Preparation and characterization of polyimide/Al2O3 hybrid films by sol-gel process

A sol-gel process has been developed to prepare polyimide (PI)/Al2O3 hybrid films with different contents of Al2O3 based on pyromellitic dianhydride (PMDA) and 4,4'-oxydianiline (ODA) as monomers. FESEM and TEM images indicated that Al2O3 particles are relatively well dispersed in the polyimide matrix after ultrasonic treatment of the sol from aluminum isopropoxide and thermal imidization of the gel film. The dimensional stability, thermal stability, mechanical properties of hybrid PI films were improved obviously by an addition of adequate Al2O3 content, whereas, dielectric property and the elongation at break decreased with the increase of Al2O3 content. Surprisingly, the corona-resistance property of hybrid film was improved greatly with increasing Al2O3 content within certain range as compared with pure PI film.

Preparation and Luminescence Properties of YVO4:Ln and Y(V, P)O-4:Ln (Ln = Eu3+, Sm3+, Dy3+) Nanofibers and Microbelts by Sol-Gel/Electrospinning Process

One-dimensional YVO4:Ln and Y(V, P)O-4:Ln nanofibers and quasi-one-dimensional YVO4:Ln microbelts (Ln = Eu3+, Sm3+, Dy3+) have been prepared by a combination method of sol-gel process and electrospinning. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric and differential thermal analysis (TG-DTA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), photoluminescence (PL), low-voltage cathodoluminescence (CL), and time-resolved emission spectra as well as kinetic decays were used to characterize the resulting samples.

Preparation and luminescence properties of Mn2+-doped ZnGa2O4 nanofibers via electrospinning process

One-dimensional Mn2+-doped ZnGa2O4 nanofibers were prepared by a simple and cost-effective electrospinning process. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric and differential thermal analysis (TG-DTA), scanning electron microscopy (SEM), energy-dispersive X-ray spectrum (EDS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), photoluminescence (PL) and cathodoluminescence (CL) spectra as well as kinetic decays were used to characterize the samples. SEM results indicated that the as-formed precursor fibers and those annealed at 700 degrees C are uniform with length of several tens to hundred micrometers, and the diameters of the fibers decrease greatly after being heated at 700 degrees C. Under ultraviolet excitation (246 nm) and low-voltage electron beams (1-3 kV) excitation, the ZnGa2O4:Mn2+ nanofibers presents the blue emission band of the ZnGa2O4 host lattice and the strong green emission with a peak at 505 nm corresponding to the T-4(1)-(6)A(1) transition of Mn2+ ion.

Preparation of SrAl2O4:Eu2+, Dy3+ fibers by electrospinning combined with sol-gel process

One-dimensional SrAl2O4:Eu2+, Dy3+ fibers were fabricated by a simple electrospinning combined with sol-gel process. X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy and photoluminescence were used to characterize the fibers. The results show that the phase structure of SrAl2O4:Eu2+, Dy3+ belongs to a monoclinic one, the composite fibers and fibers calcined at high temperature remain the original one-dimensional texture, and the SrAl2O4:Eu2+, Dy3+ was a green emission. (C) 2010 Elsevier Inc. All rights reserved.

New process for the preparation of 3,5-dihydroxy-1-pentylbenzene

A new process for the preparation of 3,5-dihydroxy-1-pentylbenzene, which is used as medicinal intermediate and raw material for the synthesis of HIV restrainer, is proposed in this paper. Technical 3,5-dimethoxybenzoic acid reacted with lithium hydride to form a salt (I) which acylated n-butyllithium directly to give 1-(3,5-dimethoxyphenyl)-1-pentanone (II) in 85.06% yield. Then (II) was reduced through a Wolff-K-Huangminglong reaction at 210 degrees C to give 3,5-dimethoxy-1-pentylbenzene (III). Finally, (III) refluxed with melt pyridine hydrochloride at 200 degrees C for 2 h to afford the target product 3,5-dihydroxy-1-pentylbenzene (IV). The total yield of (IV) amounted to 61.50% and its mass percentage was 98.22%. The products were characterized by means of IR, H-1-NMR, GC and HLPC-MS. The results indicated that this synthetic route was feasible, characterized by simple process and higher yield, and superior to the published ones.

