离子交换树脂均匀沉淀法制备MgO纳米粒子

以(Mg(NO3)2·6H2O, (NH4)2CO3 和NH3·H2O为原料,采用两种离子交换树脂均匀沉淀法分别制备MgO纳米粒子.用热分析、X射线粉末衍射(XRD)、透射电子显微镜(TEM)、高分辨电子显微镜(HR TEM)、选区电子衍射(SAED)和BET等对所制备的MgO粒子进行了表征.结果表明:经700 ℃焙烧后制备的MgO纳米晶体属六方晶系,样品分散性较好,平均粒径约为25 nm;MgO纳米晶体清晰、有序的电子衍射点阵,表明晶体的结晶度较好;纳米粒子a和b的比表面积分别为31 m2/g and 32 m2/g.     

不同形貌二水草酸钙晶体的合成、表征及其对肾上皮细胞的损伤作用

合成了4种不同形貌和尺寸的二水草酸钙(COD)晶体,分别为尺寸20μm的花状、10μm的十字形、2μm的四方双锥形和1μm的棒状COD晶体.采用X射线衍射、傅立叶变换红外光谱、扫描电子显微镜(SEM)和比表面测试仪对上述4个COD晶体的理化性质进行了表征.花状和十字形COD晶体都具有尖锐的棱角;棒状、四方双锥形COD都具有完整的(100)面.随着晶体尺寸的降低和晶体表面正电荷密度高的(100)面比例增大,其Zeta电位绝对值不断减小.不同形貌COD晶体均对非洲绿猴肾上皮细胞(Vero)具有毒性作用,其细胞毒性大小与多因素相关,包括晶体的尺寸、晶面、尖锐程度、比表面积以及Zeta电位等.本研究有助于进一步阐明尿微晶形貌差异影响肾结石形成的分子和细胞机制.     

纳米ZnO的形态控制及其发光性能

以醋酸锌为原料,以聚合物和表面活性剂为添加剂,水热法合成了两种新型的纳米ZnO结构.并采用X射线衍射(XRD)、透射电镜(TEM)和高分辨透射电镜(HRTEM)以及光致发光光谱(PL)等测试方法对所得产物形貌和光学性能进行了研究,并对对两种纳米形态的形成机理进行了初步的探讨.结果表明:所得产物为六角纤锌矿型氧化锌纳米晶,分散性良好,形貌为枣核状,而这种枣核状的粒子是由众多短棒状粒子取向生长而形成的.升高温度,则得到了直径约100 nm,长约2 μm 的两头尖的纳米棒,棒的表面依附生长了针状颗粒.     

Bridgman法生长的大尺寸钨酸铅晶体的光学和闪烁性能

本文报道了我们采用改进的Bridgman法为欧洲核子研究中心(CERN)大型强子对撞机(LHC)上的紧凑型μ子螺线管(CMS)实验生长的大尺寸掺Y3+钨酸铅闪烁晶体,给出了晶体的光学和闪烁性能,如光致发光谱、X射线致发光光谱、纵/横向的透射光谱、光产额以及辐照硬度.测试结果表明,掺Y2O3的钨酸铅晶体光产额很高(>13pe/MeV),且全为100ns以内的快发光,其辐照硬度已接近CMS电磁量能器(ECAL)端帽晶体的要求,同一批晶体彼此间的性能一致性好.     

上海光机所研制超薄Ce∶YAG闪烁晶体用于高分辨X光成像

<正>近期,中国科学院上海光学精密机械研究所中科院强激光材料重点实验室利用提拉法生长出的高品质Ce∶YAG闪烁晶体开展了高分辨率X射线成像系统核心器件——闪烁体研制工作,成功制备了尺寸为30mm,厚度为30~45μm的高品质闪烁晶体元件,并和中科院上海应用物理研究所合作,研制基于超薄Ce∶YAG闪烁晶体的高分辨X光探测器,实现X光辐照条件下高分辨成像。在同等实验条件下,与Crytur公司同     

铜掺杂类金刚石纳米点阵列的制备及场发射性能研究

利用磁过滤等离子体结合氧化铝模板(AA0)技术在室温下制备了具有优异场发射性能的铜掺杂类金刚石(DLC)纳米点阵列.微观分析表明,铜掺杂类金刚石纳米点阵列分布均匀,密度高达109cm-2;利用X射线光电子能谱对制备的铜掺杂类金刚石纳米点阵列进行结构分析,测得铜的掺杂量为3.6;且sp3键含量高达60;;通过对铜掺杂类金刚石纳米点阵列的场发射性能测试,试验结果表明,铜掺杂类金刚石纳米点阵列开启电场和阈值电场分别为0.08V/μm,0.42V/μm,并且在电场值为0.67V/μm时,发射电流密度高达95mA/cm2,场发射性能明显优于无掺杂类金刚石纳米点阵列.     

