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.     

三维分级花球结构Bi2WO6的制备及其光催化性能研究

以L-赖氨酸为模板剂,采用水热法成功制备出三维分级花球结构Bi2WO6光催化剂.采用X射线衍射(XRD)、扫描电镜(SEM)等测试方法对所制备样品进行了表征.研究了水热反应过中反应温度、时间及L-赖氨酸添加量等因素对样品形貌的影响,提出三维分级花球结构Bi2 WO6的可能形成机理.此外,以罗丹明B溶液为模拟染料废水,在模拟太阳光照射下考察了样品的光催化活性,结果表明:以L-赖氨酸为模板剂所制备的花球形Bi2WO6 (L-BWO)具有较高的光催化活性,与不添加模板剂情况下所制备的片状Bi2WO6 (BWO)相比,L-BWO光催化剂的降解效率约是BWO的1.5倍.     

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.     

多级孔TiO2/ZSM-5催化剂的孔道效应对 亚甲基蓝催化降解性能影响

以廉价凹凸棒石为原料,通过调控介孔模板剂聚乙二醇(PEG-1000)用量用水热合成法制得多级孔ZSM-5分子筛,并用溶胶-凝胶法制备了TiO2/ZSM-5光催化剂.通过FT-IR、XRD、SEM和N2吸附-脱附对多级孔TiO2/ZSM-5光催化剂的官能团、晶体结构、形貌和孔道特征进行表征,并对典型的亚甲基蓝印染废水进行光催化实验,考察模板剂用量和TiO2负载量对光催化剂孔道效应和催化性能的影响.结果表明:ZSM-5分子筛作为载体,其介孔体积与介孔模板剂PEG用量成正比,调节PEG用量可定向控制载体的孔道结构;TiO2负载量在一定程度上影响光催化效率和载体孔体积.当PEG为0.16 g,TiO2负载量为10;时,多级孔TiO2/ZSM-5具有良好光催化活性,光照40 min光催化降解率可达90;.     

三种改性方法对纳米ZnO催化剂粉体的光催化性能的影响

以SnCl4·5H2O、ZnNO3·6H2O、HCl、NaOH、FeCl3·6H2O为原料,采用共沉淀法制备Fe掺杂纳米ZnO、纳米ZnO/SnO2和Fe掺杂纳米ZnO/SnO2三种复合催化剂粉体,以降解甲基橙溶液反应为模型,研究了不同比例的ZnO/SnO2复合、Fe元素掺杂量以及SnO2复合Fe元素掺杂同时作用对纳米ZnO粉体光催化活性的影响,采用X射线衍射(XRD)测试方法对不同量Fe元素掺杂纳米ZnO粉体进行了表征.采用透射电镜对三种改性方法ZnO粉体进行表征.结果表明:随着ZnO/SnO2的物质的量比增加,ZnO/SnO2复合光催化剂的催化活性先增加,然后降低;随着Fe掺杂量的增加,纳米ZnO粉体的光催化活性先增加,然后降低.三种改性方法都能提高纳米ZnO粉体的光催化活性,其中Fe元素掺杂以及SnO2复合改性纳米ZnO粉体的光催化效果最好,物相为ZnO和SnO2,颗粒尺寸为15 ～20 nm,分散性好,比表面积为68.7m2/g.     

SnO2负载TiO2纳米管的制备与光催化活性

结合阳极氧化法和脉冲沉积法合成SnO2/TiO2纳米管光催化剂,实现了SnO2纳米颗粒在TiO2纳米管表面的均匀负载.利用场发射扫描电子显微镜(FE-SEM)、能谱仪(EDS)、X射线衍射仪(XRD)以及紫外-可见漫反射光谱(UV-Vis DRS)对样品进行表征,以甲基橙为模拟污染物,评价了纳米管的光催化活性.结果表明,SnO2/TiO2纳米管经750℃煅烧后主晶相为锐钛矿相TiO2,含少量金红石相TiO2和SnO2,三者两两之间形成三元异质结,促进光生电子-空穴对的分离,此时SnO2/TiO2纳米管表现出最佳的光催化活性,紫外光下对甲基橙1 h分解比例由32.4;提升至96.5;.     

水热法制备钛掺杂二氧化锡微球及其乙醇气敏性研究

以SnCl2·2H2O和TiCl4为原料,采用水热法制备钛掺杂SnO2微球.通过X射线衍射仪(XRD)、扫描电镜(SEM)和透射电镜(TEM)对材料的物相和形貌进行表征,并测试材料对乙醇的气敏性.结果表明,所得钛掺杂SnO2微球呈四方金红石结构,钛离子掺入并没有改变SnO2晶体结构,也无新晶相出现;由钛掺杂SnO2微球制得的气敏元件在工作温度350℃条件下,对乙醇有较高灵敏度,如对50 ppm乙醇的灵敏度为2.053,响应时间在10 s内,恢复时间也在3 min内;并对其气敏机理进行了进一步探讨.     

三维有序大孔TiO2/CeO2光催化剂的制备及性能研究

以自组装SiO2纳米球为模板,通过煅烧和模板刻蚀制备具有三维有序大孔结构的TiO2/CeO2复合光催化剂(3DOM TiO2/CeO2).用XRD、SEM、FT-IR、DRS、PC等手段对所制备的光催化剂进行表征,在模拟太阳光下,以罗丹明B为模型降解物,对样品的光催化活性进行测试.结果表明,3DOM TiO2/CeO2的光催化降解活性与TiO2/CeO2相比得到进一步提高,其原因可能是由于3DOM结构可以产生慢光子效应,提高了TiO2/CeO2复合光催化剂的光吸收能力,进而提高了TiO2/CeO2的光催化性能.     

超声辅助乙酸溶液球磨法制备SnO2纳米粉末

采用超声波辅助乙酸溶液球磨法制备了金红石型的SnO2纳米粉末.采用X射线衍射仪(XRD)、傅氏转换红外线光谱分析仪(FT-IR)、透射电镜(TEM)对反应产物进行表征,研究了不同液体介质(乙酸溶液、纯水、乙醇溶液)、乙酸浓度、超声波频率对合成SnO2纳米颗粒的影响.结果表明,当反应进行到21 h,SnO2已经完全形成.合成的SnO2纳米粒子的平均粒径为10 nm左右,并且粒子形态统一、尺寸均匀.合成的SnO2纳米颗粒具有良好的光催化性能.锡粉在乙酸溶液中球磨21 h可以合成SnO2,而在水和乙醇溶液中球磨40h,仍不能合成SnO2;乙酸浓度越高,合成SnO2的反应速率越快;超声波频率越低,在超声辅助乙酸溶液体系中的反应速度越快.     

CuO/SnO2/TiO2复合光催化剂的制备及光催化性能

采用硬脂酸法制备了CuO/SnO2/TiO2复合光催化剂,采用XRD及TG-DTA分析对其物相和热稳定性进行了表征,并通过苯酚的光催化降解行为对所制备催化剂的活性进行了评价.结果表明,经500 ℃热处理的CuO/SnO2/TiO2复合光催化剂属于单一的锐钛矿相,且铜、锡氧化物的引入抑制了TiO2的结晶和晶粒的生长.当催化剂组成为Cu:Sn:Ti=0.25:5:100(物质的量比),焙烧温度为500 ℃,催化剂投加量为0.5 g·L-1,溶液pH为4.0时,经3 h光催化反应苯酚的降解率达97.1;.     

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.