赶酸对微波消解-氢化物发生-原子荧光法测定谷物中砷元素的影响

在利用氢化物发生-原子荧光分测定谷物类样品中砷元素时,硫脲-抗坏血酸的还原效果会受到硝酸含量的影响,试液中硝酸含量过高,会与硫脲-抗坏血酸溶液发生氧化还原反应,降低其还原效率。本研究通过对赶酸时间和赶酸温度进行试验,获得最佳的赶酸条件,结合微波消解技术,利用氢化物发生-原子荧光光谱法测定谷物中的微量砷,结果表明,谷物中砷浓度与荧光强度呈线性关系,线性方程为 y=0.0028x-0.1728,线性相关系数R2=0.9993,检出限为1.72ng/g。 通过对9份样品进行检测,其相对标准偏差RSD在4.32-7.59%之间,其准确度相对误差RE均小于±6.50%。经多次检测证实该方法较稳定,可用于谷物类样品中砷元素的快速测定。     

Multiple time step molecular dynamics simulation for interaction between dislocations and grain boundaries

A multiple time step algorithm, called reversible reference system propagator algorithm, is introduced for the long time molecular dynamics simulation. In contrast to the conventional algorithms, the multiple time method has better convergence, stability and efficiency. The method is validated by simulating free relaxation and the hypervelocity impact of nano-clusters. The time efficiency of the multiple time step method enables us to investigate the long time interaction between lattice dislocations and low-angle grain boundaries.The project supported by the National Natural Science Foundation of China (the 973 Project 2004CB619304).     

Grain fragmentation in ultrasonic-assisted TIG weld of pure aluminum

Under the action of acoustic waves during an ultrasonic-assisted tungsten inert gas (TIG) welding process, a grain of a TIG weld of aluminum alloy is refined by nucleation and grain fragmentation. Herein, effects of ultrasound on grain fragmentation in the TIG weld of aluminum alloy are investigated via systematic welding experiments of pure aluminum. First, experiments involving continuous and fixed-position welding are performed, which demonstrate that ultrasound can break the grain of the TIG weld of pure aluminum. The microstructural characteristics of an ultrasonic-assisted TIG weld fabricated by fixed-position welding are analyzed. The microstructure is found to transform from plane crystal, columnar crystal, and uniform equiaxed crystal into plane crystal, deformed columnar crystal, and nonuniform equiaxed crystal after application of ultrasound. Second, factors influencing ultrasonic grain fragmentation are investigated. The ultrasonic amplitude and welding current are found to have a considerable effect on grain fragmentation. The degree of fragmentation first increases and then decreases with an increase in ultrasonic amplitude, and it increases with an increase in welding current. Measurement results of the vibration of the weld pool show that the degree of grain fragmentation is related to the intensity of acoustic nonlinearity in the weld pool. The greater the intensity of acoustic nonlinearity, the greater is the degree of grain fragmentation. Finally, the mechanism of ultrasonic grain fragmentation in the TIG weld of pure aluminum is discussed. A finite element simulation is used to simulate the acoustic pressure and flow in the weld pool. The acoustic pressure in the weld pool exceeds the cavitation threshold, and cavitation bubbles are generated. The flow velocity in the weld pool does not change noticeably after application of ultrasound. It is concluded that the high-pressure conditions induced during the occurrence of cavitation, lead to grain fragmentation in a pure aluminum TIG weld during an ultrasonic-assisted TIG welding process.     

复层籽晶制备单晶畴YBCO超导块材

本文介绍了沿c轴方向排布复层籽晶制备YBCO超导单畴的方法.该方法能够使123晶畴在不同深度进行生长.通过c轴方向籽晶的排布,研究了YBCO单畴中的(001)/(001)晶界.虽然由于压模中籽晶ab面的倾斜,造成部分(001)/(001)晶界出现大角晶界,使晶界上残余有液相,但仍有晶界连接良好、晶界上不存在残余液相和211粒子、错配角小于5°的(001)/(001)晶界的形成.对于制备有深度要求的单畴块材,复层籽晶法是一种有效的生长方法.在定向控制好籽晶方向的条件下,该方法可以提高超导单畴的生长深度.在77K,0.5T下,测试该样品磁悬浮力达到37N.     

A possible role of amorphous regions at grain-boundary vertex points as linear defects on flux pinning in MgB2 films with columnar grain structure

We measured the transport properties of MgB₂ films having columnar grain structure with their axis normal to the substrate. When an external magnetic field was applied parallel to the grain axis, an enhanced critical current density has been observed, and this result has been ascribed to flux pinning induced by grain boundaries. The shape of the angular dependence of critical current density and its magnetic field dependence showed a quite similar resemblance to those of YBa₂Cu₃O_x films containing columnar defects, implying a possible existence of linear defects in MgB₂ films of columnar structure. We propose that the amorphous regions at the vertex points of three or more grain boundaries observed in microstructural studies correspond to the linear defects and these linear defects anchor the end points of the flux line dislocations of Frank-Read sources, by which the shear in the flux line lattice is actuated. This assumed mechanism is found to reasonably explain the magnetic field dependence of the flux pinning force density of MgB₂ films with columnar grain structure.     

