Preparation and characterization of CuO/SiO2 and NiO/SiO2 with bimodal pore structure by sol-gel method

CuO/SiO₂ and NiO/SiO₂ with bimodal pore structure were prepared by sol-gel reactions of Tetra-methoxysilane (TMOS) and the respective metal nitrate in the presence of poly (ethylene oxide) (PEO) with an average molecular weight of 10 000 and the catalyst of acetic acid. In this process, the interconnected macroporous morphology was formed when transitional structures of spinodal decomposition were frozen by the sol-gel transition of silica. The addition of copper and nickel into the silica-PEO system had a negligible effect on the morphology formation. In gel formation, it was found that NiO crystalline sizes in the samples increased with decreasing Si/Ni molar ratio. It was considered that PEO interacted with both silica and nickel cations. In the CuO/SiO₂ with the presence of PEO_, CuO crystalline sizes were larger than those of NiO/SiO_2. It was considered that there was no obvious interaction between the Cu cation and PEO, most of the copper ions in wet silica gel were present in the outer solution. They easily aggregated as copper salts in the drying process of wet gel and decomposed into CuO particles in heating. While in the CuO/SiO₂ with the absence of PEO, the Cu was selectively entrapped as small particles in the gel skeleton due to the interaction between Cu aqua complex and silica gel network.     

Long-term and thermally stable superhydrophobic surfaces of carbon nanofibers

Carbon nanofibers were prepared from polyvinyl alcohol (PVA) by a simple wetting-compatible method. The surfaces of the aligned carbon nanofibers show excellent thermal- and time-stable superhydrophobicity. The average water contact angle (CA) values are about 153.1+/-2.2 degrees at room temperature, with little difference coming from experimental error. In addition, the CA of the aligned carbon nanofibers surface maintains 139.1+/-3.2 degrees after 10 months of exposure to the ambient environment. Nanostructure on the surface of carbon nanofibers and the intrinsic thermal resistance of carbon contribute to this unique surface property.     

Fabrication and characterization of composition-gradient CuO/SiO2 composite aerogel

With tetramethoxysilane as the silica precursor, CuCl₂·2H₂O as the copper–oxide precursor, acetonitrile as the solvent and gelled by PO via a sol–gel process, the CuO/SiO₂ composite aerogel was fabricated. By adjusting the amount of CuCl₂·2H₂O, CuO/SiO₂ composite aerogels with different molar ratio of Cu/Si such as 1, 5, 10, 20, 30 and 35 % was prepared. Finally, via a self-built device and sol-co-gelation technic, a continuous formation process was developed to fabricate the composition-gradient CuO/SiO₂ composite aerogel. Density of these aerogels was about 200 mg/cm³, the composition-gradient CuO/SiO₂ composite aerogel was cylindrical and about 2.5 cm in height. Scanning electron microscope was used to characterize its microstructure at different position. X-ray diffraction, energy dispersive spectrometer and Fourier transform infrared spectrometer were used to characterize its composition and composition distribution, the results showed that the cylindrical CuO/SiO₂ composite aerogel’s molar ratio of Cu/Si changed from 31.06 to 4.43 % as the measure point from the bottom up, the whole sample displayed obvious composition-gradient.     

Preparation and characterization of vanadium oxide deposited on thermally stable mesoporous titania

Vanadium oxide was deposited on mesoporous titania by the molecular designed dispersion method to investigate the potential properties of these catalysts. Mesoporous titania was synthesized following the evaporation-induced self-assembly (EISA) method with a subsequent treatment with ammonia to increase the thermal stability. As a result, the mesoporous titania obtained shows a high surface area (approximately 350 m2/g) and high stability. Vanadium oxide was deposited by the MDD method using a vanadyl acetylacetonate complex that was transformed into VOx after a controlled calcination in air flow at 300 degrees C. The mesostructure and porosity characteristics of titania remain even until the maximum V-loading was reached (0.4 mmol/g), as it was shown by N2 sorption measurements at -196 degrees C. The catalysts were characterized by chemical analysis, Fourier transform infrared-photoacoustic spectroscopy (FTIR-PAS), UV-vis diffuse reflectance (DR), and Fourier transform Raman spectroscopy. Raman spectra showed isolated V species for the different V-containing catalysts. Furthermore, UV-vis-DR revealed a higher contribution of polymeric species as the V loading increases. The VOx/mesoporous titania catalysts were highly active in the selective catalytic reduction of NOx. A high activity in the NO conversion was observed, which increases with increasing metal loading.     