中子辐照6H-SiC晶体中的钉扎效应

分别对两种不同的6H-SiC晶体进行了总通量为5.74×10~(18) n· cm~(-2)、8.2×10~(18) n· cm~(-2)和1.72×10~(19) n· cm~(-2)的不同剂量的中子辐照,利用X射线衍射等手段观测了中子辐照引起的晶体内部损伤.结果表明:两种样品在不同的中子通量辐照下,消除部分原始缺陷的、纯度较高的样品辐照后的内部损伤明显小于纯度较低、内部原始缺陷较多的样品.样品的辐照损伤不仅取决于中子辐照剂量,还取决于其辐照时的成分和结构.晶体的结构缺陷和杂质,作为一种"钉扎",在辐照过程中作用极大,它们导致了晶体的长程缺陷(如位错)的大幅度增加.     

蓝宝石单晶窗口材料空间粒子辐照效应研究

蓝宝石单晶(α-Al2O3)窗口材料服役于空间环境中将不可避免地受到各种不同射线及离子流的辐照作用,影响其使用性能.本文研究了蓝宝石单晶经不同剂量质子流、电子流以及综合流辐照后其表面粗糙度、透过率以及面形精度等光学性能和结构的变化.实验表明空间粒子辐照使蓝宝石表面粗糙度增大且具有剂量效应,其中综合流对表面粗糙度影响最大,质子次之,电子影响最小;UV-Vis-VIR及FTIR测试实验表明空间粒子辐照使蓝宝石透过率下降,在紫外波段下降最明显,且在不同波段范围内不同辐照粒子种类对蓝宝石单晶透过率的影响程度也不同;粒子辐照对面形精度的影响不明显.     

不同有机物模板作用下Bi2S3的制备与表征

以硝酸铋为铋源、硫脲为硫源,分别以小分子有机物-巯基乙酸、柠檬酸及聚合物半导体-羧基化PPV(羧基化的聚对苯乙炔)为模板,利用水热反应法制备了不同形貌的Bi2S3微晶,并对产物用X射线衍射(XRD)、扫描电子显微镜(SEM)、紫外-可见-近红外光谱(UV-Vis-Near-IR)等进行表征.结果表明,所制备的Bi2S3微晶为斜方晶系的辉铋矿;在巯基乙酸的作用下,Bi2S3排列成直径约为2～3 μm的花状微晶;在柠檬酸的作用下,Bi2S3晶体呈絮状,结成直径约为2μm左右的绒球;在羧基化PPV的作用下,Bi2S3构成直径约为2μm的绒球.通过由UV-Vis-Near-IR光谱绘制的(αhv)2～hv曲线图计算得到,在不同有机物模板作用下得到的Bi2S3微晶的能带间隙均大于无模板作用得到的Bi2S3,且羧基化PPV的作用效果优于小分子有机物,使能带间隙提高为1.64 eV.     

硝酸银辅助的氧化锌纳米线的气相法制备

以硝酸银作为催化剂前驱物,通过低成本的CVD法,成功合成了氧化锌纳米线.利用场发射扫描电镜(FE-SEM)、X射线衍射仪(XRD)、高性能X射线能谱仪(EDS)、荧光光谱仪等研究了氧化锌纳米线的形貌、相结构、化学成份和光致发光特性.研究结果表明:所获得的氧化锌纳米线具有六方纤锌矿结构;平均直径为50nm,长度在3～5μm之间;室温下,氧化锌纳米线除了有明显的紫外发射外,在421nm附近还有紫光发射.整个氧化锌纳米线的生长由气-液-固机制所控制.     

