（S）-噻吗洛尔半水合物的合成及表征

为了开发β受体阻断剂新药（S）-噻吗洛尔半水合物，采用3-吗啉-4-氯-1，2，5-噻二唑为起始原料，经水解反应得到中间体1（3-吗啉-4-羟基-1，2，5-噻二唑）。中间体1与R-环氧氯丙烷发生醚化反应，经后处理及重结晶得到中间体2 {（R）-4-［4-（环氧乙烷-2-基甲氧基）-1，2，5-噻二唑-3-基］吗啉}。中间体2经胺化反应、马来酸成盐及重结晶得到（S）-马来酸噻吗洛尔。（S）-马来酸噻吗洛尔经游离、纯水转晶得到符合药典标准的（S）-噻吗洛尔半水合物，总收率14.05%且e.e.值为99.66%。最终成品经IR、1H-NMR、13C-NMR、MS、TGA、DSC表征，并优化各步反应条件。结果表明:以三乙胺为醚化反应缚酸剂75 ℃反应最佳；以乙醇为胺化反应溶剂46 ℃反应16 h最佳；S-噻吗洛尔的转晶拆分以水作溶剂，比传统不对称合成工艺安全稳定，操作简单，适合工业化生产。     

Investigations on grinding process of woven ceramic matrix composite based on reinforced fiber orientations

Fiber orientations play the decisive role in grinding process of woven ceramic matrix composites, but the influence of woven fibers in grinding process is not clear. This paper studies the surface quality and grinding force by comparing different woven surfaces. Through a series of experiments in optimized sampling conditions, we analyze characteristics of the material surface topography height, wave distribution and surface support properties in details. And we find some outstanding characteristics of the surface microstructure. We also study the influence of grinding processing parameters on surface microstructure. The results show that machining surface which contains more parallel fibers is rougher and more keenness than gauss surface. Grinding wheel speed and depth of cut have great influence on surface topography and surface support properties. And it is discovered that grinding forces are also highly dependent on fiber orientations. The mechanism of the grinding phenomena is also analyzed in this paper according to knowledge of fracture mechanics and mechanical damage phenomenology. The research obtained will be an important technical support on improving the processing quality of woven ceramic matrix composites.     

New nanocomposite based on poly(lactic-co-glycolic acid) copolymer and magnetite. Synthesis and characterization

The study presents the preparation of the new magnetic nanocomposite based on PLGA and magnetite. The PLGA used to obtain the magnetic nanocomposites was synthesized by the copolymerization of lactic acid with glycolic acid, in the presence of tin octanoate [Sn(Oct)₂] as catalyst, by polycondensation procedure. Magnetite was obtained by co-precipitation from aqueous salt solutions FeCl₂/FeCl₃. The particles size of magnetite was 420 nm, and the saturation magnetization 62.78 emu/g, while the PLGA/magnetite nanocomposite size was 864 nm and the saturation magnetization 39.44 emu/g. The magnetic nanocomposites were characterized by FT-IR, DLS technique, SEM, VSM and simultaneous thermal analyses (TG–FTIR–MS). The polymer matrix PLGA acts as a shell and carrier for the active component, while magnetite is the component which makes targeting possible by external magnetic field manipulation. Based on the gases resulted by thermal degradation of PLGA copolymer, using the simultaneous analysis TG–FTIR–MS, a possible degradation mechanism was proposed.     

Characteristics and formation mechanism of porosities in CFRP during laser joining of CFRP and steel

An experimental investigation on the mechanism of porosity formation during the laser joining of carbon fiber reinforced polymer (CFRP) and steel is presented. The porosity morphology and distribution were characterized by optical and scanning electron microscopy, and the thermal pyrolysis behaviors were investigated by thermal analysis and designed back-side cooling experiments. The results show that there are two types of porosities in CFRP. Porosity I only appears when the heat input is more than 77.8 J/mm. It has a smooth inner wall and distributes near the bonding interface between CFRP and steel at the central area of melted zone, which is caused by gaseous products such as CO₂, NH₃, H₂O, and hydrocarbons produced by the pyrolysis of CFRP. Porosity II can be seen under all joining conditions. It has a rough inner wall and distributes far away from the bonding interface, concentrating at the final solidification locations. Porosity II is caused by the shrinkage of melted CFRP during solidification stage.     

Design of functionalized α-Fe2O3 (III) films with long-term anti-wetting properties

The design of functional anti-wetting ceramic coatings is always a bottleneck restricting the development of ceramic techniques. This study proposes a liquid phase synthesis method to fabricate α-Fe₂O₃ (III) ceramic powders with promising applications and introduces a facile electrophoretic deposition (EPD) technique to construct the corresponding functionalized hydrophobic films – superhydrophobic functionalized α-Fe₂O₃ ceramic films (SFOFS) with roughly even distribution and a high water contact angle (CA) of 169°±1° – followed by heat posttreatments. The microtopography and crystalline structures of the product were investigated by FESEM, EDX, and XRD techniques. The EPD controllability of SFOFS was studied by adjusting the EPD time and the applied field strengths. In addition, the SFOFS show excellent long-term anti-wetting properties for twenty-four months after undergoing a series of tests, including soaking, water droplet impacting, immersion by droplets with different surface tensions and exposure to different gases and relative humidity conditions, etc. This study substantially helps the design of other kinds of functional anti-wetting films through the proposed convenient method beyond the oxide limit.     