Novel thermally stable polyimides based on flexible diamine: synthesis, characterization, and properties

A novel diamine with built-in sulfone, ether, and amide structure was prepared via three-step reactions. Nucleophilic reaction of 4-aminophenol with 4-nitrobenzoyl chloride in the presence of propylene oxide led to preparation of N-(4-hydroxy phenyl)-4-nitrobenzamide (HPNB). The nitro group of this compound was reduced with hydrazine and Pd/C to afford 4-amino-N-(4-hydroxy phenyl)benzamide (AHPB). Two moles of AHPB were reacted with bis-(4-chloro phenyl)sulfone to provide a novel sulfone ether amide diamine (SEAD). All the prepared compounds were characterized by common spectroscopic methods. The prepared diamine (SEAD) used to prepare related polyimides by reaction with different aromatic dianhydrides. The obtained poly(sulfone ether amide imide)s were characterized and their properties were studied.     

Preparation and characterization of SiO2 two-step aerogels

Aerogels are well suited as transparent insulation materials in solar architecture and collector systems. Their nanoporous structure provides a high solar transmittance and a low thermal conductivity, generally below 0.02 W m^–1 K^–1. Transparent aerogels with densities above 80 kgm^–3 can easily be prepared at room temperature via a one-step sol-gel process with subsequent supercritical drying. Separating hydrolysis and condensation via a two-step method allows the preparation of transparent ultra-low density SiO₂-aerogels. To optimize the optical properties, characterized by the scattering coefficient of the gels, we have investigated the influence of preparation parameters, such as pH-value of the sol-gel starting solution and macroscopic density, on the gel structure. To determine the nanostructure we performed spectral light scattering as well as small angle X-ray scattering (SAXS) measurements.     

Synthesis and characterization of novel thermally stable aromatic and semiaromatic polyamides derived from thiourea-based flexible diacid dichlorides

Abstract  

New diacid dichlorides bearing phenyl thiourea groups were prepared by a facile synthetic approach and characterized using spectroscopic and elemental analyses. A series of novel aromatic and semiaromatic polyamides were prepared via a condensation route from the synthesized diacid dichlorides with 4,4′-oxydianiline. The polymers were characterized by FT-IR, ¹H NMR, ¹³C NMR, and their physical properties, including their solution viscosities, solubilities and thermal properties, were studied too. Polyamides with phenyl thiourea moieties in the backbone showed good solubilities in amide solvents such as DMAc, DMF, DMSO, and NMP. All of the synthesized polymers had η _inh values of 0.042–0.053 dm³/g, and were obtained in quantitative yield. GPC measurements of the synthesized polyamides indicated M _w values of 64,759–86,172. The crystallinity of the polymers was evaluated via their X-ray diffraction patterns. Their glass transition temperatures were found to be 218–229 °C. Furthermore, thermogravimetric analysis indicated that the polymers were thermally stable in the range 300–398 °C in a N₂ atmosphere.     

Synthesis and characterization of thermally stable sulfonated polybenzimidazoles

A series of sulfonated polybenzimidazoles (sPBI-IS) with controlled sulfonation degrees (SDs) were synthesized from various stoichiometric ratio mixtures of 5-sulfoisophthalic acid monosodium salt (SIPN), 4,4′-sulfonyldibenzoic acid and 3,3′-diaminobenzidine by solution copolycondensation in poly(phosphoric acid). The resulting sulfonated polymers were characterized by means of FTIR, ¹H NMR and GPC, in addition to TGA and DMA. The number-average molecular weights (M_n) of the sPBI-IS are in the range of 45,500-64,000, and the polydispersity indices (M_w/M_n) vary from 1.9 to 2.4. The synthesized sPBI-IS samples present good solubilities in polar aprotic solvents and they are easy to form the transparent, flexible and tough films by solution casting. These polymer membranes show excellent thermal stabilities and dynamic mechanical properties. The thermal stability of the sodium form sPBI-IS remarkably increases with increasing SD. However, the acidic form sPBI-IS presents less thermal stability than the non-sulfonated sample (sPBI-IS0). The onset decomposition temperature (T_d) and the glass-transition temperature (T_g) of the acidic form sPBI-IS70 are 439 °C and 196 °C, respectively. The sulfonated membranes show higher storage moduli and loss moduli than sPBI-IS0. The resulting sPBI-IS membranes with high hygroscopicity show potential application as the high temperature proton exchange membrane in fuel cell.     

Preparation and characterization of poly(butylene terephthalate) nanocomposites from thermally stable organic-modified montmorillonite

In this paper, cetyl pyridium chloride (CPC) was employed to modify the montmorillonite. TGA analysis shows that the organic modified clay has higher thermal stability than hexadecyl trimethyl ammonium chloride modified montmorillonite and is suitable to be used for preparing poly(butylene terephthalate) (PBT)/clay nanocomposites at the high temperature. And then PBT/clay nanocomposites were prepared by direct melt intercalation. The results of XRD, TEM and HREM experiments show the formation of exfoliated-intercalated structure. The thermal stability of the nanocomposites does not evidently decrease, but the char residue at 600 °C remarkably increase compared with pure PBT. DSC results indicate that clay improves the melting temperature, the crystallization rate and crystallinity of the PBT molecules in the nanocomposites.     

