2，2，3-三甲基丁烷(C7H16)晶体的成核动力学

High temperature solid phase I of 2,2,3-trimethylbutane(C7H16)(TMB) was investigated by X-ray powder diffraction. The electron diffraction technique for observing the kinetics of phase transitions in the condensed matter has been applied to study the freezing of TMB clusters with diameter of~13nm. Cluster beams were generated from the supersonically expanded TMB vapor with mole fraction of 0.01 in neon carrier gas. The freezing evolution was monitored by electron diffraction in interval of 7-9 μs. Clusters with an average size of ~5,500 molecules were observed to freeze into the solid phase I at a nucleation rate of 3.5 × 1028 m-3•s- 1 at the freezing temperature of clusters, ～170K. The estimated growth rate of postcritical nuclei indicates that the observed nucleation in the present experiment corresponds to mononuclear freezing of the clusters into single crystals of solid phase I.     

纳米材料的结构Ⅰ:四氟化硅纳米粒子的结构(英文)

通过超声膨胀产生了直径约为4．3nm的SiF4纳米粒子，并用电子衍射表征其结构．在选择的射流部分中，粒子大小的分布是很窄的，因而可以用541个分子构成的分子簇进行结构精化．在SiF4的纳米粒子中，分子的堆积可用大块物质的立方晶体结构来模拟.还谈到纳米粒子表面上由于平动和转动运动引起的分子混乱．     

1,10-双(1’-苯基-3’-甲基-5’-氯代吡唑-4’-基)癸二酮-[1,10]对铁(Ⅲ)、钴(Ⅱ)和镍(Ⅱ)的萃取行为

1,10-双(1’-苯基-3’-甲基-5’-氧代吡唑-4’-基)癸二酮-[1,10](以下简称H_2A)是近年来开发的一个新型螯合萃取剂。蒋次清等研究了本文标题化合物的同系物1,9-双(1’-苯基-3’-甲基-5’-氧代吡唑-4’-基)壬二酮-[1,9]对铁(Ⅲ)、钴(Ⅱ)和镍(Ⅱ)的萃取行为,发现它能将铁(Ⅲ)与钴(Ⅱ)和镍(Ⅱ)分离,但不能实现钴(Ⅱ)和镍(Ⅱ)的分离。本文研究表明,当上述化合物的主碳链中C从9个增加到10个后,在适当条件下能实现铁(Ⅲ)、钴(Ⅱ)和锦(Ⅱ)间的相互分离。     

配合物Ni(C14H10N2O3)(C5H5N)的合成和晶体结构

A novel nickel(Ⅱ) complex with 2,4-dihydroxybenzalidene benzoylhydrazone and pyridine ligands, Ni(C₁₄H₁₀N₂O₃)(C₅H₅N), has been synthesized and characterized by elemental analysis and IR. The crystal structure of the title complex has been determined by single crystal X-ray diffraction techniques. The crystal belongs to orthorhombic, space group Pbca. The cell parameters are: a=1.580 20(19) nm, b=1.362 18(16) nm, c=1.616 50(19) nm, and V=3.479 5(7) nm³, Z=8, D_c=1.497 Mg·m^-3, μ(MoKα)=1.139 mm^-1, F(000)=1 616, R=0.032 9 and wR=0.077 0 for 2 772 observed reflections (I>2σ(I)) out of 3810 unique ones. The nickel(Ⅱ) ion lies in a distorted square-planar environment composed of two oxygen atoms, one nitrogen atom of tridentate acyhydrazone schiff base ligand and one nitrogen atom of the pyridine ligand. The analysis of the crystal structure indicates that the complex has a one-dimensional chain structure, which is formed by intermolecular hydrogen bonds. CCDC: 244668.     

草酸根桥联的双核铜(Ⅱ)配合物[Cu2(phen)2(H2O)2(μ2-C2O4)](NO3)2的合成及晶体结构

A new binuclear copper(Ⅱ) complex, [Cu₂(phen)₂(H₂O)₂(μ₂-C₂O₄)](NO₃)₂, has been synthesized and characterized by elemental analysis, IR and UV-Vis spectrum. Its crystal structure was determined by single crystal X-ray diffraction techniques. Crystal data: monoclinic, space group P2₁/c, a=0.712 21(8) nm, b=1.170 93(14) nm, c=1.783 7(2) nm, β=111.828(2)°, and V=1.380 8(3) nm³, D_c=1.769 Mg·m^-3, Z=2, F(000)=744, R₁=0.025 4, wR₂=0.069 5, Gof=1.077, Δρ=328～-455 e·nm^-3. The complex is packed by one centrosymmetry binuclear copper(Ⅱ) unit, oxalate dianion and NO₃^- anion. In the molecule structure of the title complex, two Cu(Ⅱ) ions are bridged by oxalate dianion and each Cu(Ⅱ) ions coordinates with two nitrogen atoms from 1,10-phenanthroline ligand and one oxygen atom from water to form a five-coordinate distorted square-pyramidal configuration. The hydrogen bonds are observed between coordinated water molecules and NO₃^- anions. The analysis of the crystal structure indicates that the complex has a two-dimensional stacking network structure, which is formed by intramolecular hydrogen bonds, intermolecular hydrogen bonds and stacking effect of aromatic ring. CCDC: 255345.     

