Synthesis, Structure and Characterization of [Cu(2,2'-bpy)2][{Cu(2,2'-bpy)2}2W12O40(H2)]·4H2O

An organic-inorganic compound [Cu(2,2'-bpy)2][{Cu(2,2'-bpy)2}2W12O4o(H2)]·4H2O (Mr = 4048.00) was prepared from the hydrothermal reaction of Na2WO4·2H2O, CuCl2·2H2O,2,2'-bipyridine (2,2'-bpy) and H2O at 160 ℃ for 4 days. The compound crystallizes in the monoclinic system, space group P21/n with a = 18.9196(8), b = 20.4212(8), c = 21.8129(9)(A), β=96.992(3)°, V= 8365.0(6) (A)3, Dc= 3.214 g/cm3, Z = 4,μ(MoKα) = 17.269 mm-1 and F(000) = 7324.Of the 119837 total reflections, 17315 were unique (Rint = 0.0489). The final R = 0.0385 and wR =0.0770 for 11142 observed reflections with I ＞ 2σ(I). Single-crystal X-ray diffraction reveals that the structure is composed of [{Cu(2,2'-bpy)2}2W12O40(H2)]2- anions, discrete [Cu(2,2'-bpy)2]2 cations and lattice water molecules, and the anion is made up of a {W12O40(H2)}6- α-Keggin core decorated with two {Cu(2,2'-bpy)2}2 groups through bridging oxygen atoms.     

Microwave Pyrolysis and Electrochemical Supercapacitor of S-doped g-C_3N_4 Nanoparticles

In this study, S-doped g-C_3N_4 nanoparticles were successfully prepared by one-step solid-state microwave synthesis. The detailed characterizations through XRD, FT-IR, SEM and XPS were studied. In addition, the electrochemical properties as supercapacitor of the sample were tested by cyclic voltammetry(CV), galvanostatic charge-discharge(GCD) and electrochemical impedance spectroscopy(EIS) techniques. The results showed a high specific capacitance of 691 F/g at current density of 4 A/g in 2 M KOH + 0.15 M K_3[Fe(CN)_6] electrolyte. This study shows that the microwave synthesis is a promising way to design carbon-based electrodes for supercapacitor.     

碘化铅单晶体生长新方法探索

本文分析了用布里奇曼法生长碘化铅单晶体的结晶过程。发现坩埚下降法生长碘化铅单晶体过程中,碘的蒸发与凝结、铅的分凝与沉淀是影响晶体质量的两个重要因素。提出了采用U型安瓿提拉方式生长碘化铅单晶体的新方法,有效抑制了碘的蒸发并排除了分凝的铅,获得了桔红色半透明的碘化铅晶体。经测试,晶体的结晶性好,红外透过率达45%,电阻率为1.7×1012Ω.cm,为制备性能优异的碘化铅室温核辐射探测器奠定了基础。     

燃烧剂对低温燃烧合成Pr-CeO2粉体结构与性能的影响

以乙酸铵和柠檬酸为燃烧剂,Ce(NO3)3·6H2O和Pr6O11为主要原料,采用低温燃烧法(LCS)制备了Ce0.95Pr0.5O2纳米晶粉体.用DSC、XRD、SEM及色度测试等手段研究了Ce0.95Pr0.5O2纳米晶微粒前驱体的着火温度、产物晶体结构、晶体形貌及色度.结果表明:乙酸铵和柠檬酸作为燃烧剂的反应前驱体着火温度分别在250℃和300℃左右.两种燃烧产物均为单一的萤石型固溶体.与柠檬酸相比,乙酸铵作为燃烧剂得到的燃烧产物结晶程度更完善、Pr离子进入CeO2晶格的含量更多、呈色更好,且颗粒的团聚程度变小.根据Scherrer公式计算,用两种燃烧剂制备产物的平均晶粒尺寸分别为20～30 nm和10～15 nm,为纳米晶颗粒.最后得到Ce0.95Pr0.5O2粉体的颗粒尺寸则在200～300 nm之间.乙酸铵与硝酸铈的最佳摩尔配比为2:1,柠檬酸与硝酸铈的最佳摩尔配比为3:1.     

