of zincblende (sphalerite) structure on the initial stage of growth of N-doped tetrapods. Besides, SEM observation indicated that tetrapods have perfect tetrahedral symmetry. N-Doped ZnO samples exhibit a broad orange-red PL emission band, peaking near 2.1 eV, in good agreement with the deep-acceptor model for the nitrogen impurity. An IR absorption peak at 3146 cm^–1 at room temperature was observed for N-doped sample. This peak has been unambiguously assigned to N–H complex.     

半导体硫化锌纳米微粒的合成与表征

采用液相均沉淀法,用不同原料(采用不同硫源或金属离子螯合剂)从3个途径合成了不同粒径的半导体ZnS纳米粒子,并用透射电子显微镜、X射线粉末衍射仪对粒子进行表征.     

Synthesis and characterization of nanosilica prepared by precipitation method

Nanosilica was prepared by precipitation method and was characterized by various analytical tools. From transmission electron micrograph the silica particles are found to have almost spherical shape with a dimension of 50 nm. The surface area is found to be of 560 m² g⁻¹ and density 2.2 g cm⁻³. From thermogravimetric analysis the total silanol density in the silica is found to be 7.68 nm⁻². A two tier hydration model is proposed from the results of thermogravimetric analysis. The number of reactive silanols that forms hydrogen bond with water molecules is found to be 2.48. The infrared spectral data supports the presence of hydrogen bonded silanol group and the siloxane groups in silica.     

Synthesis and characterization of a novel layered zinc phosphate

The syntheses and crystal structures of a novel layered zinc phosphate and its high temperature variant are described. Both structures were solved from powder diffraction data using both synchrotron and conventional X-ray radiation. The as-synthesized material (UiO-27-as) with composition [C₆H₁₇N₃]²⁺[Zn₃(HPO₄)(PO₄)₂]²⁻·H₂O crystallizes in the space group P2₁/c with a=12.67072(15), b=8.24293(8), c=18.48425(19) Å, β=109.1346(7)° and V=1823.904(35) ų. The zinc phosphate layers are built from corner sharing hexameric secondary building units. In the interlamellar space there are organic cations and water molecules. A high temperature variant exists around 200°C (UiO-27-200). This compound [C₆H₁₇N₃]²⁺[HZn₃(PO₄)₃]²⁻ crystallizes in the monoclinic space group P2₁/c with a=12.29010(23), b=8.39995(13), c=18.49914(30) Å, β=114.2504(11)° and V=1741.261(51) ų. The transformation to UiO-27-200 involves removal of the interlamellar water molecules. The atomic arrangement within the zinc phosphate layers is maintained; however, the layers are brought closer which leads to inter-layer hydrogen bonding interactions.     

Synthesis and characterization of mesoporous zinc layered hydroxide-isoprocarb nanocomposite

The ion exchange method was used to intercalate a poor water-soluble insecticide, isoprocarb into zinc layered hydroxide (ZLH). PXRD analysis indicated the successful intercalation with good crystallinity for the resulting nanocomposite, with a basal spacing of 33.1 Å. FTIR analyses showing the resemblance of an absorption peak of the nanocomposite with the host and the guest anion. The thermal analysis confirmed that the nanocomposite had better thermal stability compared to the pristine isoprocarb. The nanocomposite also characterized by elemental and surface morphology analysis. The surface analyses of the host and nanocomposite showed mesoporous-type material characteristics. On the whole, the intercalation process decreased the pore size of the nanocomposite compared to the pristine host, layered zinc layered hydroxide-sodium dodecyl sulphate (ZLH-SDS). The obtained material is believed has a great potential as an environmentally friendly insecticide.     

