八—4—(四氢糠氧基)双酞菁衍生物钕(Ⅲ)、铕(Ⅲ)的合成和LB膜的气敏性

八—４—（四氢糠氧基）双酞菁衍生物钕（Ⅲ）、铕（Ⅲ）的合成和ＬＢ膜的气敏性张引＊辛春梅王丹（吉林省教育学院化学系，长春１３００２２）梁冰洁＊＊陈文启席时权（中科院长春应用化学研究所，长春１３００２２）关键词：希土双酞菁衍生物ＬＢ膜气敏性荧光性紫外可见...     

Fabrication of high performance thin films from metal fluorocomplex aqueous solution by the liquid phase deposition

The hetro-structured oxide thin films from metal fluorocomplex solution have been prepared by the liquid phase deposition (LPD) method. The Pt/Nb₂O₅ and Au/Nb₂O₅ composite films can be prepared from a mixed solution of niobium source, H₃BO₃, Pt(NH₃)₄Cl₂ and HAuCl₄ aqueous solutions under the ambient temperature and atmosphere. In the case of Au/SiO₂ composite film, (NH₄)₂SiF₆ solution is used as a mother solution. The Pt and Au ionic species are deposited in Nb₂O₅ and SiO₂ matrices. They are reduced to their metallic state after treatment above 200 °C. The size of dispersed particles can be controlled by heat treatment temperature. It is also clear that, gold nanoparticles are also found to interact with SiO₂, although the interaction is smaller than that with Nb₂O₅ showing the size of Au nanoparticles remain smaller in Nb₂O₅ that in SiO₂.     

Synthesis and properties of niobia films derived from niobium pentaethoxide

The hydrolysis of niobium pentaethoxide precursor in the presence of triethylamine (TEA) is discussed. Three precursors with TEA/Nb(OEt)₅ mole ratios of 0.25, 0.4 and 0.8 were prepared. Niobia colloids with different appearance were obtained after autoclaving the above precursors at 250°C during 12 h. The surface roughness and microstructure of niobia films prepared with the colloids by spread coating method are strongly dependent on the TEA/Nb(OEt)₅ mole ratio. At a value of 0.4 TEA/Nb(OEt)₅ mole ratio, a niobia film with large surface roughness can be achieved. It is opaque and mechanically stable and has differently ordered needle microstructure. The crystalline structure and photoelectrochemical property of niobia film with the largest surface roughness were examined. The effect of CO₂ gas bubbling, reflux and addition of 2-methoxyethanol on the hydrolysis of Nb(OEt)₅ and the nature of the Nb₂O₅ films is also discussed.     

α-Fe2O3纳米微粒/硬脂酸交替L-B膜的结构表征

We reported in this paper FTIR linear diehroic spectroscopy and anisotropic properties of the nanoparticulate α-Fe_2O_3-stearate alternating Langmuir-Blodgett films (Fe_2O_3-St LB films) a new inorganic-organic quantum superlattice system. A new method fitted to inorganic-organic alternating films is used to study the molecular orientation and discuss the order arrangement of the nanopartieles in the films. The the results show that a configuration of stearate ions bound to the surface of the nano-particles: COO~- group are spherically bound to the surface of the nanoparticles; the hydrocarbon chains are almost perpendicular (31°±5°) to the substrate (7 nm-Fe_2O_3-St LB films). The orientation of hydrocarbon chains and CH_2 scissors vibration show the existence of trans-zigzag planar structure for C—C broken bone of the hy7drocarbon chains, which is related to high-order structure of the alternate films.     

红外光谱法研究LB膜中的分子取向

The structure information of orientation and packing of molecular chains can be obtained from infrared transmission and reflection-absorbance (RA) spectra. In the present paper, on the basis of Umemura et al., their FORTRAN program of minicomputer was developed and can be run on 486 personal computer. By comparison of infrared transmission and RA intensities, surface enhancement factors and molecular orientation angle were calculated using the above program, and the influence of complex refractive index, angle of incidence, and thickness of LB film were discussed. These results are consistent with that of Umemura et al.     