Preparation and luminescence properties of ormosil hybrid materials doped with Tb(Tfacac)(3)phen complex via a sol-gel process

In this paper, silica-based transparent organic-inorganic hybrid materials were prepared via the sol-gel process. Tetraethoxysilane (TEOS) and 3-glycidoxypropyltrimethoxysilane (GPTMS) were used as the inorganic and organic precursors, respectively. The terbium complex, Tb(Tfacac)(3)phen (Tfacac = 1,1,1-trifluoroacetylacetone, phen = 1, 10-phenanthroline) was successfully doped into organically modified silicate (ormosil) matrix derived from TEOS and GPTMS, and the luminescent properties of the resultant ormosil composite phosphors [ormosil/Th(Tfacac)(3)phen] were investigated compared with those of the Tb(Tfacac)(3)phen incorporated into SiO2 derived from TEOS (labeled as silica/Tb(Tfacac)(3)phen). Both kinds of the materials show the characteristic green emission of Tb3+ ion. The luminescence behavior of the resultant composite products was dependent on the matrix composition. The optimized lanthanide complex concentration in the ormosil/Tb(Tfacac)(3)phen was increased compared with in silica/Tb(Tfacac)(3)phen. Furthermore, the lifetime of Tb3+ in Tb(Tfacac)(3)phen, silica/Tb(Tfacac)(3)phen and ormosil/Tb(Tfacac)(3)phen follows the sequence: onmosil/Tb(Tfacac)(3)phen>silica/Tb(Tfacac)(3)phen>pure Tb(Tfacac)(3)phen.

Preparation and characterization of luminescent thin films doped with rare earth (Tb3+, Eu3+) complexes derived from a sol-gel process

Sol-gel derived luminescent thin films doped with rare earth (RE) complexes were prepared using an in-situ synthesis method with a two-step hydrolysis process and the luminescence spectra were measured. Fluorescence Lifetime and thermal stability were investigated. The results show that a broad excitation band indicates the formation of RE complexes in the solid thin films. RE ions, which are restrained in a silica matrix, present longer lifetime and higher thermal stability than that in DMF/PVB films containing the corresponding pure complexes. (C) 2000 Elsevier Science B.V. All rights reserved.

Preparation of polyimide-BaTiO3 hybrid films by a dispersion process and their microstructure

Barium titanate (BaTiO3) powders with particle sizes of 30 similar to 50 nm were prepared from barium stearate, titanium alkoxides and stearic acid by stearic acid-gel method. Dispersing the agglomerate of BaTiO3 nanoparticles into poly(amic acid) solution followed by curing led to the formation of polyimide hybrid films. The hybrid films were transparent and well distributed with BaTiO3 nanoparticles when the BaTiO3 content was less than 1 wt%. Highly loaded hybrid film containing 30 wit % BaTiO3 was tough, had a smooth surface and possessed much higher dielectric and piezoelectric constants than the parent polyimide.

Preparation and luminescence properties of terbium-Sal complex in-situ synthesized in silica matrix by a two-step sol-gel process

In-situ synthesis of terbium complex with salicylic acid (Sal) in silica matrix was made by a two-step sol-gel process. The terbium complex with salicylic acid was formed in sol-gel derived silica gel, and confirmed by the luminescence excitation spectra and infrared(IR) spectra. As compared to the pure terbium complex powder, the silica gel containing terbium complex exhibits its characteristic emission and presents a longer fluorescence lifetime than that for the pure complex. The luminescence properties of the complex containing;silica gel were investigated and compared with that of both terbium doped the silica gel and thp pure complex powder. The reasons leading to the above results were also discussed.

An in-situ modified sol-gel process for monolith catalyst preparation used in the partial oxidation of methane

An in-situ modified sol-gel method for the preparation of a Ni-based monolith-supported catalyst is reported. With the presence of a proper amount of plasticizer and binder, and at an optimized pH value, the stable boehmite sol was modified with metal ions (Ni, Li, La) successfully without distinct growth of the particle size. Monolith-supported Ni-based/gamma-Al2O3 catalysts were obtained using the modified sol as the coating medium with several cycles of dip-coating and calcination. Combined BET, SEM-EDS, XRD and H-2-TPR investigations demonstrated that the derived monolith catalysts had a high specific surface area, a relatively homogeneous surface composition, and a high extent of interaction between the active component and the support. These catalysts showed relatively stable catalytic activities for partial oxidation of methane (POM) to syngas under atmospheric pressure. The monolith catalysts prepared by this sol-gel method also demonstrated an improved resistance to sintering and loss of the active component during the reaction process.

