224 resultados para in situ Mossbauer spectroscopy


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Synchrotron small angle X-ray scattering was used to study the deformation mechanism of high-density polyethylene that was stretched beyond the natural draw ratio. New insight into the cooperative deformational behavior being mediated via slippage of micro-fibrils was gained. The scattering data confirm on the one hand the model proposed by Peterlin on the static structure of oriented polyethylene being composed of oriented fibrils, which are built by bundles of micro-fibrils. On the other hand it was found that deformation is mediated by the slippage of the micro-fibrils and not the slippage of the fibrils. In the micro-fibrils, the polymer chains are highly oriented both in the crystalline and in the amorphous regions. When stretching beyond the natural draw ratio mainly slippage of micro-fibrils past each other takes place. The thickness of the interlamellar amorphous layers increases only slightly. The coupling force between micro-fibrils increases during stretching due to inter-microfibrillar polymer segments being stretched taut thus increasingly impeding further sliding of the micro-fibrils leading finally to slippage of the fibrils.

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A new-type Mg2Si composite was prepared with Mg-9Al-1Zn (AZ91) alloy and vermiculite as raw materials by melt infiltration method. The results show that the microstructure of composite consists of a large amount Of Mg2Si precipitates and a little amount of MgO embedded in alpha-Mg matrix. The Vickers hardness of the composite is obviously higher than that of matrix of AZ91 alloy. Moreover, the composite exhibits excellent compressive property. The ultimate compressive strength of the material is 290 MPa, the yield strength is 175 MPa, and the elongation is about 5%, which are higher than those of AZ91 alloy.

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A new process of graft copolymerization of poly(vinyl chloride) (PVC) and polyethylene (PE) with other monomers was developed. The grafted chlorinated poly(vinyl chloride) (CPVC) and chlorinated polyethylene (CPE) were synthesized by in situ chlorinating graft copolymerization (ISCGC) and were characterized. Convincing evidence for grafting and the structure of graft copolymers was obtained using FT-IR, H-1-NMR, gel permeation chromatography (GPC), and the vulcanized curves. Their mechanical properties were also measured. The results show that the products have different molecular structure from those prepared by other conventional graft processes. Their graft chains are short, being highly branched and chlorinated. The graft copolymers have no crosslinking structure. The unique molecular structure will make the materials equipped with special properties.

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A new straightforward strategy for synthesis of novel hyperbranched poly (ether amide)s from readily available monomers has been developed. By optimizing the reaction conditions, the AB(2)-type monomers were formed dominantly during the initial reaction stage. Without any purification, the AB(2) intermediate was subjected to further polymerization in the presence (or absence) of an initiator, to prepare the hyperbranched polymer-bearing multihydroxyl end-groups. The influence of monomer, initiator, and solvent on polymerization and the molecular weight (MW) of the resultant polymers was studied thoroughly. The MALDI-TOF MS of the polymers indicated that the polymerization proceeded in the proposed way. Analyses of H-1 NMR and C-13 NMR spectra revealed the branched structures of the polymers obtained. These polymers exhibit high-moderate MWs and broad MW distributions determined by gel permeation chromatography (GPC) in combination with triple detectors, including refractive index, light scattering, and viscosity detectors. In addition, the examination of the solution behavior of these polymers showed that the values of intrinsic viscosity [eta] and the Mark-Houwink exponent a were remarkably lower compared with their linear analogs, because of their branched nature.

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inorganic-organic hybrid nanoparticles multilayer films were fabricated by extending the method of nucleation and growth of particles in polymer assemblies. The polyelectrolyte matrix was constructed by layer-by-layer self-assembly method. Synthesis of polyoxometalate nanoparticles was achieved by alternately dipping the precursor polyelectrolyte matrix into AgNO3 and H4SiW12O40 aqueous solutions. Repeating the above synthesis process, Ag4SiW12O40 nanoparticles with controllable diameters of 20 to 77 nm were synthesized in the multilayer films in-situ. UV-vis absorption spectra indicate that the nanoparticles grew gradually in the synthesis process. Transmission electron microscopy was used to observe the size and morphology of the nanoparticles.

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Silica-gel nanowire/Na+-montmorillonite (Na+-MMT) nanocomposites were prepared by the in situ sol-gel process of tetraethyl orthosilicate (TEOS) in the presence of Na+-MMT and ammonia as catalyst. Microstructure characterization of the nanocomposites was done by SEM, , EDX, XRD and FTIR. It was found that a lot of silica-gel nanowires grew along the edges of Na+-MMT. The combination between the nanowires and Na+-MMT was accomplished via polycondensation of the hydrolyzed TEOS and the edge-OH groups of Na+-MMT.

