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.     

蝎子毒素多肽WaTx的高效化学合成及氧化折叠研究

相比于1-羟基-7-氮杂苯并三氮唑(HOAt)、1-羟基苯并三唑(HOBt)等传统偶联试剂, 新型多肽偶联试剂2-肟氰乙酸乙酯(Oxyma)具有安全、偶联效率高、消旋率低等优势, 在多肽合成特别是微波固相合成中得到广泛应用. 但是, 不同反应温度(例如28、50和75 ℃)对N,N'-二异丙基碳二亚胺(DIC)/Oxyma的偶联效率以及对甲硫氨酸(Met)等易氧化氨基酸的影响尚有待研究. 瞬时受体电位锚蛋白1(TRPA1)通道在感受温度、听觉和炎症痛中发挥重要作用. 蝎子毒素多肽芥末受体毒素(WaTx)是一种新型、非共价结合的TRPA1特异性激动剂. 本研究利用6-氯苯并三氮唑-1,1,3,3-四甲基脲六氟磷酸酯(HCTU)/N,N'-二异丙基乙胺(DIEA)和DIC/Oxyma缩合体系, 首次探索了不同温度下线性WaTx的合成效率以及Met残基的氧化情况. 通过一次氧化折叠和两次氧化折叠策略, 实现了WaTx的体外快速复性折叠, 利用圆二色谱和钙荧光检测等技术评价WaTx的结构和活性. 本研究建立了WaTx的温和、高效合成以及复性折叠方法, 为固相多肽合成特别是手动固相合成WaTx等含有易氧化基团的二硫键构象锁定多肽提供了重要参考.     

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.     

微分干涉差共焦显微膜层微结构缺陷探测系统

多层膜极紫外光刻掩模"白板"缺陷是制约下一代光刻技术发展的瓶颈之一,为提高对掩模"白板"上的膜层微结构缺陷的分辨能力,提出了一种微分干涉差共焦显微探测系统方案。基于标量衍射理论,计算了系统横向和轴向分辨率。利用MATLAB建模仿真,在数值孔径为0.65、工作波长为405 nm时,分析比较了微分干涉差共焦显微系统、传统显微系统和共焦显微系统的分辨率。结果表明微分干涉差共焦显微系统具有230 nm的横向分辨率和25 nm轴向台阶高度差的分辨能力(对应划痕等缺陷形式)。此外,仿真和分析了实际应用中探测器尺寸、样品轴向偏移等的影响,模拟分析了膜层微结构缺陷的探测,结果表明本系统可以探测200 nm宽、10 nm高的微结构缺陷,较另外两种系统有更好的探测能力。     

热障涂层高温失效行为的正射投影-单相机三维数字图像相关实验研究

热障涂层(Thermal Barrier Coating,TBC)作为一种隔热材料,可降低发动机高温部件的表面温度,提高涡轮发动机的整体性能。涂层服役过程中,TBC陶瓷层的失效将导致高温部件中的金属基底直接暴露于恶劣的高温环境中,严重影响发动机的安全性。其高温服役环境下的力学性能研究是备受材料和力学工作者关注的问题。本文结合热障涂层高温检测的需求,实现了涂层-基底异质表面的高对比度高温散斑制作;发展了正射投影-单相机三维数字图像相关方法(正射投影-单相机3DDIC),构建了跨界面形函数,实现了涂层与基底的三维形貌及位移、应变的同时测量;基于涂层结构的高温拉伸实验结果,建立了依据涂层-基底应变方差差值的涂层失效判断方法,得到了热障涂层在室温(27℃)至1000℃的断裂极限应变。实验结果表明,正射投影-单相机3DDIC方法作为一种可靠测试方法,可以应用于涂层结构高温下的力学失效行为研究。     