用化学溶液方法在Ni-5at%W基底上制备La2Zr2O7过渡层的研究

La2Zr2O7(LZO)过渡层以其独特的物理化学性质越来越受到人们的关注。本文以乙酰丙酮镧和乙酰丙酮锆为前驱盐,丙酸为溶剂配置前驱液,用化学溶液方法(CSD)在具有立方织构的Ni-5at%W基底上制备了LZO过渡层薄膜。研究了前驱液成分、性质以及退火温度对LZO成相以及取向的影响。用常规XRD和X射线四环衍射仪分析了LZO薄膜的相成分和织构。结果显示,在1050℃下退火可以获得强立方织构的LZO薄膜,其中(222)峰的Phi扫描半高宽值为8.95°;(400)峰的Chi扫描半高宽值为6.8°。用高分辨扫描电子显微镜(FE-SEM)观察到LZO薄膜表面均匀致密,没有裂纹和空洞。     

Tailoring Pore Structure and Morphologies in Covalent Organic Frameworks for Xe/Kr Capture and Separation

As a rising star among porous solid materials, covalent organic frameworks(COFs) with excellent properties including but not limit to facilely controllable structure, high porosity, and multi-chemical functionality represent significant potential for efficient ¹²⁷Xe/⁸⁵Kr capture and separation. In this study, through tuning the length of the organic ligands, two-dimensional(2D) COF mate-rials with identical connection group but different pore properties, denoted as ATFG-COF and TpPa-COF with AA-stacking model and TpBD-COF with AB-stacking model were synthesized and tested for Kr and Xe adsorption for the first time. Adsorption measurements indicate that the narrower pore apertures and higher porosity are conducive for COF materials to capture Xe and Kr. Furthermore, the Henry's constant, isosteric heat of adsorption(Q_st), and ideal adsorbed solution theory(IAST) selectivity of ATFG-COF, the pore size of which is closest to the kinetic diameter of the Xe atom(0.41 nm) among 2D COF materials, were carried out based on the single component sorption isotherms. The results illustrate that the high isosteric heat values of Xe/Kr adsorption on ATFG-COF are 25 and 16 kJ/mol at room temperature, respectively. Henry's law predicts that the selectivity factor of Xe to Kr is 6.07, consistent with the adsorption selectivity(ca. 6) calculated based on the IAST.     

MOS器件辐照过程和辐照后效应模拟

模拟MOS器件脉冲电离辐射响应和长时间恢复效应.假设隧道电子从硅进入氧化层和界面态的建立是辐射效应的恢复机理.在整个退火恢复期,采用卷积模型并考虑了栅偏置压的效应.模拟结果表明:退火过程所加栅偏压的大小以及隧道电子效应与建立的界面态所占比例的不同影响器件的恢复率.     

ISOVALEROYL OXOKADSURANE,A NOVEL DIBENZOCYCLOOCTADIENE LIGNAN POSSESSING A SPIROBENZOPURANOID SKELETON

Isovaleroyl oxokadsurane, a novel dibenzocyclooctadiene lignan pos-sessing a spirobenzofuranoid skeleton was isolated from the stems of Kadsura coccinea.Its structure and relative configuration were determined by X-ray diffraction analysis.     

辐射量热计在HT-6BTokamak上的测量

一、引言 在现行的托卡马克实验中,辐射损失和中性粒子损失是高温等离子体能量损失的主要通道之一。为了更好地了解托卡马克等离子体中能量平衡、辐射损失以及这些损失随等离子体参数的变化;了解等离子体中杂质含量和杂质输运以及等离子体与器壁的相互作用,辐射能量损失的时间特性、空间分布的测量显得很有必要。为