工艺参数对动态流量控制法挤压弯管应力的影响

采用有限元模拟和实验研究了挤压钛合金弯曲管件。通过实验验证了工件的形状和尺寸精度,并通过有限元模拟分析了工艺参数对挤出过程中变形体的平均压应力分布情况和挤出弯管件的曲率半径的影响规律。结果表明:有限元模拟中,弯管件的曲率半径误差为6.03%,弯管直径误差为3.82%;在靠近定径带处,平均压应力呈非均匀分布;在焊合腔内,靠近细分流孔区域的平均压应力小于靠近粗分流孔区域的平均压应力,平均压应力的大小顺序在通过粗、细分流孔前后相反;在模具结构固定不变时,弯管件的曲率半径随挤压速度的减小而增大,不随挤压温度的变化而变化。     

Influence of Se and Te substitutions at Tl-site of Tl(Ba,Sr)CaCu2O7 superconductor on the AC susceptibility and electrical properties

The Sr and Ba bearing Tl-1212 phase, Tl(Ba,Sr)CaCu₂O₇ is an interesting superconductor. The Sr only bearing TlSr₂CaCu₂O₇ is not easily prepared in the superconducting form. The Ba only bearing TlBa₂CaCu₂O₇ on the other hand does not show improvement in the transition temperature with elemental substitution. In this work the influence of multivalent Se (non-metal) and Te (metalloid) substitutions at the Tl-site of Tl_1-xM_x(Ba,Sr)CaCu₂O₇ (M = Se or Te) superconductors for x = 0–0.6 was studied. The samples were prepared via the conventional solid-state reaction method. XRD patterns showed a single Tl-1212 phase for x = 0 and 0.1 Se substituted samples. The critical current density at the peak temperature, T_p of the imaginary (χ”) part of the AC susceptibility (χ = χ’ +χ”), J_c-inter(T_p) for all samples was between 15 and 21 A cm⁻². The highest superconducting transition temperature was shown by the x = 0.3 Se-substituted sample (T_c-onset = 104 K, T_c-zero = 89 K, T_cχ’ = 104 K and T_p = 80 K). Te suppressed the superconductivity of Tl-1212 phase. The order of highest transition temperatures are as follows: Tl_1-xTe_x(Ba,Sr)CaCu₂O₇<Tl(Ba,Sr)CaCu₂O₇<Tl_1-xSe_x(Ba,Sr)CaCu₂O₇. This work showed that Se was better than Te in improving the transition temperature and flux pinning of the Tl-1212 phase. The roles of ionic radius of Se and Te on the superconductivity of Tl(Ba,Sr)CaCu₂O₇ are discussed in this paper.     

自重湿陷性黄土地基预钻孔浸水处理的可靠度设计方法

为解决传统预浸水法存在的浸水时间长、浸水处理范围难以确定等不足,基于土体中水分运移规律,依据可靠度理论、极限状态设计方法及复合 Poisson 过程原理,提出一种消除黄土湿陷性的处理浸水方法——预钻孔浸水法。给出了利用预钻孔浸水法对自重湿陷性黄土地基进行浸水时,水平向及竖直向浸水影响范围的确定模型;在此基础上结合达西定律给出了浸水孔设计参数如孔深、孔间距及浸水孔个数的确定方法。结合铜川某工程,设计进行了现场预钻孔浸水试验,对该方法的合理性进行了验证,并通过现场钻探、现场勘探、室内湿陷性试验等方法对该方法的处理效果进行了评价。该浸水方法具有浸水时间短、浸水影响范围可根据浸水孔布设进行控制等优点,且浸水处理效果良好,完全符合施工要求。     

Introduction to crystallographic refinement of macromolecular atomic models

Refinement of atomic models is a necessary step in solving the macromolecular structure by X-ray diffraction methods. Nowadays, high automation and well-developed interfaces give a possibility to use the most popular refinement programs as black boxes. Nevertheless, working with complex objects requires an understanding of the internal structure and principles of operation of these programs and critical assessment of the results of refinement. In this review, we discuss the basic principles of the organization of refinement programs and the history of their improvement and development, as the studied objects became more and more complicated. The discussions are kept at the level of basic mathematic knowledge avoiding unnecessary formalism and too detailed expressions.     

电感耦合等离子体原子发射光谱法测定辛酸铑催化剂中铂钯铅铁铜铝镍

准确测定辛酸铑催化剂中杂质元素含量,是判定产品是否合格的重要指标之一。以往常采用直流电弧发射光谱法(摄谱法)进行检测,但测定周期长,且重复性较差。用电感耦合等离子体原子发射光谱法(ICP-AES)测定辛酸铑催化剂中微量杂质元素时,辛酸铑催化剂样品中含有的大量有机组分和铑基体会对测定有严重干扰。实验采用反复滴加硝酸消解样品中有机组分,再用王水溶解盐类,选用合适背景点扣除的方式消除铑基体的干扰,建立了使用ICP-AES测定辛酸铑催化剂中0.001%~0.1%(质量分数)Pt、Pd、Pb、Fe、Cu、Al、Ni等7种微量杂质元素的方法。各元素在0.10~10.00μg/mL范围内与其发射强度呈线性关系,相关系数均大于0.9999;方法检出限(μg/mL)为0.075(Pt)、0.0033(Pd)、0.015(Pb)、0.0036(Fe)、0.010(Cu)、0.001(Al)、0.012(Ni)。实验方法用于测定辛酸铑催化剂样品中Pt、Pd、Pb、Fe、Cu、Al、Ni,结果的相对标准偏差为(RSD,n=7)为1.4%~9.6%。按照实验方法测定辛酸铑催化剂中Pt、Pd、Pb、Fe、Cu、Al、Ni,并与直流电弧发射光谱法的测定结果进行比对,结果相一致。     