三元混合配合物Cu(C10H8N2O3)·(C5H5N)·(H2O)的合成和晶体结构

The novel copper(Ⅱ) complex with 2-oxo-propionic acid benzoyl hydrazone and pyridine ligands, Cu(C₁₀H₈N₂O₃)·(C₅H₅N)·(H₂O) (C₁₀H₈N₂O₃^2- is the dinegative ion of 2-oxo-propionicacid benzoyl hydrazone), has been synthesized and characterized by elemental analysis and IR. The crystal structure of the title complex was determined by single crystal X-ray diffraction technique. Complex crystallized in the triclinic space group P1 with a = 0.729 08(10) nm, b= 1.020 01(14) nm, c= 1.126 28(15) nm, α = 71.644(2) °, β = 80.437(2) °, γ = 89.160(2)°, V= 0.78328(18) nm³, Z= 2, D_c= 1.547 Mg·m^-3, μ(MoKα) = 1.417 mm^-1, F(000) = 374. The final R₁ = 0.030 6, wR₂= 0.084 2 for 2 992 observed reflections [I≥2σ(I)] out of 3357 unique reflections. In this complex, copper(Ⅱ) ion is square-pyramidally coordinated by two oxygen atoms and one nitrogen atom of tridentate C₁₀H₈N₂O₃^2- ligand, one nitrogen atom of the pyridine ligand, and one oxygen atom of water molecule with the oxygen atom of water molecule locating at the apical position. The analysis of the crystal structure indicates that the complex has a one-dimensional chain structure, which is formed by intermolecular hydrogen bonds. CCDC: 222656.     

轮廓爆破孔壁压力峰值计算方法

爆破孔壁压力峰值是进行非流固耦合爆破动力响应分析的重要参数。针对轮廓爆破孔壁压力峰值的计算方法问题，理论分析了爆炸冲击波与弹性壁面的相互作用，推导了空气冲击波与弹性壁碰撞后压力增大倍数的理论解，并采用流固耦合动力有限元数值分析方法，研究了3种岩体介质、2种轮廓爆破常用炸药、5种常用不耦合系数、2种轴向装药系数工况下轮廓爆破的冲击波碰撞压力增大倍数和炮孔壁压力峰值。结果表明:轮廓爆破时，爆炸冲击波与孔壁碰撞后压力增大倍数并不是常值，与炸药特性、孔壁介质条件、不耦合装药系数等因素相关，孔壁压力峰值也与上述因素密切相关。基于模拟的孔壁压力峰值数据的统计分析，并结合理论推导成果及常用爆破孔壁压力峰值计算形式，提出了一种新的轮廓爆破孔壁压力峰值计算方法。     

模具法制备CVD金刚石热沉片的温度场与流场研究

本文通过有限元仿真研究了模具法制备CVD金刚石热沉片的温度场和流场,并对制备参数进行了优化.实验与仿真的结果均表明,进气量的大小对衬底附近流场的均匀性影响显著,热丝温度、热丝间距以及热丝到衬底的距离对衬底的平均温度影响显著,热丝间距和热丝温度对衬底温度的均匀性影响显著;模具法制备的CVD金刚石复制了模具型腔,保证了热沉片的结构完整性和尺寸精度,最终制备了精度较高的小型CVD金刚石热沉片.     

环形障碍物-轴棱锥产生局域空心光束

提出一种产生局域空心光束(bottle beam)的新方法,它是在传统的轴棱锥底面上放置一个环形障碍物.平面波入射到带有环形障碍物的轴棱锥底面时,将在轴棱锥产生的最大无衍射距离内形成bottle beam,而在bottle beam的前后仍然保持无衍射贝塞尔光.通过变化障碍物大小及轴棱锥底角实现bottle beam尺寸的控制.利用衍射理论描述了平面波经带有环形障碍物的轴棱锥产生bottle beam的原理,分析和模拟了传输过程中不同位置的截面光强分布及整个过程的三维光强分布,并给出相关的实验结果.研究结果对bottlebeam的实际应用具有积极的意义.     

中空纤维两相液相微萃取技术用于芝麻中共轭亚油酸的测定

基于中空纤维两相液相微萃取提取新技术,建立了芝麻中共轭亚油酸的液相微萃取/高效液相色谱测定的新方法。通过研究萃取剂pH值、萃取时间和搅拌速率的影响,确定了最优化的液相微萃取条件:pH11.0的KOH溶液为萃取剂,萃取时间为30 min,搅拌速率为1 000 r/min。采用高效液相色谱法对共轭亚油酸进行定性和定量测定,结果表明,该方法的线性范围宽,相关系数(r2)为0.993,检出限(S/N=3)为17μg/L,相对标准偏差(n=6)为4.9%,共轭亚油酸的富集倍数为12.4倍。用于3种不同品牌芝麻中共轭亚油酸的分析,回收率为81.4%～94.8%。本法为植物中共轭亚油酸的分析检测提供了一种简捷有效的方法,可为乳品、植物油等其他复杂基质样品中共轭亚油酸的检测提供有效参考。