硫化锌微米球的水热合成和光催化性能

采用简单的低温水热法成功合成了硫化锌微球.利用X射线衍射(XRD)、场发射扫描电镜(FESEM)、透射电镜(TEM)、光催化、光致发光(PL)和紫外-可见吸收光谱(UV-Vis)技术对ZnS样品的结构、形貌及光学和光催化性能进行表征和分析.结果表明ZnS微米球为立方闪锌矿,所制备样品的PL发射中心位于468 rn,室温UV -Vis吸收峰位于276.5nm.光催化性能显示,在自然光照射1h时,甲基橙的降解率达到93.15;.实验制备的硫化锌样品具有较好的光催化性能和应用前景.     

Ag/ZnS核壳结构纳米棒的制备及其光催化性能分析

在制备的Ag纳米线的基础上,用水热法合成了Ag/ZnS核壳结构纳米棒.使用X射线衍射仪(XRD)、场发射扫描电子显微镜(FESEM)、X射线能谱仪(EDS)、高分辨透射电子显微镜(HRTEM)、紫外-可见双光束分光光度计(UV-vis)、光致发光扫描仪(PL)等检测设备对样品的成分、形貌、微结构及光学性能进行了表征.结果显示,制备的Ag/ZnS复合材料为ZnS纳米颗粒包覆Ag纳米线的核壳结构,其紫外吸收峰位于350 nm处,相对于ZnS纳米颗粒变宽并发生红移,PL发射峰位于462 nm处,相对于ZnS纳米颗粒发生了蓝移,强度明显降低.光催化结果显示,Ag/ZnS核壳结构纳米棒的光催化性能优于ZnS纳米颗粒,分析了光催化反应机理.     

氧化锌空心球的制备及其光催化性能研究

以葡萄糖、尿素和醋酸锌为原料在低温下合成了炭微球,高温煅烧后制备了氧化锌空心微球.通过X-射线衍射(XRD)、扫描电子显微镜(SEM)等手段对制得的样品进行了表征.以甲基橙溶液为研究对象考察了氧化锌空心微球的光催化性能.实验结果表明,当葡萄糖和醋酸锌质量比为3∶1时,制备的ZnO微球具有较好的光催化性能.     

纳米结构四氧化三铁空心微球的合成及磁性研究

用乙二醇为溶剂,三氯化铁和尿素为起始反应试剂,通过水热反应合成了Fe3O4空心微球.用X射线衍射仪(XRD)、透射电子显微镜(TEM)和扫描电子显微镜(SEM)表征样品的结构和形貌,结果表明,所制备的单分散Fe3O4空心微球为立方单晶结构,其直径约400 nm,是由纳米颗粒组装而成.用振动样品磁强计(VSM)测量了Fe3O4空心微球的室温磁性,发现其表现为铁磁性.     

Bi4Ti3O12/BiOBr复合材料的溶剂热合成及可见光催化性能

采用一步溶剂热法合成了Bi4Ti3O12/BiOBr复合光催化剂,采用X-射线衍射仪(XRD)、扫描电子显微镜(SEM)、比表面积及孔径测定仪(BET)以及紫外可见漫反射光谱仪(DRS)等对样品的组成、形貌及可见光催化性能等进行了表征,讨论了合成条件对样品光催化活性的影响,探究了光催化反应过程中的活性物种及反应机理.研究结果表明,Bi、Ti、Br的投料比为10∶7∶5、乙二醇为溶剂、聚乙烯吡咯烷酮为表面活性剂且加入量为0.2g时,合成样品具有较高的光催化活性和较好的循环稳定性.在7 W LED灯照射140 min后,光催化剂对罗丹明B(RhB)的降解率达到85.1;.·O2-与h+在降解过程中起主要作用.     