First-principles coexistence simulations of supercooled liquid silicon

We perform first-principles coexistence simulations of the low-density and the high-density phases of supercooled liquid silicon and find a negative slope for the coexisting line in the temperature-pressure plane. Electron density maps and electron-localization function plots of the two phases of silicon show marked differences. The calculated differences suggest more localized electrons in the low-density liquid compared to the high-density liquid, coming from an increased population of covalent bonds, which further explain the calculated negative slope in the two phase coexistence regime. This is consistent with the presence of a pseudo-gap in low-density liquid silicon, absent in the high-density liquid which shows a metallic behavior.     

Triethyl ammonium salt of O,O′-bis(p-tolyl)dithiophosphate, [Et3NH]+[(4-MeC6H4O)2PS2]−

Triethyl ammonium Salt of O,O′-bis(p-tolyl)dithiophosphate and O,O′-bis(m-tolyl)dithiophosphate have been obtained by reaction of p- and m-cresol, respectively with P₂S₅ in toluene and have been characterized by elemental analysis, IR, ¹H and ³¹P NMR spectroscopy. The molecular structure of O,O′-bis(p-tolyl)dithiophosphate has been determined. Crystal data: [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻: Monoclinic, P2₁/c, a=15.2441(9) ?, b=10.415(2) ?, c=3.9726(9) ?, β=91.709(7)°, V=2217.5(1) ?⁻³, Z=4.Supplementary materials Additional material available from the Cambridge Crystallographic Data Centre (CCDC no. 600927 for [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻ comprises the final atomic coordinates for all atoms, thermal parameters, and a complete listing of bond distances and angles. Copies of this information may be obtained free of charge on application to The Director, 12 Union Road, Cambridge CB2 2EZ, UK (fax: +44-1223-336033; email: deposit@ccdc.cam.ac.uk or www:http://www.ccdc.cam.ac.uk).     

Crystal structures of thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane

Structures of both thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane, ?C₆H₄?CH₂SCH₂?C₆H₁₀?CH₂SCH₂?, have been determined, wherecis andtrans refer to the attachments to the cyclohexane ring. Thecis form crystallizes in the monoclinic space groupP2₁/c witha=8.4299(11)Å,b=21.772(2)Å,c=8.9724(13)Å, β=116.574(11)^o, andZ=4. Thetrans isomer packs into the monoclinic space groupP2₁ witha=8.159(16)Å,b=10.185(5)Å,c=9.558(2)Å, β=112.435(18)^o, andZ=2. The cyclohexane ring of thecis isomer is in the chair conformation, while the cyclohexane of thetrans isomer is found in a twisted boat conformation.     

CTAB与SDBS对碳酸锶粒子生长形态调控及机理研究

以表面活性剂CTAB和SDBS为化学添加剂,采用化学共沉淀法对碳酸锶晶体的生长形态进行调控,成功地制备出了实心的树枝状和花瓣为空心的花状碳酸锶粉体,并用X射线衍射(XRD)、扫描电子显微镜(SEM)和傅里叶变换红外光谱(FT-IR)等分析手段对样品进行了表征;最后重点对化学添加剂可能产生的影响机理进行了初步的探讨.结果表明,CTAB和SDBS在晶体生长的过程中能起到显著的影响作用,两者对粒子分散性能的作用效果相反,而且后者对晶体(013)和(213)晶面表面能降低的贡献明显大于前者.     

Crystal structures of the cis and trans isomers of a tetrathia[3.3.3.3]cyclophane

Both the cis and trans isomers of 3,11,18,26-tetrathiatricyclo[26.2.2.1^5,9.2^13,16.1^20,24] hexatriaconta-5,7,9,20,22,24-hexene have been prepared and structurally characterized. Each of these centrosymmetric tetrathia dimers includes two cyclohexane rings in chair conformations with either 1,4-cis or 1,4-trans bonding and two meta-substituted benzene rings. The cis isomer packs into the monoclinic space group P2₁/a with a = 10.485(3)Å, b = 10.3956(18)Å, c = 14.1343(10)Å, = 105.200(13)°, Z = 2 and refined to an R factor of 0.046. The trans isomer crystallizes in the monoclinic space group P2₁/c with a = 10.7217(12)Å, b = 5.6797(7)Å, c = 25.415(5)Å, = 96.001(12)°, Z = 2 and refined to an R factor of 0.043. In the cis structure each benzene ring faces a cyclohexane ring while in the trans structure the cyclohexane rings face one another.     

