W掺杂对Nb固溶体抗氢脆及透氢性能的改性研究

元素掺杂是消除Nb金属氢脆问题的有效方法。本文制备了W掺杂的Nb100-xWx (x=2,5,8,10,16)合金，采用XRD、SEM、Sieverts 气体吸附技术、电化学方法和三点弯曲试验研究了掺杂量对合金结构、氢化物形成焓、氢扩散系数和抗氢脆机械力学性能的影响。研究证实，熔炼制备Nb100-xWx为Nb-bcc结构的固溶体合金，W掺杂引起晶体结构畸变收缩，其畸变行为随掺杂量增大更为明显。Nb基固溶体在匀晶转变时存在非平衡转变，形成富W和贫W区相间分散的枝状结晶形貌。随W掺杂量增大，其枝状结构趋于更加细化和致密、分界明显。W掺杂引起合金的氢化物形成焓增大、有利于H原子的释放，Nb84W16合金样品具有最大的氢扩散系数（1.66×10-9 cm2·s-1），约是Nb98W2合金的1.8倍。W掺杂提高Nb100-xWx固溶体合金的抗氢脆性能，Nb84W16合金膜有最大的临界载荷值（78.4N）和最大位移量（0.83mm），分别是Nb98W2合金膜的1.9倍和1.8倍，力学性能的改善与其枝状结晶结构有关。     

全自动固相萃取-气相色谱/质谱法测定水中的甲萘威

[目的]建立了全自动固相萃取-气相色谱/质谱联用测定水体中甲萘威的方法。[方法]优化了固相萃取的条件,采用ProElut PLS固相萃取柱,以甲醇作为洗脱溶剂萃取水样中的甲萘威,用气相色谱/质谱法测定。[结果]甲萘威质量浓度在5.0~250.0μg/L范围内与其气相色谱/质谱响应值线性关系良好,相关系数为0.9999,检出限为0.022μg/L。样品加标回收率在90.2%~92.5%之间,测定结果的相对标准偏差为1.9%~3.2%。[结论]该方法自动化程度高、快速、准确,适合于水中甲萘威的测定。     

基于聚集诱导发光效应的高固低黏丙烯酸荧光树脂的制备及其性能研究

为了研制一种具有荧光功能特性的高固低黏羟基丙烯酸树脂。从聚集诱导发光效应（AIE）出发，将具有 AIE性质的二对丙烯酸四苯乙烯酯荧光分子通过自由基共聚连接于聚合物链段。由于聚合物链段对荧光分子化学键固定以及聚合物链的包裹束缚作用，导致荧光分子运动受限，从而实现涂层在紫外灯下荧光发光。通过荧光光谱的实时跟踪，探索高固低黏羟基丙烯酸树脂的合成以及固化规律。此外，由于聚合物链段对外界刺激具有实时响应性，从而间接影响了所连接的荧光分子的荧光发光行为。因此，文中也探索了涂层在外界温度与化学气体的影响下所发生的荧光变化的规律，以探索其在功能涂层中应用的可行性。     

基于稳定固溶体团簇模型的无扩散阻挡Cu合金薄膜的成分设计

随着超大规模集成电路的发展,器件特征尺寸不断缩小,必然会出现Cu互连扩散阻挡层厚度无法进一步减小等瓶颈问题。因此,开发新型无扩散阻挡层Cu合金薄膜(Cu种籽层)势在必行。该新型互连结构在长时间的中高温(400~500℃)后续工艺实施过程中,需同时具备高的稳定性(不发生互扩散反应)和低的电阻率。基于此,首先综述了目前无扩散阻挡层结构的研究现状及问题,然后对基于稳定固溶体团簇模型设计制备的无扩散阻挡Cu-Ni-M薄膜的研究工作进行了梳理,通过多系列薄膜微观结构、电阻率及稳定性的对比,深入探讨了第三组元M的选择原则及其对薄膜热稳定性的影响。为进一步验证稳定固溶体团簇模型的有效性,对第二组元的变化进行了相关讨论。结果证实,选取原子半径略大于Cu、难扩散且难溶的元素作为第三组元M,薄膜表现出良好的扩散阻挡能力;当M/Ni=1/12,即合金元素完全以团簇形式固溶于Cu基体时,薄膜综合性能达到最优,能够满足微电子行业的要求。所有研究表明,稳定固溶体团簇模型在无扩散阻挡层Cu合金薄膜的成分设计方面十分有效,该模型也有望在耐高温Cu合金及抗辐照材料成分设计方面推广使用。     

Phase equilibria studies in the CaO–SiO2–Al2O3–MgO system with CaO/SiO2 ratio of 0.9

Phase equilibria and liquidus temperatures in the CaO–SiO₂–Al₂O₃–MgO system at a CaO/SiO₂ weight ratio of 0.9 in the liquid phase have been experimentally determined employing high-temperature equilibration and quenching technique followed by electron probe X-ray microanalysis. Isotherms at 1573, 1623, 1673, and 1773 K were determined and the primary phase fields of wollastonite, melilite, olivine, periclase, spinel, and corundum have been located. Compositions of the olivine and melilite solid solutions were analyzed and discussed. Comparisons between the newly constructed diagram, existing data, and FactSage predicted phase diagrams were performed and differences were discussed. The present study will be useful for guidance of industrial practices and further development of thermodynamic modeling.     