高分辨连续光源原子吸收光谱法测定铀铌铅多金属矿中痕量银

铀铌铅多金属矿组成成分复杂,准确有效的测定其中的痕量银,有利于银的回收利用。采用HCl-HNO₃-HF-HClO₄处理铀铌铅多金属矿样品,以HCl(1+4)-2g/L酒石酸为测定介质,以λ_Ag=328.068nm为分析谱线,建立了高分辨连续光源原子吸收光谱法(HR-CS-AAS)测定铀铌铅多金属矿样品中痕量银的新方法。对仪器参数进行了优化,确定采用迭代基线校正(IBC)背景校正方式,CCD检测器有效像素点选择5个;由银的平均吸收光谱图和吸光度-波长-时间三维吸收光谱图可知,银的CCD检测器分辨率为0.0020nm/pixel,λ_Ag=328.068nm在327.86~328.27nm范围内没有受到溶液中其他共存元素的谱线干扰。在优化的实验条件下,银的吸光度与其质量浓度在0.40~1.60μg/mL范围内运用二次方程最小二乘法拟合校准曲线,相关系数为0.9999,特征浓度为0.0148μg/mL,方法检出限为0.0013μg/mL。将HR-CS-AAS测定样品中银的参数与空心阴极灯原子吸收光谱法(HCL-AAS)相比,其检出限更低,特征浓度更低,标准溶液系列的吸光度更高。按照实验方法对铀铌铅多金属矿样品中的银进行测定,结果与电感耦合等离子体质谱法基本一致,相对标准偏差(RSD,n=9)为0.63%~3.3%。按实验方法在铀铌铅多金属矿样品中加入银标准溶液进行加标回收试验,回收率为97%~104%,满足国家地质矿产行业标准DZ/T 0130—2006的要求。     

基于数据拼接的金刚石刀具刃口三维形貌表征技术

原子力显微镜(AFM)是获取金刚石刀具刃口纳米级三维形貌的重要手段,但其存在测量范围小,难以表征参与切削区域整段刃口形貌特征的问题。采用基于迭代最近点法的刃口AFM测量数据拼接算法,获得了由多组数据拼接得到的刃口纳米级三维形貌,并进行了切削实验验证。实验结果表明,采用的数据拼接方法可较好地用于表征刀具刃口三维形貌。     

What is a crystal to the new chemical crystallographer,after that first,automated structure analysis?

This educational review postulates the importance of maintaining an adequate level of crystallographic education among structure-dependent scientists whose interests are not primarily in crystallography, at a time when automation and validation have made it possible to obtain high-quality structure analyses in many cases with a minimum of crystallographic background. The topics addressed are intended to form a second round of crystallographic education for a novice user whose first round involved hands-on experience with structure solution and an introduction to elementary concepts. The specific topics, chosen for their relevance as basic knowledge and their lack of emphasis in many formal treatments, are (1) crystallographic reference frames and the utility of the reciprocal cell in geometrical calculations; (2) the relationship between the two concepts that constitute our model of the crystal, namely the unit cell and the lattice; (3) the manner in which an atom is represented in concept and in practice; (4) the importance of interleaved symmetry elements required by the presence of additional symmetry on a lattice; (5) the harnessing of the natural properties of the crystalline state for the potential manipulation of properties of synthetic crystals; and (6) useful terminology for navigating a crystal structure.     

采煤工作面煤层注水参数试验研究

通过在6198采煤工作面现场施工煤层注水钻孔采取煤样,实验室试验注水钻孔水压力分布、煤样含水率变化,得到了工作面煤层注水影响半径等技术参数,为采煤工作面煤层注水提供了一定的参考依据。     

原子荧光光度法测定卤味香膏中砷含量的不确定度评定

评价氢化物原子荧光光度法测定卤味香膏中砷含量的不确定度。方法 根据实验流程，分析实验过程中不确定度来源，评定不确定度分量，最后计算合成不确定度和扩展不确定度。结果 当卤味香膏样品中砷的含量为0.46 mg/kg 时, 扩展不确定度U=0.04 mg/kg，(k=2)。结论 氢化物原子荧光光度法测定卤味香膏样品中砷的含量时，对不确定度影响较大的是标准曲线拟合和标准溶液配制， 这两项分量占总不确定度的68.77 %；测定重复性和仪器校准次之，样品称量和试样定容影响较小。实验中要准确配制标准溶液，绘制合理标准曲线，关注线性范围，线性相关系数应大于0.997，保证检测结果的准确性。