Residual stress evolution regularity in thermal barrier coatings under thermal shock loading

Residual stress evolution regularity in thermal barrier ceramic coatings (TBCs) under different cycles of thermal shock loading of 1100°C was investigated by the microscopic digital image correlation (DIC) and micro-Raman spectroscopy, respectively. The obtained results showed that, as the cycle number of the thermal shock loading increases, the evolution of the residual stress undergoes three distinct stages: a sharp increase, a gradual change, and a reduction. The extension stress near the TBC surface is fast transformed to compressive one through just one thermal cycle. After different thermal shock cycles with peak temperature of 1100°C, phase transformation in TBC does not happen, whereas the generation, development, evolution of the thermally grown oxide (TGO) layer and micro-cracks are the main reasons causing the evolution regularity of the residual stress.     

Experimental set-up for determination of the large-strain tensile behaviour of polymers at low temperatures

In this study, we present a method to determine the large-strain tensile behaviour of polymers at low temperatures using a purpose-built temperature chamber made of polycarbonate (PC). This chamber allows for several cameras during testing. In our case, two digital cameras were utilized to monitor the two perpendicular surfaces of the test sample. Subsequently, the pictures were analysed with digital image correlation (DIC) software to determine the strain field on the surface of the specimen. In addition, a thermal camera was used to monitor self-heating during loading. It is demonstrated that the PC chamber does not influence the stress-strain curve as determined by DIC. Applying this set-up, a semi-crystalline cross-linked low-density polyethylene (XLPE) under quasi-static tensile loading has been successfully analysed using DIC at four different temperatures (25 °C, 0 °C, −15 °C, −30 °C). At the lower temperatures, the conventional method of applying a spray-paint speckle failed due to embrittlement and cracking of the spray-paint speckle when the tensile specimen deformed. An alternative method was developed utilising white grease with a black powder added as contrast. The results show a strong increase in both the Young’s modulus and the flow stress for decreasing temperatures within the experimental range. We also observe that although the XLPE material is practically incompressible at room temperature, the volumetric strains reach a value of about 0.1 at the lower temperatures.     

Flow injection analysis as a tool for enhancing oceanographic nutrient measurements—A review

Macronutrient elements (C, N and P) and micronutrient elements (Fe, Co, Cu, Zn and Mn) are widely measured in their various physico-chemical forms in open ocean, shelf sea, coastal and estuarine waters. These measurements help to elucidate the biogeochemical cycling of these elements in marine waters and highlight the ecological and socio-economic importance of the oceans. Due to the dynamic nature of marine waters in terms of chemical, biological and physical processes, it is advantageous to make these measurements in situ and in this regard flow injection analysis (FIA) provides a suitable shipboard platform. This review, therefore, discusses the role of FIA in the determination of macro- and micro-nutrient elements, with an emphasis on manifold design and detection strategies for the reliable shipboard determination of specific nutrient species. The application of various FIA manifolds to oceanographic nutrient determinations is discussed, with an emphasis on sensitivity, selectivity, high throughput analysis and suitability for underway analysis and depth profiles. Strategies for enhancing sensitivity and minimizing matrix effects, e.g. refractive index (schlieren) effects and the important role of uncertainty budgets in underpinning method validation and data quality are discussed in some detail.     

A method to determine mixing enthalpies by DSC

A method has been developed that utilizes a special custom-made mixing device and HPLC micro liter syringe to perform mixing experiments of liquid systems directly in open measuring cells of differential scanning calorimeters. The present paper describes how to determine mixing enthalpies from time scans of the isothermal heat flux during an exothermal or endothermal process. Using ethylene glycol and the slightly volatile component water to calibrate the mixing calorimeter, the mixing enthalpy of the binary system poly(ethylene glycol) 400/water could be determined with sufficient precision compared to the results of measurements with a conventional flow calorimeter. This revised version was published online in July 2006 with corrections to the Cover Date.     

Biosynthesis of silver nanocrystals by Bacillus licheniformis

The use of microorganisms for the synthesis of nanoparticles is in the limelight of modern nanotechnology. Using the bacterium Bacillus licheniformis, the biosynthesis of silver nanoparticles was investigated. These silver nanoparticles were characterized by means of UV-vis spectroscopy, scanning electron microscopy (SEM), electron diffraction spectroscopy (EDX) and X-ray diffraction (XRD). The nanoparticles exhibited maximum absorbance at 440 nm in UV-vis spectroscopy. The XRD spectrum of silver nanoparticles exhibited 2theta values corresponding to the silver nanocrystal. SEM micrographs revealed the formation of well-dispersed silver nanoparticles of 50 nm, and the presence of silver was confirmed by EDX analysis.     

