系列硅铝比纳米薄层ZSM-5分子筛的合成和表征

以自制不对称双子季铵盐表面活性剂为模板, 在水热合成体系中控制合成系列硅铝比纳米薄层ZSM-5分子筛.采用X射线衍射(XRD)、N₂吸附-脱附、X射线荧光光谱(XRF)、扫描电镜(SEM)和²⁷Al魔角旋转核磁共振(²⁷Al MAS-NMR)对合成的样品进行了表征. 详细研究了晶化温度、晶化时间、结构导向剂(SDA)用量、碱度等对合成的影响和纳米薄层ZSM-5分子筛的形成过程. 结果表明: 分子筛硅铝比越高, 结构导向剂用量越大, 所需的晶化时间越短; 晶化温度越高, 晶化时间越短; 且不同硅铝比纳米薄层ZSM-5分子筛的形貌规整度、比表面积和介孔/微孔孔容比例随着硅铝比而变化.     

2,2'-联吡啶-3,3',6,6'-四羧酸过渡金属配合物的合成、结构及性质

以2,2'-联吡啶-3,3',6,6'-四羧酸(H₄bptc)为配体,通过水热合成的方法与过渡金属盐合成了3个配合物,其分子式分别为[Co₂(H₂bptc)₂(H₂O)₄]·bpe·9H₂O(1),[Ni₂(H₂bptc)₂(H₂O)₄]·bpe·9H₂O(2),[Ni₂(H₂bptc)₂(H₂O)₄]·0.5bpp·7H₂O(3)(bpe=1,2-二(4-吡啶基)乙烯,bpp=1,2-二(4-吡啶基)乙烷)。用红外光谱,X-射线单晶衍射对化合物的晶体结构进行了表征,并对这3个配合物的热稳定性进行了测试。化合物1~3为单核结构的配合物,它们均通过分子间氢键形成三维超分子结构。     

ChemInform Abstract: Structure,Ionization, and Fragmentation of Hydrogenated Aluminoboron Clusters: Al2B2H2n (n = 0—6).

Energetic and structural stability of Al₂B₂H_2n (n = 0—6) clusters is investigated by DFT calculations and a stochastic search algorithm.     

Polyaspartamide–Polylactide Graft Copolymers with Tunable Properties for the Realization of Fluorescent Nanoparticles for Imaging

Here, the synthesis and the characterization of novel amphiphilic graft copolymers with tunable properties, useful in obtaining polymeric fluorescent nanoparticles for application in imaging, are described. These copolymers are obtained by chemical conjugation of rhodamine B (RhB) moieties, polylactic acid (PLA), and O‐(2‐aminoethyl)‐O′‐methyl poly(ethylene glycol) (PEG) on α,β‐poly(N‐2‐hydroxyethyl)‐d,l ‐aspartamide (PHEA). In particular, PHEA is first functionalized with RhB to obtain PHEA–RhB with a derivatization degree in RhB (DD_RhB) equal to 0.55 mol%. By varying the reaction conditions, different amounts of PLA are grafted on PHEA–RhB to obtain PHEA‐RhB‐PLA with DD_PLA equal to 1.9, 4.0, and 6.2 mol%. Then, PEG chains are grafted on PHEA‐RhB‐PLA derivatives to obtain PHEA‐RhB‐PLA‐PEG graft copolymers. The preparation of polymeric fluorescent nanoparticles with tunable properties and spherical shape is described by using PHEA‐RhB‐PLA‐PEG with DD in PLA and PEG equal to 4.0 and 4.9 mol%, by following easily scaling up processes, such as emulsion‐solvent evaporation and high pressure homogenization (HPH)‐solvent evaporation techniques.

     

Baroque glass mosaics from the Capela de São João Baptista (Chapel of Saint John the Baptist,Lisbon): unveiling the glassmaking records

For the first time, 18th‐century glass mosaics from the Capela de São João Baptista (Chapel of St. John the Baptist, Lisbon) were analysed by Raman microscopy (RM). This masterpiece in baroque mosaic art had one of its major contributors the most famous glassmaker in Rome, Alessio Mattioli. Mattioli was celebrated because of the opacity of his mosaics and the astonishing number of hues he was able to produce for mosaic decorating Saint Peter's Basilica in Rome. This study had two goals in mind: (1) characterising the materials involved in the manufacture of these glass mosaics and (2) lengthening the understanding of what was left of Mattioli's glassmaking records. As expected the mosaics presented a high ratio of crystalline phases, making RM the ideal technique for non‐destructive analysis. The mosaics contained a white ‘background’ or opacifier added identified as Ca₂Sb₂O₇. The yellow tesserae are opacified with lead antimonate (Pb₂Sb₂O₇) and ternary oxides, structures related to lead antimonate but with other ions entering the position of Sb⁴⁺ (namely Sn⁴⁺). Those ternary oxides are pervasive in most colours, admixed with other colorants. The red, orange, pink and brown colours were accomplished with cuprous oxide (Cu₂O) and admixed with a ternary oxide to create the latter three colours. The red copper‐based colours were made according to the procedure to make a ruby copper glass and with the exception of the red colour; all mosaics exhibited a dark layer on each side of the mosaic, named scorzetta. This layer is the outcome of an oxidation reaction because of a quick cooling process and is composed of CuO. Finally the blue and green colours are accomplished with cobalt oxide and copper oxide, respectively, and the purple/black colour with manganese oxide. Copyright © 2015 John Wiley & Sons, Ltd.     