(Ce0.9Nd0.1)1-xMoxO2-δ (0.00≤x≤0.10)的合成、表征与电性能

采用溶胶-凝胶法合成(Ce0.9Nd0.1)1-xMoxO2-δ(x=0.00、0.02、0.05、0.10)氧化物, 通过X射线衍射(XRD)、场发射扫描电镜(FESEM)等手段对氧化物进行结构表征, 交流阻抗谱测试电性能. 结果表明: 所有样品均为单一萤石立方结构; 少量MoO3的加入提高了材料的致密性, 降低了材料的总电阻、晶界电阻和晶界电阻在总电阻中所占比例, 提高了材料的电导率. 1200 ℃烧结样品24 h, 测试温度700 ℃时, (Ce0.9Nd0.1)1-xMoxO2-δ(x=0.00)总电导率和晶界电导率分别为0.05和0.19 S·m-1, 掺Mo材料(Ce0.9Nd0.1)1-xMoxO2-δ(x=0.02)的总电导率和晶界电导率分别为2.42 和3.96 S·m-1.     

Adsorption at the air-water interface and emulsification properties of grain legume protein derivatives from pea and broad bean

Functional properties of native and modified (through induced autolysis) pea (Pisum sativum L.) and broad bean (Vicia faba L.) protein derivatives are studied. In specific, protein solubility and behavior at the air–water interface through surface pressure measurements are investigated. Furthermore the ability of the protein products to act as emulsifying agents and to stabilize emulsions is studied through oil droplet size distribution measurements and by the protein adsorbed at the oil–water interface. The data reveal that the ability of the proteins to act as surfactants and build up a rigid film around the oil droplets, mainly depends on their suitable molecular configuration and structure. Hydrolysis did not promote the functionality of the legume proteins. Broad bean exhibited better functionality than pea, before and after hydrolysis. Some comparisons were also made with lupin (Lupinus albus L.) protein isolate.     

Formation of crystalline TiO2−xNx and its photocatalytic activity

Amorphous precursors to nitrogen-doped TiO₂ (NTP) and pure TiO₂ (ATP) powders were synthesized by hydrolytic synthesis and sol-gel method (SGM), respectively. Corresponding crystalline phases were obtained by thermally induced transformation of these amorphous powders. From FT-IR and XPS data, it was concluded that a complex containing titanium and ammonia was formed in the precipitate stage while calcination drove weakly adsorbed ammonium species off the surface, decomposed ammonia bound on surface of precipitated powder and led to substitution of nitrogen atom into the lattice of TiO₂ during the crystallization. The activation energies required for grain growth in amorphous TiO_2−xN_x and TiO₂ samples were determined to be 1.6 and 1.7 kJ/mol, respectively. Those required for the phase transformation from amorphous to crystalline TiO_2−xN_x and TiO₂ were determined to be 129 and 142 kJ/mol, respectively. A relatively low temperature was required for the phase transformation in NTP sample than in ATP sample. The fabricated N-doped TiO₂ photocatalyst absorbed the visible light showing two absorption edges; one in UV range due to titanium oxide as the main edge and the other due to nitrogen doping as a small shoulder. TiO_2−xN_x photocatalyst demonstrated its photoactivity for photocurrent generation and decomposition of 2-propanol (IPA) under visible light irradiation ().     

Segregation of H, C and B to Σ = 5 (0 1 3) α-Fe grain boundary: A theoretical study

The ASED-MO theory is used to study the effects of H and the HC and HB pairs in the electronic structure of a Fe grain boundary (GB). The results obtained for H in a GB model are consistent with its behavior as a chemical embrittler. The total energies calculated for FeH, FeC and FeB clusters indicate that all interstitials segregate to the GB. C has the lowest energy, followed by B, and could compete with other impurities for the site location on the GB.The results obtained for FeCH and FeBH are consistent with the observed behavior of C and B as cohesion enhancers. A strong repulsive interaction between C and H and B and H atoms is developed if they occupy the nearest interstitial site on the GB. When C or B are present, the total energies are similar to that obtained for the FeH cluster. This indicates that H is displaced from the capped trigonal prism (CTP). Also, we do not detect any CH or BH interaction.Density of states (DOS) and crystal orbital overlap population (COOP) curves are used to shed more light on the interstitial-Fe GB interaction. The existence of strong metal-metalloid bonds is shown, which are primarily due to Fe 3d, 4s and C (or B) 2s, 2p interactions.     

含He纳米钛膜的XRD研究

本文采用直流磁控溅射方法,在He／Ar混合气氛中,通过分别改变He／Ar流量比和沉积偏压制备不同He含量的钛膜。利用XRD(X-ray diffraction)对含He钛膜的微观结构和晶粒尺寸进行了研究。结果表明,在其它实验参数不变的情况下,当He／Ar流量比从1.0增加到25时,钛膜的平均晶粒尺寸从19.02nm减小到8.63nm。随着膜中He含量的增加,衍射峰宽化,晶粒细化,He的掺入有抑制纳米晶粒长大的趋势。而当沉积偏压从24V增加到151V时,其平均晶粒尺寸基本不变。He引入引起了（002）晶面衍射峰向小角度移动,晶格参数c增加,而a不变。