On-wafer thermomechanical characterization of a thin film polyimide formed by vapor deposition polymerization for through-silicon via applications: Comparison to plasma-enhanced chemical vapor deposition SiO2

Thin-film polyimides were prepared by solvent-less vapor deposition polymerization (VDP) from pyromellitic dianhydride and 4,4′-oxydianiline at 200 °C for liner dielectric formation of vertical interconnects called through-silicon vias (TSVs) used in three-dimensionally stacked integrated circuit (3DICs). FTIR, synchrotron XPS, and TDS were employed for determining the imidization ratio, and in addition, the mechanical properties, coefficient of thermal expansion and Young's modulus, of the VDP polyimide were characterized on Si wafers. The VDP polyimide exhibited extremely high conformality, beyond 75%, toward high-aspect-ratio deep Si holes, compared with conventional SiO₂ prepared by plasma-enhanced chemical vapor deposition. The adhesion between the VDP polyimide and Si wafer was enhanced by an Al-chelate promotor. Remarkably, the VDP polyimide TSV liner dielectrics showed much less thermomechanical stresses applied to the Si surrounding the TSVs than the plasma-chemical vapor deposition SiO₂. The small keep-out zone is expected for scaling down highly reliable 3DICs for the upcoming real artificial intelligence society.     

Segment Coupling to a Highly Hindered N-Terminal, Alamethicin-Related alpha-Aminoisobutyric Acid (Aib) Residue

A model [6+5] segment coupling process involving a C-terminal valine hexapeptide acid and a resin-attached pentapeptide amide, which N-terminated in a hindered Aib unit, was examined using a variety of HOAt-derived coupling reagents. Best results were observed with N-HAPyU in DCM solvent in which loss of configuration amounted to 5.8%.     

Microwave-assisted guanidinylation in solid phase peptide synthesis: comparison of various reagents

The guanidinylation of a peptide chain on a polymeric support under microwave conditions using derivatives of thioureas—S-alkylisothioureas, pyrazole-carboxamidine, and guanidine as guanidinylating reagents is described. The best results are obtained with N,N′-di-Z-S-methylisothiourea and N,N′-di-Z(2-Cl)-S-methylisothiourea. It is found that guanidinylation with reagents containing Boc groups is accompanied by side reactions.     

碱金属团簇碰撞动力学研究

采用距离相关紧密束缚的分子动力学模型 ,研究了钠原子团簇的碰撞动力学行为 .研究得出 ,对Na6(3D) +Na8系统 ,碰撞参数为b =9a0 时 ,对应于深度非弹性碰撞过程 (DIC) ,在b =13a0 时 ,则对应于准弹性碰撞过程 .另外 ,得到碰撞过程中存在转动 ,其能量大小与碰撞能量Eproj/n以及碰撞参数b均有关系 .随着Eproj/n的增大 ,相对转动减小 ;随着b的变化 ,转动能量先增大后减小 .在b =7a0 时转动最大 ,最大转动能量可达总能量的十分之一 .     

Model‐based quantification of the volatility of options at transaction level with extended count regression models

In this paper, we elaborate how Poisson regression models of different complexity can be used in order to model absolute transaction price changes of an exchange‐traded security. When combined with an adequate autoregressive conditional duration model, our modelling approach can be used to construct a complete modelling framework for a security's absolute returns at transaction level, and thus for a model‐based quantification of intraday volatility and risk. We apply our approach to absolute price changes of an option on the XETRA DAX index based on quote‐by‐quote data from the EUREX exchange and find that within our Bayesian framework a Poisson generalized linear model (GLM) with a latent AR(1) process in the mean is the best model for our data according to the deviance information criterion (DIC). While, according to our modelling results, the price development of the underlying, the intrinsic value of the option at the time of the trade, the number of new quotations between two price changes, the time between two price changes and the Bid–Ask spread have significant effects on the size of the price changes, this is not the case for the remaining time to maturity of the option. Copyright © 2006 John Wiley & Sons, Ltd.