Crack initiation and propagation in braided SiC/SiC composite tubes: Effect of braiding angle

Crack initiation and propagation in three braided SiC/SiC composite tubes with different braiding angles are investigated by in situ tensile tests with synchrotron micro-computed tomography. Crack networks are precisely detected after an image subtraction procedure based on Digital Volume Correlation. FFT based simulations are performed on the full-resolution 3D images to assess elastic stress/strain fields. Quantitative measurements of the crack geometries are performed using a novel method based on grey levels. The results show that braiding angle has no obvious effect on the location of crack onsets (initiation always occurs at tow interfaces), whereas it significantly affects the paths of crack propagation. This work provides an explicit demonstration of the crack propagation scenarios with respect to the mesoscopic fibre architectures.     

Simultaneous synthesis of a heat exchanger network with multiple utilities using utility substages

Heat exchanger network synthesis (HENS) has progressed by using mathematical programming-based simultaneous methodology. Although various considerations such as non-isothermal mixing and bypass streams are applied to consider real world alternatives in modeling phase, many challenges are faced because of its properties within non-convex mixed-integer nonlinear programming (MINLP). We propose a modified superstructure, which contains a utility substage for use in considering multiple utilities in a simultaneous MINLP model. To improve model size and convergence, fixed utility locations according to temperature and series connections between utilities are suggested. The numbers of constraints, discrete, and continuous variables show that overall model size decreases compared with previous research. Thus, it is possible to expand the feasible search area for reaching the nearest global solution. The model's effectiveness and applications are exemplified by several literature problems, where it is used to deduce a network superior to that of any other reported methodology.     

Mechanical damage characterization of glass fiber-reinforced polymer laminates by ultrasonic maps

A method for simultaneous measurement of the thickness and density for Glass Fiber-Reinforced Polymer (GFRP) laminate plates with ultrasonic waves in C-Scan mode is presented in the form of maps. The method uses three different signals in immersion pulse-echo C-Scan mode. The maps obtained based on the density show the heterogeneity of the material at high resolution at the pixel level (1 × 1 mm²) and therefore they represent an efficient tool to assess and evaluate the damage of the composite structures after manufacturing and after an applied mechanical loading.     

Influence of ZrB2 hard ceramic reinforcement on mechanical and wear properties of aluminum

In this work, the effect of ZrB₂ (0, 5, 10 and 20?vol%) ceramic reinforcement on densification, structure, and properties of mechanically alloyed Al was investigated. The milling of Al-ZrB₂ powder compositions resulted in formation of agglomerates with varied size. In particular, the size of agglomerates was reduced considerably with increased addition of ZrB₂ to Al. Interestingly, the densification of hot pressed Al increased from 96.06% to 99.22% with ZrB₂ addition. The reduction of agglomerates size was attributed to the enhanced densification of Al-ZrB₂ composites. Pure Al showed relatively low hardness (0.94?GPa) and it was improved to 1.78?GPa with the addition of 20?vol% ZrB₂. The mechanical properties have significantly been improved for Al-ZrB₂ composites. Especially Al - 20?vol% ZrB₂ possessed a very high yield strength (529?MPa), compressive strength (630?MPa) and compressive strain of 19.25%. Realization of such a good combination of mechanical properties is the highest ever reported for Al composites so far in the literature. The coefficient of friction (COF) of Al-ZrB₂ varied narrowly between 0.33 and 0.40 after dry sliding wear against steel disc. The wear rate of Al-ZrB₂ composites was within mild wear regime and varied between 98.88?×?10^?6 and 34.66?×?10^?6 mm³/Nm. Among all the compositions, Al - 20?vol% ZrB₂ composite exhibited the lowest wear rate and high wear rate was noted for pure Al. Mild abrasion, tribo-oxidation, third body wear (wear debris) and delamination were the major material removal mechanisms for Al-ZrB₂ composites. Overall the hardness, strength and wear resistance of Al - 20?vol% ZrB₂ composite was improved by 84.3%, 84.3% and 64.2%, respectively when compared to pure Al.     

Core–shell NTC materials with low thermal constant and high resistivity for wide-temperature thermistor ceramics

Core–shell structures have been proposed to improve the electrical properties of negative-temperature coefficient (NTC) thermistor ceramics. In this work, Al₂O₃-modified Co_1.5Mn_1.2Ni_0.3O₄ NTC thermistor ceramics with adjustable electrical properties were prepared through citrate-chelation followed by conventional sintering. Co_1.5Mn_1.2Ni_0.3O₄ powder was coated with a thin Al₂O₃ shell layer to form a core–shell structure. Resistivity (ρ) increased rapidly with increasing thickness of the Al₂O₃ layer, and the thermal constant (B) varied moderately between 3706 and 3846 K. In particular, Co_1.5Mn_1.2Ni_0.3O₄@Al₂O₃ ceramic with 0.08 wt% Al₂O₃ showed the increase of ρ double, and the change in its B was less than 140 K. The Co_1.5Mn_1.2Ni_0.3O₄@Al₂O₃ NTC ceramics showed high stability, and their grain size was relatively uniform due to the protection offered by the shell. The aging coefficient of the ceramic was less than 0.2% after aging for 500 hours at 125°C. Taken together, the results indicate that as-prepared Co_1.5Mn_1.2Ni_0.3O₄@Al₂O₃ NTC ceramics with a core–shell structure may be promising candidates for application as wide-temperature NTC thermistor ceramics.