Preparation and characterization of crosslinked chitosan-based nanofibers

Crosslinked chitosan-based nanofibers were successfully prepared via electrospinning technique with heat mediated chemical crosslinking followed.The structure,morphology and mechanical property of nanofibers were characterized by attenuated total reflection-Fourier transform infrared spectroscopy(ATR-FTIR),scanning electron microscopy(SEM),Instron machine,respec- tively.The results showed that,nanofibers exhibited a smooth surface and regular morphology,and tensile strength of nanofibers improved with increasing of triethylene glycol dimethacrylate(TEGDMA)content.     

Preparation and characterization of polymer composite multilayers on SiO2

Poly(diallyldimethylammonium chloride) (PDADMAC) and poly(sodium 4-styrenesulfonate) (PSS) have been consecutively adsorbed onto 1.5-microm charged silica (SiO2) particles. Time-dependent adsorption studies indicate that, due to the strong ionic charge of the dissociated polycation in water, adsorption is complete in less than 30 min. Indications of the maximum adsorption density, changes in surface charge, and stability of the layered particles are demonstrated through adsorption isotherms and electrophoretic mobility (EPM) measurements. Further stability of the PDADMAC layer is demonstrated through multiwashing with ultra pure deionized water. Preliminary desorption studies of the PSS layer also illustrate a stabilized two-layer system. Due to the nature of the electrostatic charges on the surface of the SiO2 core particles and both polyelectrolytes in aqueous media, the use of polyelectrolytes as layering elements serves as a model for the assembly of time-released drug delivery particle systems.     

魔芋葡甘聚糖／SiO2纳米复合物的制备与表征

用纳米SiO2为原料,以魔芋葡甘聚糖(KGM)为基体,采用共混法制得KGM/SiO2纳米复合物。通过傅立叶红外光谱(FTIR)、热重分析(TG)、透射电镜(TEM)等手段对该体系进行了表征。结果表明:由于纳米SiO2粒子的引入,KGM分子FTIR的某些特征峰的波数发生明显变化;纳米SiO2在复合物中的分散性较好;复合材料的热稳定性高于KGM薄膜;此外,复合材料的力学性能有所提高。     

Preparation and characterization of aqueous stable electro-spun nanofibers using polyvinyl alcohol/polyvinyl pyrrolidone/zeolite

Cross-linked polyvinyl alcohol/polyvinyl pyrrolidone/zeolite fibers were prepared in the presence of potassium peroxodisulphate (K₂S₂O₈) under the curing process by the electrospinning technique. The narrowest nanofibers of PVA/PVP (50:50) were prepared under optimum experimental conditions of 2.5 × 10^?4 mol of K₂S₂O₈, an applied voltage of 22 KV, the distance of 15 cm and the feed rate of 0.2 mL/h. The progress of the cross-linking was examined by immersion of the prepared nanofibers in water and following the swelling degrees. By raising the K₂S₂O₈ amount and curing time, the cross-linking density was increased. X-ray diffraction (XRD) demonstrated that the crystallinity of the nanofibers was decreased by the increase of K₂S₂O₈ and the lowest crystallinity was observed for PVA/PVP (70:30). The contact angle of nanofibers was decreased from 72° to 34 by increasing PVP ratio from 30 to 70. The morphology of the nanofibers before and after immersion in the simulated body fluid (SBF) was studied using electron scanning microscopy (SEM) and PVA/PVP (70:30) showed the highest changes in the morphology while the lowest one was observed for PVA/PVP (50:50). Moreover, the cross-linked PVA/ PVP with the ratio of 50:50 had the narrowest diameter of 200 ± 100 nm, and by addition of about 0.5% zeolite, it was even reduced more to 150 ± 50 nm. The cross-linked nanofibers (50:50) with 0.5 wt% and 1.5 wt% zeolite nanoparticles showed the tensile modules of 416.26 and 703.52 MPa, respectively, while in the absence of zeolite, it was209.25 MPa. Fibroblast L929 cells were cultured on the cross-linked PVA/PVP/zeolite (50:50:0.5) nanofiber, and the cell proliferation and growth was evaluated by MTT (3-(4, 5-dimethylthiazol-2-yl)-2, 5-diphenyltetrazolium bromide) assay. Fibroblasts grew on the surface of scaffold showed good morphology and proliferation after seven days and the absorption amount was increased from 0.075 to 0.78     

