Characterization and physical properties of polymethylphenylsilsesquioxane (PMPSQ) and hydroxyl‐functionalized polystyrene (PS–OH) hybrids

Polymethylphenylsilsesquioxane (PMPSQ–OH) and trimethylsilyl end‐blocked PMPSQ (PMPSQ–EC) were prepared. The thermal decomposition behavior of these polymers was studied by thermogravimetric analysis (TGA) and FT‐Raman spectroscopy. Hydroxyl‐functionalized polystyrene (PS–OH) was also prepared by anionic living polymerization. Thin hybrid films of PMPSQ/PS–OH with various blend ratios were obtained by spin‐coating on freshly cleaned glass. The surface morphology of the hybrid films was investigated by atomic force microscopy (AFM). In 80/20 PMPSQ/PS–OH hybrid film, the PS–OH component produced a very uniformly dispersed phase. This hybrid film contained small domains of PS–OH whose size ranged from 60 to 80 nm. As the content of PS–OH was increased, the domain morphology coarsened and phase inversion took place around 50 wt %. In the phase‐inversed system, the PMPSQ‐rich phase was uniformly distributed in the PS–OH‐rich continuous phase. In addition, temperature‐dependent dielectric properties of PMPSQ/PS–OH hybrids were investigated. Relaxation of the hybrids was observed with an increasing content of the PS–OH component due to the amorphous glass transition behavior of PS–OH. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 90: 2801–2812, 2003     

不同空间插值方法在辽西降水空间插值的精度对比分析

本文结合区域降水站点实测降水数据,对比分析了反距离加权插值和克里金插值方法在辽西降水空间插值的精度。研究结果表明:反距离加权插值法由于考虑插值点之间的权重,在辽宁西部降水空间插值的精度高于克里金插值方法,反距离加权插值方法下降水插值和实测降水之间年和月尺度的误差分别为6.2%和20.7%,年相关系数达到0.79,克里金插值方法下降水插值和实测降水之间年和月尺度误差分别为10.9%和24.6%,年相关系数为0.51,反距离插值方法更适用于辽西地区的降水空间插值计算。研究成果可为辽宁西部无资料地区降水空间插值计算提供方法参考。     

Efficient and color pure blue light emitting random copolymer with fluorene and fluorenylstilbene

A blue electroluminescent polymer, random copolymer of fluorenylstilbene and fluorene, was prepared by the nickel catalyzed coupling reaction. The structure and properties of the copolymer were analyzed by various spectroscopic methods. The obtained polymer had good solubility and thermal stability with high T_g. The polymer in thin film emits strong blue luminance (max=468 nm) with narrow bandwidth upon photoexcitation. PL spectrum of the polymer in the film is almost consistent with that of solution one as well as the EL spectrum, indicating that the aggregation and the excimer fluorescence are suppressed by the introduction of fluorenylstilbene comonomer. Moreover, the introduction of fluorenylstilbene comonomer lowered the oxidation potential to lead feasible hole injection, when the compared with poly(fluorene) homopolymer. The ITO/PEDOT/polymer/LiF/Al device showed the maximum brightness of 3500 cd/m² with a turn on voltage of 4.4, the maximum efficiency of 0.878 lm/W and blue emission with CIE chromaticity coordinates of ((x,y)=(0.17, 0.25)).     

Chattering free full-order sliding-mode control

In conventional sliding-mode control systems, the sliding-mode motion is of reduced order. Two main problems hindering the application of the sliding-mode control are the singularity in terminal sliding-mode control systems and the chattering in both the conventional linear sliding-mode and the terminal sliding-mode control systems. This paper proposes a chattering-free full-order terminal-sliding-mode control scheme. Since the derivatives of terms with fractional powers do not appear in the control law, the control singularities are avoided. A continuous control strategy is developed to achieve the chattering free sliding-mode control. During the ideal sliding-mode motion, the systems behave as a desirable full-order dynamics rather than a desirable reduced-order dynamics. A systematic design method of full-order sliding-mode control for nonlinear systems is presented, which allows both the chattering and singularity problems to be resolved. Simulations validate the proposed chattering free full-order sliding-mode control.     

Microstructure and Properties of Spark Plasma-Sintered ZrO2–ZrB2 Nanoceramic Composites

In a recent work, ¹ we have reported the optimization of the spark plasma sintering (SPS) parameters to obtain dense nanostructured 3Y-TZP ceramics. Following this, the present work attempts to answer some specific issues: (a) whether ZrO₂-based composites with ZrB₂ reinforcements can be densified under the optimal SPS conditions for TZP matrix densification (b) whether improved hardness can be obtained in the composites, when 30 vol% ZrB₂ is incorporated and (c) whether the toughness can be tailored by varying the ZrO₂–matrix stabilization as well as retaining finer ZrO₂ grains. In the present contribution, the SPS experiments are carried out at 1200°C for 5 min under vacuum at a heating rate of 600 K/min. The SPS processing route enables retaining of the finer t -ZrO₂ grains (100–300 nm) and the ZrO₂–ZrB₂ composite developed exhibits optimum hardness up to 14 GPa. Careful analysis of the indentation data provides a range of toughness values in the composites (up to 11 MPa·m^1/2), based on Y₂O₃ stabilization in the ZrO₂ matrix. The influence of varying yttria content, t -ZrO₂ transformability, and microstructure on the properties obtained is discussed. In addition to active contribution from the transformation-toughening mechanism, crack deflection by hard second phase brings about appreciable increment in the toughness of the nanocomposites.     