ChemInform Abstract: Crystal Structure of Potassium Sodium Heptahydrogen Hexamolybdocobaltate(III) Octahydrate: An Extra‐Protonated B‐Series Anderson‐Type Heteropolyoxidometalate.

KNa[Co^III(OH)₇{Mo₆O₁₇}] ·8H₂O is obtained by ion‐exchange from a solution of K₃ [Co(μ₃‐OH)₆Mo₆O₁₈] ·7H₂O at ≈pH 1.4 using Amberlite IR120 ion exchange resin followed by concentrating the solution in a hot water bath.     

[100]LiF单晶在60 GPa以内冲击加载下的高压屈服强度特性

获取光学窗口自身的高压强度特性是开展材料高压高应变率冲击响应行为精密测量和数据反演的重要基础。利用平板撞击和双屈服面法,通过冲击-卸载、冲击-再加载原位粒子速度剖面精细测量和数据反演,获得了约60 GPa范围内[100]LiF屈服强度特性随冲击压力的变化规律。结果表明:在实验压力范围内,[100]LiF的屈服强度随加载压力的提高而显著提高,压力硬化效应显著;同时,LiF在冲击加载下的屈服强度高于磁驱准等熵加载结果,应变率硬化效应强于热软化效应。采用Huang-Asay模型确定了可描述冲击加载[100]LiF强度特性的本构模型参数,为LiF在强度、相变、层断裂等加窗测量实验中的深入应用和数据准确解读提供了重要支撑。     

一种弹体入水冲击波阴影成像可视化系统及其试验研究

扩大成像视野对于开展充水容器中弹体入水冲击波传播及弥散方面的可视化研究具有重要的实际意义。阴影成像技术适用于大视野实验,且对流场冲击波和扰动的可视化研究具有简单性和通用性,其中直接阴影成像最为简单,但可靠点光源的缺乏是阻碍其发展应用的瓶颈。因此基于国产短弧氙灯管,自制了短弧氙灯点光源,根据阴影成像原理,设计出一种弹体入水冲击波阴影成像可视化系统,详细介绍了其组成和运行原理。利用该系统对高速弹体入水进行了试验研究,获得了弹体入水冲击波的阴影成像和冲击波信号的压力时程曲线,通过阴影成像和冲击波信号相结合分析了弹体入水冲击波的传播特性,并进行了理论验证。结果表明:该弹体入水冲击波阴影成像可视化系统具有可靠性和设计的合理性。弹体高速入水后,初始冲击波的强度最大,随着冲击波的传播,冲击波强度逐渐降低,水中冲击波的传播速度不断降低,球形冲击波的半径逐渐增大。     

爆炸载荷下脆性颗粒体系破碎特性的数值研究

试验发现,以球形TNT为中心爆源,球形玻璃珠构成的颗粒和球壳中发生破碎的颗粒体积分数随当量比(颗粒球壳的质量与TNT炸药的质量比)的增加呈现指数衰减规律。采用有限元与离散元耦合的连续非连续数值方法,揭示了中心炸药起爆后颗粒环壳内爆炸波的传播衰减和在环壳外界面反射后的稀疏卸载过程。由于爆炸波的短脉冲特性,颗粒内部应力场始终处于应力非均衡状态,采用应力均衡状态下颗粒破碎强度的Weibull分布会得到远高于试验测得的破碎颗粒体积分数。因此采用破坏波传播特征时间内的平均诱导应力而非瞬时诱导应力作为颗粒破碎强度的应力指标,并通过试验结果确定破坏波传播特征时间。考虑了应力传播的非均匀性对于颗粒破碎的影响,得到了平均诱导应力峰值的概率分布随比例距离的变化规律,结合修正后的颗粒破碎强度Weibull分布建立了破碎颗粒体积分数随比例距离的变化模型。     

延性材料平面冲击波基本实验数值模拟的若干问题

假设屈服强度正比于剪切模量,分别构建了四种强度模型,并用于数值模拟Ly12铝的平面冲击波试验的质点速度剖面以及钨合金的平面冲击波试验的锰铜计应力记录.研究发现,基于Steinberg等的屈服强度模型比较符合实验.还对平面冲击波试验的层裂现象进行了简化的数值模拟,其中,采用了该文作者所提出的一种基于空穴聚集的层裂模型,该模型的特点是分别引入了层裂过程的早期及后期应力松弛方程.