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SiO2/polyacrylamide (PAM) composite was prepared via the polymerization of acrylamide in the presence of silica sol in water/hexane emulsion, and pure SiO2 was also prepared without the use of acrylamide in the same way. Field emission scanning electron micrographs (FESEM) showed that PAM covered the silica nanoparticles to form SiO2/PAM nanospheres, which loosely agglomerated to form SiO2/PAM secondary particles, while SiO2 secondary particles were made up of tightly agglomerated silica nanoparticles. Metallocene catalyst was then immobilized over SiO2 and SiO2/PAM respectively to prepare supported metallocene catalyst for ethylene polymerization. Transmission electron micrographs (TEM) showed that support particles broke up to smaller particles and even nanoparticles in polyethylene (PE) matrix when the support particles were the fragile SiO2/PAM secondary particles, which shows a novel way to prepare silica/polyacrylamide/polyethylene nanocomposite.

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A novel approach to the preparation of polyethylene (PE) nanocomposites, with montmorillonite/silica hybrid (MT-Si) supported catalyst, was developed. MT-Si was prepared by depositing silica nanoparticles between galleries of the MT. A common zirconocene catalyst [bis(cyclopentadienyl)zirconium dichloride/methylaluminoxane] was fixed on the MT-Si surface by a simple method. After ethylene polymerization, two classes of nanofillers (clay layers and silica nanoparticles) were dispersed concurrently in the PE matrix and PE/clay-silica nanocomposites were obtained. Exfoliation of the clay layers and dispersion of the silica nanoparticles were examined with transmission electron microscopy. Physical properties of the nanocomposites were characterized by tensile tests, dynamic mechanical analysis, and DSC. The nanocomposites with a low nanofiller loading (<10 wt %) exhibited good mechanical properties. The nanocomposite powder produced with the supported catalyst had a granular morphology and a high bulk density, typical of a heterogeneous catalyst system.

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Polyaniline (PANI) was cathodically synthesized at an evaporated gold electrode using an in situ electrogenerated intermediate as oxidant during reduction of the dissolved oxygen. The obtained PANI layer showed an electrochemical response similar to that synthesized by the conventionally anodic polymerization, and the average rate for the growth of PANI layer at polycrystalline gold electrode was 1.59 nm h(-1), while that at the Au (111) electrode was 4.93 nm h(-1). Based on these results, the thickness of the resulted layer can be easily controlled at molecular level for potential nanodevice applications. The obtained PANI layer showed morphology from an island-like nanostructure to an ultrathin film, depending on the crystal orientation of the electrode used.

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Single-walled carbon nanotubes (SWNTs) were modified with polyethylene (PE) prepared by in situ Ziegler-Natta polymerization. Because of the catalyst pre-treated on the surface of the SWNTs, the ethylene was expected to polymerize there. Scanning electron microscopy images and solubility measurements showed that the surface of the SWNTs was covered with a PE layer, and a crosslink may have formed between the SWNTs and PE. When the SWNTs covered with a PE layer were mixed with commercialized PE by melt blending, the resulting composite had better mechanical properties than the composite from the SWNTs without a PE layer. The yield strength, the tensile strength and modulus, the strain at break, and the fracture energy of the modified-SWNT/PE composites were improved by 25, 15.2, 25.4, 21, and 38% in comparison with those of the raw-SWNT/PE composites.

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Lanthanide-doped sol-gel-derived materials are an attractive type of luminescent materials that can be processed at ambient temperatures. However, the solubility of the lanthanide complexes in the matrix is a problem and it is difficult to obtain a uniform distribution of the complexes. Fortunately, these problems can be solved by covalently linking the lanthanide complex to the sol-gel-derived matrix. In this study, luminescent Eu3+ and Tb3+ bipyridine complexes were immobilized on sol-gel-derived silica. FT-IR, DTA-TG and luminescence spectra, as well as luminescence decay analysis, were used to characterize the obtained hybrid materials. The organic groups from the bipyridine-Si moiety were mostly destroyed between 220 and 600 degreesC. The luminescence properties of lanthanide bipyridine complexes anchored to the backbone of the silica network and the corresponding pure complexes were comparatively investigated, which indicates that the lanthanide bipyridine complex was formed during the hydrolysis and co-condensation of TEOS and modified bipyridine. Excitation at the ligand absorption wavelength (336 nm for the hybrid materials and 350 nm for the pure complexes) resulted in strong emission of the lanthanide ions: Eu3+ D-5(0)-F-7(J) (J = 0, 1, 2, 3, 4) and Tb3+ D-5(4)-F-7(J) (J = 6, 5, 4, 3) emission lines due to efficient energy transfer from the ligands to the lanthanide ions.

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A facile strategy for the in situ synthesis of terbium complex-silica nanocomposites is described. The resultant spherical nanocomposites possess good monodispersity and exhibit luminescent properties of terbium complex.