Effect of pH, sulfate and sodium on the EDTA titration of calcium

The ethylenediaminetetraacetic acid (EDTA) titration method limits the measurement of calcium concentration to 50 mg/l in water. However, various acids and salt solutions are used in the investigation of the durability of concrete, and the adaptability of the EDTA titration method to determine the calcium in these solutions must be investigated. Hence, the purpose of this study was to investigate the interfering effects of hydrochloric acid, sulfuric acid, sodium chloride and sodium sulfate on measuring the calcium in the aqueous leaching solutions using the EDTA titration method. The calcium standard solutions were prepared using CaCl₂ with initial pH from −0.8 to 7 and calcium concentration up to 160 mg/l. Sulfuric acid and hydrochloric acid were used to prepare calcium solutions with lower pH. Salt solutions with 3% NaCl and 3% Na₂SO₄ were used to evaluate the interfering effects of salt elements such as sulfate and sodium on the EDTA titration. Results indicated that the EDTA titration method was reliable in measuring the calcium up to 160 mg/l, the maximum concentration investigated in this study, in hydrochloric acid with pH higher than zero and 3% sodium chloride solution. Sulfuric acid with pH higher than zero and 3% sodium sulfate solutions showed 3% to 4% less calcium in the solutions. Acid solutions with pH less than zero showed interference with calcium measurement.     

Poly(butylene terephthalate)/organoclay nanocomposites prepared by in situ interlayer polymerization and its fiber (II)

Intercalated nanocomposites with poly(butylene terephthalate) (PBT) incorporated between the montmorillonite layers were synthesized from dimethyl terephthalate and 1,4-butane diol by using an in situ interlayer polymerization. The PBT nanocomposites were melt-spun at different organoclay contents to produce monofilaments. The samples were characterized by using wide angle X-ray diffraction, electron microscopy, thermal analysis, and tensile testing. The extent of the clay layer in the PBT was confirmed by using X-ray diffraction and electron microscopy, and the clay layer was found to be highly dispersed on a nanometer scale. The addition of only a small amount of organoclay was enough to improve the thermo-mechanical properties of the PBT hybrid fibers. The hybrids were extruded with various draw ratios (DRs) to examine the tensile mechanical property of the fibers. At DR=1, the ultimate tensile strength of the hybrid fibers increased with the addition of clay up to a critical content and then decreased. However, the initial modulus monotonically increased with increasing amount of organoclay in the PBT matrix. When the DR was increased from 1 to 6, for example, the strength and the initial modulus values of the hybrids containing 3 wt% organoclay decreased linearly.     

An experimental investigation of mixing of carbon nanotube/polymer composite in a batch-type screw mixer

We develop a miniaturized batch-type screw mixer (BSM) for uniform mixing of polymer resin and nanoparticles, based on the stretching of material elements. This stretching is induced by the combination of recirculating cross-sectional flows in deep channels of the screw and high shear stress developed at flight regions. The BSM is used to produce a polymer nano-composite composed of multi-walled carbon nanotubes and polydimethylsiloxane resin. The mixing performance of the BSM is characterized quantitatively by estimating two different types of mixing efficiencies (i.e., dispersive mixing and distributive mixing) via transmitted light microscope images. The developed BSM highly improves the mixing performance rather than that of a conventional ultrasonic mixing device.     

Miscibility and Probe Tack of Acrylic Pressure Sensitive Adhesives—Acrylic Copolymer/Tackifier Resin Systems

Miscibility between acrylic copolymers and tackifier resins are investigated in terms of phase diagrams, and the probe tack of the blends are measured as a function of both temperature and rate of separation in order to obtain the master curves. It is found that the probe tack of the pressure sensitive adhesives are closely related to the miscibility between the components. The master curves of the miscible blends shift along the X(rate)-axis according to the change of T_g of the bulk materials with a gradual variation of the peak heights. However, those of the immiscible blends will not shift along the X(rate)-axis, but the magnitude will decrease with increase of a dispersed phase.     

Effects of Heat Treatment in a Wet Hydrogen Atmosphere on the Reliability of Sintered α-Silicon Carbide

Sintered α-SiC was exposed, for times up to 2 h, to a flowing wet H₂ atmosphere ( P _H2O= 1 × 10^-4 MPa) at temperatures of 1300°, 1400°, and 1500°C. The effect of such conditions on the reliability of the ceramic was estimated by comparing the Weibull modulus of the groups of specimens, tested in four-point flexure, before and after exposure. The Weibull modulus of as-polished specimens was 6.7, indicating a wide variation in room-temperature flexural strength. The Weibull modulus was increased to 14.2 by the heat treatment for 2 h in wet H₂ at 1400°C. The average strength was also improved from 347 to 446 MPa by such exposure. Heat treatment at 1300° and 1500°C also improved the reliability of the material, as indicated by increases in the Weibull modulus, but to less a degree than did exposure at 1400°C. The increases in reliability and average strength were attributed to the blunting of surface flaws by the formation of a thin SiO₂ layer on the sample surface.