微波合成Bi2S3/g-C3N4复合光催化剂及其光催化性能研究

采用微波合成法制备了Bi2 S3/g-C3 N4复合光催化剂,利用X射线衍射(XRD)、傅里叶红外光谱(FT-IR)、X射线光电子能谱(XPS)、紫外可见-漫反射吸收光谱(Uv-vis)、物理吸附仪(BET)等对其进行了表征,以罗丹明B(RhB)为目标化合物对其光催化性能进行了评价.结果表明,与纯Bi2 S3和g-C3 N4相比,复合样品的禁带宽度变小,比表面积增大,光生载流子的复合效率降低,显著提高了其光催化降解RhB的效率.复合样品5-CNBS对RhB的降解率达99;以上,分别是纯g-C3 N4和Bi2 S3单体对RhB降解效率的1.59倍和4.95倍.     

水热法制备类花状MoS2纳米纸微球

采用水热合成技术,以钼酸钠、硫脲为反应剂,草酸为助还原剂,去离子水为溶剂,合成了类花状结构的MoS2纳米纸微球,采用X射线衍射仪(XRD)、拉曼光谱、透射电镜(HRTEM)、扫描电子显微镜(SEM)和X射线能量色散谱(EDS)对样品的结构、形貌和成分进行分析,重点研究了草酸浓度对MoS2纳米纸微球的形貌和结构的影响规律.结果表明:在适当的反应剂浓度下,合成的MoS2是由大量厚度约30 nm左右的纳米纸花瓣聚集在一起形成的类花状微球组成的.MoS2微球具有2H型六方晶系结构,而每片纳米纸花瓣是单晶结构的层状MoS2.反应前驱液中草酸的浓度对微球的大小、形貌和结晶度有显著的影响.最后讨论了类花状结构的MoS2纳米纸微球的生长机理.     

TiO2/ZnO复合微球的制备及其光催化性能研究

以碳微球为模板,采用溶胶凝胶法、水热法等方法分别制备了TiO2微球、ZnO微球和TiO2/ZnO复合微球,采用扫描电子显微镜、X-射线衍射仪等对样品进行了表征,结果表明:制备的TiO2微球、ZnO微球和TiO2/ZnO复合微球,各微球直径在5 ～ 10 μm之间.在紫外光和可见光下研究了制备的光催化剂对亚甲基蓝溶液和湖水的光催化性能,光催化实验表明:三种微球中TiO2/ZnO复合微球具有良好的光催化性能.     

不同钙源种类对CaTi2O5粒子的光催化性能影响

采用溶剂热法制备了CaTi2O5微纳结构.用X射线衍射(XRD)、扫描电子显微镜(SEM)和比表面积分析仪(BET)对样品进行了表征,并用紫外-可见吸收光度计分析样品对光的吸收特性,研究不同钙源种类对CaTi2O5样品的物相、微观形貌及光催化性能的影响.结果表明:CaTi2O5样品更有利于降解甲基橙溶液.钙源为CaCl2所制备的CaTi2O5样品的结晶度高、颗粒大小均匀,具有低的反射率和高的吸收率,高的比表面积(112.34 m2·g-1),因此样品呈现出较高的光催化性能.     

CdS/沸石分子筛复合光催化剂的制备及光催化性能

以煤矸石为原料,经Na2CO3碱熔活化和水热合成获得了沸石分子筛;利用Cd2+对沸石分子筛进行离子交换并通过沉淀过程制得了CdS/沸石分子筛复合粉体.采用X射线粉末衍射(XRD)和扫描电子显微镜(SEM)对所得样品进行表征,并以模拟太阳光为光源,罗丹明B (RhB)为目标降解物,对其光催化活性进行了研究.结果显示:沸石分子筛上负载的CdS的晶相为立方相,制得的CdS/沸石分子筛复合粉体具有较好的光催化活性,且三次循环利用后仍具有较好的催化活性,在模拟太阳光辐照下,CdS/zeolite(0.5 M)复合粉体重复利用3次后,处理260 min对RhB的降解率仍可达91.3;.所得粉体对RhB的光催化过程符合一级动力学方程式,光催化过程中,RhB 紫外可见光谱的蓝移现象揭示所得CdS/沸石分子筛可通过脱乙基-共轭显色基团断裂途径降解RhB.     

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).     

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.     

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.