JEE—4x型真空镀膜仪功能扩展

报道了对ＪＥＥ－４ｘ型真空镀膜仪蒸发装置的改进以及建立蒸发材料回收装置的具体方法，并介绍了改进后该仪器在高分辨扫描电镜样品制备上的应用实例．实验证明，上述改进不但扩展了ＪＥＥ—４ｘ型真空镀膜仪的制样功能又节省了蒸发材料，集中了离子溅射法及常规高真空镀膜法的优点，完全满足ＳＥＭ样品的分析要求，该方法简单易操作．     

阳极氧化膜WO3（Ⅱ）：电显色的介质效应

用循环计时电量法、循环伏安法、电化学现场(in-situ)紫外可见反射光谱技术和光电流谱技术研究了溶剂和阳离子(H~+,Li~+)对阳极氧化膜WO_3电显色稳定性和过程的影响。从循环计时电量图可以测定表征膜稳定性的氢或锂的累积量和暂态周期数。实验发现W/WO_3/LiCLO_4乙腈溶液体系具有高的电显色稳定性。引起WO_3膜可逆电显色的H~+和Li~+离子的嵌-脱过程的界面电化学机理不同。着色态WO_3膜的色心是自由电子,其密度超过10~(21)/cm~3,生色机理是等离子体振荡。     

Direct and simultaneous voltammetric analysis of heavy metals in tap water samples at Assiut city: an approach to improve the analysis time for nickel and cobalt determination at mercury film electrode

Tap water samples (Assiut city, lie in the middle north of upper Egypt, approx. 370 km from Cairo, January-March, 2002) were taken from the eight sampling sites of different locations at Assiut city. The samples are analyzed to determine the total content of cadmium, copper, lead and zinc by differential pulse anodic stripping voltammetry (DPASV) while nickel and cobalt are determined by a new simple differential pulse adsorptive stripping voltammetry (DPAdSV), using dimethylglyoxime (DMG) as the complexing agent. This method uses sodium sulfite as the supporting electrolyte, which facilitates the removal of oxygen interference without the traditional necessity of purging with inert gas. The effect of various parameters was studied using DPASV (for Cd, Pb, Cu and Zn) and AdSV (for Ni and Co) methods. Subsequently, under the so found experimental conditions, the stability of calibration curves and the detection limits (μg/l) have been determined. The data achieved (for all metals utility) are comparable to those measured by the graphite furnace atomic absorption spectrophotometric (GF-AAS) method. The effects of the interferences between these metal ions have been investigated. Moreover, the effect of storage was discussed and the obtained results were compared favorably with standard official methods. Statistical analysis of the database exhibits applicability and the accuracy of the techniques. The results obtained from the two techniques (Voltammetry and GF-AAS) are in very good agreements in the most tap water samples.     

Influence of molecular characteristics on overall isothermal melt-crystallization behavior and equilibrium melting temperature of syndiotactic polypropylene

Overall isothermal melt-crystallization and subsequent melting behavior of metallocene-catalyzed syndiotactic polypropylene resins of various molecular weights were investigated using differential scanning calorimetry (DSC) technique. Two sets of molecular weight range were synthesized with two different metallocene catalyst systems. The kinetics of the overall isothermal melt-crystallization process was analyzed based on various macrokinetic models, i.e. the Avrami, Malkin and Urbanovici-Segal models. The effective activation energy describing the overall isothermal crystallization process over the crystallization temperature range studied was estimated based on an Arrhenius approximation of the obtained Avrami crystallization rate constants. The equilibrium melting temperature for each of these resins was estimated based on the linear and non-linear Hoffman-Weeks extrapolative methods.     

Photodegradation of polypropylene thermal bonded non-woven fabric

Samples of thermal bonded polypropylene non-woven fabrics were exposed to light from two TUV 30W G30T8 Philips lamps (λ = 253.7 nm) in a covered open-air chamber at room temperature (25 °C and 55% relative humidity) for different periods of time. In order to determine the state of degradation, the samples were examined by optical microscopy, scanning electron microscopy, staining with an isopropanol solution of methylene blue and Sudan III, colourimetry, Fourier transform infrared (FTIR) spectroscopy and density measurements. Although the bonded areas formed under complex thermal and mechanical deformations during the fabric production, no localized staining was observed. The colour of the irradiated and stained fabrics changed uniformly due to the even production of polar groups in the process of irradiation. It was found that the change of redness and blueness of degraded and stained samples can be correlated linearly with the evolution of POOH groups as determined by FTIR spectroscopy. Products containing carbonyl (CO), hydroxyl and/or hydroperoxide (POOH) groups increase with time of degradation with a non-linear relation. It was also observed that the density and 997 cm⁻¹/972 cm⁻¹ FTIR absorbance ratio increases with degradation time. Density fluctuation and the build up of degradation products caused fibre cracks and embrittlement.