基于体视显微镜的测量系统标定研究

微观三维变形测量系统在工程上有广泛的应用。本文构建了体视显微镜双相机微观图像采集与测量系统,可以实现对微小物体形貌、位移、变形的全场测量。微观三维变形的测量精度与成像系统的畸变模型存在密切的关系。本文采用了考虑多种不确定情况的畸变模型,能很好地表达体视显微镜测量系统的成像误差,并设计了点阵式标定模板和精密的平动平台,实现了基于Tsai标定的自动标定算法。实验表明,体视显微镜测量系统可以在各种放大倍数下稳定工作,标定的精度得到很大的提高,并给出了在不同放大倍数下对规则圆柱体的形貌和直径的测量结果。     

Stable isotope mass balances versus concentration differences of dissolved inorganic carbon – implications for tracing carbon turnover in reservoirs

The aim of this study was to identify sources of carbon turnover using stable isotope mass balances. For this purpose, two pre-reservoirs in the Harz Mountains (Germany) were investigated for their dissolved and particulate carbon contents (dissolved inorganic carbon (DIC), dissolved organic carbon, particulate organic carbon) together with their stable carbon isotope ratios. DIC concentration depth profiles from March 2012 had an average of 0.33 mmol L^–1. Increases in DIC concentrations later on in the year often corresponded with decreases in its carbon isotope composition (δ¹³C_DIC) with the most negative value of –18.4?‰ in September. This led to a carbon isotope mass balance with carbon isotope inputs of ?28.5?‰ from DOC and ?23.4, ?31.8 and ?30.7?‰ from algae, terrestrial and sedimentary matter, respectively. Best matches between calculated and measured DIC gains were achieved when using the isotope composition of algae. This shows that this type of organic material is most likely responsible for carbon additions to the DIC pool when its concentrations and δ¹³C_DIC values correlate negatively. The presented isotope mass balance is transferable to other surface water and groundwater systems for quantification of organic matter turnover.     

透明体的光学定量测量

综述了使用光学方法测量透明体的方法。介绍了两种常用的光学方法——相衬法和微分干涉相衬法。在 2 0世纪 80年代 ,一般认为相衬法和微分干涉相衬法只适用于定性观察而不能实现定量测量 ,主要是因为在其成像原理中的非线性因素的影响。但是对于微分干涉相衬法 ,最近国内外出现了几种定量测量的方法 ,本文对这几种方法进行了总结和比较。     

聚氨酯(PU)在力学性能测试中的摩擦效应与变形均匀性研究

作为防弹玻璃夹层材料,PU的动态力学性能一直受到学者们的关注。为准确表征其动态力学性能,本文采用ABAQUS有限元软件对不同摩擦系数下的单轴压缩试验进行数值仿真,分析试样加载端面的摩擦效应和几何尺寸对单轴压缩试验结果的影响;结合高速摄影技术(HSP)与数字图像相关技术(DIC)观测到试样在拉伸试验中的动态变形场和应变场,探讨标距段的应力均衡性;同时对PU材料在不同应变率下的单轴压缩、拉伸力学性能进行测试。结果表明:压缩试样的端面摩擦效应限制横向变形,影响了试样内部的受力分布,使得测量得到的应力值偏大;试样长径比越小,端面摩擦效应的影响越大;在单轴动态拉伸试验中,板状拉伸试样的标距段选取应当考虑两端倒角尺寸。通过测试PU的拉、压力学性能,发现材料具有显著的应变率敏感性。     

Separation of fluorinated amino acids and oligopeptides from their non-fluorinated counterparts using high-performance liquid chromatography

Chromatographic conditions for the separation of fluorinated amino acids and oligopeptides from their non-fluorinated counterparts were explored. The separation of six pairs of analytes, including both aromatic and aliphatic fluorocarbons, was investigated at various temperatures using both hydrocarbon and fluorocarbon columns and eluents. Our results show that when hydrocarbon eluents are used, fluorocarbon column provides better separation of fluorinated amino acids or oligopeptides from their non-fluorinated counterparts; when fluorocarbon eluents are used, hydrocarbon column provides better separation of fluorinated amino acids or oligopeptides from their non-fluorinated counterparts. These chromatographic behaviors reflect the fluorophilicity possessed by fluorinated amino acids and oligopeptides.