Synthesis and characterization of ZnO nanoparticles by thermal decomposition of a curcumin zinc complex

ZnO nanoparticles were generated by thermal decomposition of a binuclear zinc (II) curcumin complex as single source precursor. Thermal behavior of the precursor showed a considerable weight loss at about 374 °C by an exothermic reaction with a maximum weight loss rate of 14%/min. Complete decomposition of precursor was observed within 49 min with a heating rate of 10 °C/min. Synthesized nanoparticles have been characterized by X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and selected area electron diffraction microscopy. Results revealed monodispersed hexagonal zincite structure with an average size of 117 ± 4 nm.     

Exploring hydrothermally grown potassium titanate fibers by STEM-in-SEM/EDX and XRD.

During lab-scale experiments on the reforming of methanol by means of water at supercritical conditions (T > 374 degrees C, p > 22.1 MPa), a tubular reactor with a titanium liner was exposed to an aqueous solvent containing methanol (5 wt%) and KHCO3 (0.3 wt%). At the end of the run, a fibrous precipitate was found at two positions in the reactor. The material was studied in a field emission scanning electron microscope equipped with an energy dispersive X-ray analysis unit (FESEM/EDX). A thin-film support technique using carbon-filmed TEM grids was applied to perform scanning transmission-type imaging (STEM-in-SEM operation) and transmission current measurements. The analysis of the hydrothermally grown fibers resulted in a potassium titanate species composed of approximately K2TiO3, which has been confirmed by X-ray diffraction (XRD).     

Synthesis,characterization and the electrocatalytic application of prussian blue/titanate nanotubes nanocomposite

A novel kind of nanocomposite, titanate nanotubes (TNTs) decorated by electroactive Prussian blue (PB), was fabricated by a simple chemical method. The as-prepared nanocomposite was characterized by XRD, XPS, TEM, FT-IR and Cyclic voltammetry (CV). Experimental results revealed that PB was adsorbed on the surface of TNTs, and the adsorption capacity of TNTs was stronger than that of anatase-type TiO₂ powder (TNP). The PB-TNTs nanocomposite was modified onto a glassy carbon electrode and the electrode showed excellent electroactivity. The modified electrode also exhibited outstanding electrocatalytic activity towards the reduction of hydrogen peroxide and can serve as an amperometric sensor for H₂O₂ detection. The sensor fabricated by casting Nafion (NF) above the PB-TNTs composite film (NF/PB-TNTs/GCE) showed two linear ranges of 2 × 10^?5–5 × 10^?4 M and 2 × 10^?3–7 × 10^?3 M, with a detection limit of 1 × 10^?6 M. Furthermore, PB-TNTs modified electrode with Nafion (NF/PB-TNTs/GCE) showed wider linear range and better stability compared with PB-TNTs modified electrode without Nafion (PB-TNTs/GCE) and PB modified electrode with Nafion (NF/PB/GCE).     

Synthesis and characterization of zinc complexes and reactivity with primary phosphines

Zinc complexes of chelating monoanionic N-donors and neutral diphosphine ligands were synthesized by reaction of diethylzinc with 1,3-diketimine, diazabutadiene, and diphosphine ligand precursors. These complexes were reacted with primary phosphines in an attempt to solicit phosphine dehydrocoupling reactivity. In most cases, insoluble zinc-containing precipitates were formed and ligands were liberated. For the most sterically encumbered complex, (^DippL)ZnEt (3, ^DippL = [(2,6-ⁱPrC₆H₃)NC(CH₃)]₂CH^?), a product assigned as the zinc-phosphide (^DippL)ZnPHPh (6) was observed but could not be isolated as a pure compound. A new, less bulky β-diketiminate complex (^TolL)ZnEt (2, ^TolL = [(p-CH₃C₆H₄)NC(CH₃)]₂CH^?) was reacted with primary phosphines to give a precipitate and the bis(β-diketiminate)zinc complex (^TolL)₂Zn (5), an apparent product of comproportionation. (^MesAI)ZnEt (1, ^MesAI = MesNC(Me)(Et)C(Me) = NMes) and 2 were structurally characterized.