SiO2@Fe2O3核-壳结构催化剂的制备及表征

采用优化的Stöber法制备了平均粒径为230 nm的单分散球形SiO₂颗粒,并以此为内核,通过水解沉积法制备了不同壳层厚度的核-壳结构SiO₂@Fe₂O₃催化剂。采用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、N₂物理吸附和X射线衍射分析(XRD)等手段对催化剂进行表征,探讨了不同制备条件对SiO₂@Fe₂O₃催化剂形貌的影响。结果表明,通过水解沉积法制备的SiO₂@Fe₂O₃催化剂具有明显的核-壳结构,并且保持了原始SiO₂核的球形形貌,Fe₂O₃纳米粒子通过-OH的氢键作用连接在SiO₂表面,形成了2~10 nm厚的Fe₂O₃均匀连续包覆层。     

Synthesis and characterization of three new thermally stable N-heterocyclic germylenes

Three new stable germylenes, rac-1,3-di-tert-butyl-4,5-dimethyl-1,3-diaza-2-germacyclopentane-2-ylide (1), 1,3-di-tert-butyl-4,4-dimethyl-1,3-diaza-2-germacyclopentane-2-ylide (2), and rac-1,3,4-tri-tert-butyl-1,3-diaza-2-germacyclopentane-2-ylide (3) have been synthesized by the reaction of their corresponding germyl dichlorides with elemental lithium. Full synthetic procedures and characterizations are described.     

α-K8P2W17CuO61纳米纤维的制备与表征

运用高压静电纺丝和程序焙烧方法，制备α-K8P2W17CuO61纳米纤维丝．通过红外光谱（FT-IR），X-射线粉末衍射（XRD）进行了表征，结果表明制备的纳米丝是纯α-K8P2W17CuO61，扫描电子显微镜照片（SEM）显示焙烧后产物为纳米纤维丝，其平均直径大约为150nm．     

Preparation and characterization of novel organosoluble and thermally stable poly(benzimidazole-amide)s bearing phthalimide pendent groups

Novel aromatic poly(benzimidazole-amide)s, PBAs, have been synthesized by direct polycondensation of a new dicarboxylic acid, N-[3,5-bis(5-carboxylic acid-2-benzimidazole) phenyl]phthalimide (1), containing performed benzimidazole rings and a phthalimide pendent group with various aromatic diamines. The dicarboxylic acid was synthesized by reaction of 5-(N-phthalimide)isophthalic acid with 4-methyl-1,2-phenylenediamine in polyphosphoric acid, followed by its oxidation into relative dicarboxylic acid. To study the structure-property relationships of 1,3-bis(5-carboxylic acid-2-benzimidazole)benzene (2, as a reference) this compound was also synthesized. The chemical structure of 1 and 2 were confirmed by the spectroscopic methods and elemental analyses. The characterization of the polymers was performed with inherent viscosity measurements, solubility tests, FT-IR, Ultraviolet and ¹H NMR spectroscopy and thermogravimetry. The polymers were obtained in quantitative yields with inherent viscosities between 0.53 and 0.91 dl g⁻¹. The effects of the phthalimide pendent group on the polymer properties such as solubility and thermal behavior were investigated and compared with those of the corresponding unsubstituted poly(benzimidazole-amide)s. The modified poly(benzimidazole-amide)s showed enhanced solubilities in some solvents, such as m-cresol and pyridine, in comparison to the unmodified analogues. In addition, the incorporation of the pendent phthalimide groups in the poly(benzimidazole-amide)s backbone increased remarkably the thermal stability of the polymer. The glass transition temperature and 10% weight loss temperature of the poly(benzimidazole-amide)s were in range of 291-334 °C and 466-540 °C, respectively, in nitrogen.     

Preparation and characterization of porous TiO_2/ZnO composite nanofibers via electrospinning

<正>Porous TiO_2/ZnO composite nanofibers have been successfully prepared by electrospinning technique for the first time.It was generated by calcining TiO_2/ZnCl_2/PVP[PVP:polyvinyl pyrrolidone)]nanofibers,which were electrospun from a mixture solution of TiO_2,ZnCl_2 and PVP.Transmission electron microscopy(TEM) and X-ray diffraction(XRD) analyses were used to identify the morphology of the TiO_2/ZnO nanofibers and a formation of inorganic TiO_2/ZnO fibers.The porous structure of the TiO_2/ZnO fibers was characterized by N_2 adsoption/desorption isotherm.Surface photovoltage spectroscopy(SPS) and photocatalytic activity measurements revealed advance properties of the porous TiO_2/ZnO composite nanofibers and the results were compared with pure TiO_2 nanofibers,pure ZnO nanofibers and TiO_2/ZnO nanoparticles.