NiCrAlFe精密电阻合金中的L12有序结构研究

有序结构的形成是决定NiCrAlFe精密电阻合金电学性能的关键因素。本文利用第一性原理赝势平面波方法，计算了合金处于无序固溶体结构和形成L12型有序结构时的结合能、态密度、晶格常数等参数，并利用高分辨透射电子显微镜（HRTEM）对合金进行了结构表征，还测试了固溶态和时效态的电阻率。从结合能来看，该合金形成L12有序结构时比无序固溶体更加稳定；态密度以及部分态密度计算结果则表明，在L12有序结构中，Ni、Cr、Al、Fe会强烈成键而使得整个合金体系变得稳定；HRTEM分析结果证明固溶态合金经过和时效处理后出现了L12有序结构，而且该有序结构的晶格常数与计算值基本一致。对比无序固溶体与L12型有序结构费米能级处的态密度值发现，当形成L12有序结构时合金的导电能力较无序固溶体下降，电阻率升高，与实际测试结果吻合。     

Effect of interface morphology on the residual stress distribution in solid oxide fuel cell

Solid oxide fuel cell directly and efficiently converts chemical energy to electrical energy. However, the necessity for high operating temperatures can result in mechanical failure. Fuel cell is a multilayer system and its stress distribution is greatly affected by the interface morphology. In this work, cosine interfaces with different amplitudes are used to approximate the fluctuation of actual interface. The effects of interface morphology on stress state, energy release rate of crack and creep behavior have been investigated. The results show that if the interface is planar, the residual normal stress component is zero on the interface, while the nonplanarity of interface can cause the normal stress S_n and shear stress S_t on the interface. When the amplitude is relatively small, the max values of S_n and S_t on the interfaces vary linearly with increasing amplitudes in both anode and cathode. Above a certain value, nonlinearity of the interface becomes important. Max tensile S_n always occurs at the peak of convex interface, but the position of max compressive S_n varies. Max shear stress is prone to occur at 1/4 of the wavelength at small amplitude and moves towards 1/2 of the wavelength when the amplitude increases. Fracture mechanics analysis shows that the surface crack possibly penetrates into the anode function layer and then is constrained by the stiff electrolyte. On the other hand, the horizontal crack likely penetrates into the electrolyte layer when the interface is not planar. Creep analysis shows that 11 800 hours of continuous operation at high temperature cannot remove stress undulation introduced by nor-planar interface but can make max value of Sn and St decrease around 30%.     

Phase diagram of the Li2SO4–Na2SO4 system

The thermal analysis and X-ray powder diffraction studies of the Li₂SO₄–Na₂SO₄ system, including the high-temperature X-ray diffraction technique, have elucidated four phases of variable composition: three solid solutions based on the α-Li₂SO₄, α-Na₂SO₄, and α-LiNaSO₄ high-temperature polymorphs, and a low-temperature β-LiNaSO₄ phase. α-Na₂SO₄-Base solid solution disintegrates into two phases via a monotectoid phase transformation. It is quite probable that the monotectoid process is related to the conversion of the second-order phase transition to the first-order phase transition.     

Synthesis of “walnut-like” BiOCl/Br solid solution photocatalyst by electrostatic self-assembly method

In this paper, under the control strategy of surface charge of BiOCl photocatalyst and the electrostatic adsorption of anions and cations in potassium bromide (KBr) and polyvinylpyrrolidone (PVP), the self-assembly of “walnut-like” BiOCl/Br solid solution nanophotocatalyst at a lower temperature water bath was proposed for the first time. X-ray diffraction (XRD), Raman, scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), energy-dispersive system (EDS), X-ray photoelectron spectroscopy (XPS), Brunauer-Emmett-Teller (BET), UV-Vis, photoluminescence spectroscopy (PL) and Mott-Schottky curve, transient photocurrent densities, and electrochemical impedance spectroscopy (EIS) were used to analyze the properties of materials, including its morphology, element distribution and chemical states, specific surface area, electrochemical property, and photogenic charge transfer. Based on the degradation performance of RhB dye wastewater and phenol in visible and ultraviolet light, and the band structure of BiOCl/Br solid solution, the reason for the improved photocatalytic activity was deeply discussed, and the possible degradation mechanism was also put forward. The above results show that Br⁻ can be inserted into the crystal lattice of BiOCl under the effect of electrostatic adsorption to form solid solution by the interaction between atomic orbitals, which not only reduces the bandgap width but also improves the separation and mobility of photogenic electrons and holes, causing the absorbed light to shift red to the visible region. In addition, when the n_Br⁻/n_Cl⁻ = 0.67, “walnut-like” BiOCl/Br solid solution was formed, and this kind of special core-shell structure not only can increase the specific surface area, increase the number of active sites, but also can make the light reflect and refract many times in the cavity and further increase the utilization rate of light energy, and then the best photocatalytic activity was achieved. This study provides an new method to enhance the photocatalytic performance of BiOCl and be conducive to the development of modern material science.     

Design and fabrication of novel interconnectors for solid oxide fuel cells via rubber pad forming

Rubber pad forming is studied numerically and experimentally to fabricate interconnectors for solid oxide fuel cells (SOFCs) from thin Crofer sheets instead of classical thick ones with machined flow channels. In the theoretical program, the effects of the rib angle, rib width and channel depth on the formability are numerically investigated and optimized as 120°, 0.5 mm and 0.5 mm, respectively. In addition, flow simulations are performed to analyze the flow uniformity in the flow-field for the final geometry and homogenous reactant distributions are observed. In the experimental program, the interconnector with numerically optimized geometry is successfully manufactured by rubber pad forming, trimming, piercing and spot welding processes. This interconnector is used to build a two-cell stack. A similar stack is also constructed with a conventional interconnector for comparison. The performances of these stacks are measured at different operating temperatures. According to the simulation and experimental results, rubber pad forming is found to be a highly effective manufacturing route to fabricate SOFC interconnectors from thin Crofer sheets, providing higher specific and volumetric power density values for SOFC stacks compared to those of conventional stacks with interconnectors having machined flow channels.