Crystal structure of Zn4Na(OH)6SO4Cl·6H2O

The structure of Zn₄Na(OH)₆SO₄Cl·6H₂O, a secondary mineral from Hettstedt, Germany, was determined by single-crystal X-ray diffraction. The crystals are hexagonal,a=8.413(8),c=13.095(24) Å, space group $P\bar 3$ , Z=2. The structure was refined to R=0.0554 and R_w=0.0903 for 970 reflections with I≥3σ(I). The structure can be described as zinc hydroxide layers perpendicular toc, from which sulfates and chlorides extend. The layers are held together by a system of hydrogen bonds involving hexaaquo Na⁺ ions which occupy the interlayer space.     

Synthesis and Crystal Structure of 5-[2-(6-bromonaphthalenyloxymethyl)]-3-(4-morpholinomethyl)-1,3,4-oxadiazole-2(3<Emphasis Type="Italic">H</Emphasis>)-thione

Abstract  The title compound, C₁₈H₁₈BrN₃O₃S, a derivative of 1,3,4-oxadiazole, crystallizes in the triclinic space group P-1 with unit cell parameters a = 6.8731(3), b = 8.9994(4), c = 15.7099(6) ?, α = 92.779(3)°, β = 130.575(3)°, γ = 107.868(4)°, Z = 2. The dihedral angle between the mean planes of the planar naphthyl and morpholine (chair) rings with the planar oxadiazol ring is 50.1(8) and 76.8(6)°, respectively. The planar naphthyl ring is twisted 52.2(5)° with the mean plane of the morpholine ring. A group of four intermolecular close contacts are observed between a bromine atom and hydrogen atoms from the closely packed naphthyl, morpholine and oxy–methyl groups in the unit cell. These molecular interactions in concert with an additional series of π–π stacking interactions that occur between the center of gravity of the two 6-membered rings of the naphthalene group influence the twist angles of each of these three groups. A MOPAC AM1 calculation of the conformation energy of the crystal structure [226.0128(9) kcal] compared to that of the minimum energy structure after geometry optimization [29.9744(1) kcal] reveals a significantly reduced value. The twist angles of the three groups above also change after the AM1 calculation giving support to the influence of both intermolecular C–H···Br short-range interactions and Cg π–π stacking interactions on these angles which therefore play a role in stabilizing crystal packing. Graphical Abstract  Crystal structure of 5-{[(6-bromonaphthalen-2-yl)oxy]methyl}-3-(morpholin-4-ylmethyl)-1,3,4-oxadiazole-2(3H)-thione, C₁₈H₁₈BrN₃O₃S, is reported and its geometric and packing parameters described and compared to a MOPAC computational calculation. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

电沉积法制备ZnO纳米棒阵列及其发光特性

本文以掺F的SnO2导电玻璃为基板,以硝酸锌水溶液为电解液,采用三电极恒电位体系电沉积制备ZnO纳米棒阵列,系统考察了硝酸锌浓度和沉积电位等工艺参数对ZnO纳米棒阵列的微观形貌及其发光性能的影响规律.结果表明,硝酸锌浓度和沉积电位对纳米棒阵列的形貌有显著影响,控制适宜的工艺条件可以制备出直径分布均匀、结晶性好且纯度高的六方纤锌矿ZnO纳米棒阵列.荧光光谱分析表明,电沉积制备出的ZnO纳米棒阵列在385 nm附近有一个强荧光发射峰,且发光性能稳定、对纳米棒阵列微观形貌的细微变化不敏感,使其在发光二极管和激光器等领域具有广阔的应用前景.     

Crystal structure of irisolidone from the flowers of Pueraia lobata

Irisolidone (5,7-dihydroxy-6,4′-dimethoxyisoflavone) was isolated from the flowers of Pueraia lobata and its crystal structure was examined by X-ray single crystal diffraction. The crystal structure of irisolidone is monoclinic, space group P2₁/c with a = 15.491(9) ?, b = 7.895(4) ?, c = 13.321(7) ?, β = 110.546(9)° and Z = 4. Hydrogen bonding and aromatic π–π stacking assemble the title compound into a three-dimensional networking structure.