A study of the relationship between process conditions and mechanical strength of mineralized red algae in the preparation of a marine-derived bone void filler

Bone void fillers that can enhance biological function to augment skeletal repair have significant therapeutic potential in bone replacement surgery. This work focuses on the development of a unique microporous (0.5-10 mu m) marine-derived calcium phosphate bioceramic granule. It was prepared fro Corallina officinalis, a mineralized red alga, using a novel manufacturing process. This involved thermal processing, followed by a low pressure-temperature chemical synthesis reaction. The study found that the ability to maintain the unique algal morphology was dependent on the thermal processing conditions. This study investigates the effect of thermal heat treatment on the physiochemical properties of the alga. Thermogravimetric analysis was used to monitor its thermal decomposition. The resultant thermograms indicated the presence of a residual organic phase at temperatures below 500 degrees C and an irreversible solid-state phase transition from mg-rich-calcite to calcium oxide at temperatures over 850 degrees C. Algae and synthetic calcite were evaluated following heat treatment in an air-circulating furance at temperatures ranging from 400 to 800 degrees C. The highest levels of mass loss occurred between 400-500 degrees C and 700-800 degrees C, which were attributed to the organic and carbonate decomposition respectively. The changes in mechanical strength were quantified using a simple mechanical test, which measured the bulk compressive strength of the algae. The mechanical test used may provide a useful evaluation of the compressive properties of similar bone void fillers that are in granular form. The study concluded that soak temperatures in the range of 600 to 700 degrees C provided the optimum physiochemical properties as a precursor to conversion to hydroxyapatite (HA). At these temperatures, a partial phase transition to calcium oxide occurred and the original skeletal morphology of the alga remained intact.

Process for the preparation of heterocyclyl chalcogenones via reaction of elemental sulfur, selenium, or tellurium with heterocyclic cationic species.

Heterocyclic chalcogenones were prepd. by reaction of S, Se, or Te with ionic liqs. or salts [I; Ra = (substituted) alkyl, cycloalkyl, aryl, aralkyl, alkylaryl; Q = (unsatd.) (substituted) linker to form a ring of 5-10 members; X- = anion selected from conjugate bases of HX having a pKa value of >2.5]. Thus, 1-butyl-3-methylimidazolium acetate was heated with stoichiometric S at 75° for 48 h to give 1-butyl-3-methylimidazole-2-thione. [on SciFinder(R)]

Process for the preparation of water-soluble cellulose hydrolysis products.

The title process comprises admixing cellulose with an ionic liq. capable of solvating or dissolving at least some of the cellulose, the ionic liq. being a compd. comprised solely of cations and anions (e.g., 1-ethyl-3-methylimidazolium sulfate) and which exists in a liq. state at a temp. at or below 150°, and in which the anions are selected from sulfate, hydrogen sulfate and nitrate; and treating the resulting solvate or soln. with an acid in the presence of water, the acid having a pKa in water of less than 2 at 25°. [on SciFinder(R)]

Process for the preparation of water-soluble cellulose hydrolysis products.

The title process comprises admixing cellulose with an ionic liq. capable of solvating or dissolving at least some of the cellulose, the ionic liq. being a compd. comprised solely of cations and anions (e.g., 1-ethyl-3-methylimidazolium sulfate) and which exists in a liq. state at a temp. at or below 150°, the cations in the ionic liq. having the general formula R1Z(R2)(R3)R4: in which Z represents a nitrogen or phosphorus atom, R1 represents a Me or Et group, each of R2 and R3, which may be the same or different, is selected from C4-8alkyl, optionally-substituted benzyl, optionally-substituted Ph, and C5-7cycloalkyl, and R4 represents C1-8 alkyl, optionally-substituted benzyl, optionally-substituted Ph or C5-7cyclohexyl; in which the optional substituents on a benzyl or Ph ring are one, two or three substituents selected from C1-4alkyl or alkoxy groups, halogen atoms and nitro groups; and treating the resulting solvate or soln. with an acid in the presence of water, the acid having a pKa in water of less than 2 at 25°. [on SciFinder(R)]