枝状ZnO-TiO2复合纳米棒阵列的制备及表征

采用化学水浴沉积法,在预制晶种层的基底上得到垂直底面生长的有序ZnO纳米棒阵列,再用反应磁控溅射方法,沉积制备ZnO-TiO2复合结构的纳米棒阵列.利用X射线衍射(XRD)和扫描电子显微镜(SEM)对制备得到的样品进行结构和形貌表征,研究了晶种层、水浴生长液浓度和磁控溅射氧氩比对复合纳米阵列的影响.制备得到了具有TiO2分枝的复合纳米棒阵列,并初步探讨了TiO2分枝的形成机理,为制备基于复合纳米棒阵列的器件提供了条件.     

ZnO/TiO2复合光阳极染料敏化太阳能电池的研究

采用醇热法制备ZnO纳米粉体,采用水热法制备TiO2纳米粉体,将不同质量分数的ZnO与TiO2混合制备浆料,采用刮涂法在掺氟的SnO2透明导电玻璃(FTO)上制备ZnO/TiO2纳米复合薄膜光阳极,与Pt对电极和电解质组装成染料敏化太阳能电池.采用X射线衍射仪(XRD)、X射线光电子能谱仪(XPS)和扫描电镜(SEM)对所制备的样品进行表征,通过光电性能测试和电化学阻抗谱测试,研究了添加不同质量分数的ZnO对电池性能的影响.结果表明:不添加ZnO纳米粉时,纯TiO2光阳极的电池光电转换效率为7.95;,而添加了2wt; ZnO的ZnO/TiO2复合光阳极电池的效率达到9.54;,比纯TiO2电池的效率提高了20;.     

TiO2纳米棒复合结构光阳极的制备及其在染料敏化太阳电池中的应用

通过水热法制备了垂直于导电基底的金红石纳米棒阵列,首次通过磁控溅射方法制备了一维阵列金红石/锐钛矿核壳结构,并将其应用于染料敏化太阳能电池(dye-sensitized solar cells,DSSCs).样品结构和形貌分别利用X射线衍射仪、透射电镜、扫描电子显微镜进行表征观察.结果表明,磁控溅射法制备的复合结构光阳极具有更好的形貌和比表面积.光电转换性能测试表明,与单纯水热生长的金红石纳米棒光阳极相比(1.10;),磁控溅射法制备的复合结构光阳极具有更高的光电转换效率(2.85;),光电转换效率提高了将近2.6倍.     

ZnO/Fe2O3复合结构的制备及光电化学性能研究

采用水热法在FTO导电玻璃上制备出大面积高能面裸露的ZnO纳米片阵列.采用旋涂法在纳米片表面制备Fe2O3纳米颗粒形成ZnO/Fe2O3复合结构.利用X射线衍射(XRD)、扫描电子显微镜(SEM)、紫外-可见光吸收光谱和三电极光电测试系统对复合薄膜的结构组成、形貌、光学性能和光电化学性质进行了表征和分析.研究结果表明,随着Fe2O3复合次数的增加薄膜的光吸收范围逐步拓宽到可见光区,ZnO/Fe2O3复合结构光电极的光电流明显高于单纯的ZnO纳米片阵列光电极.     

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.     

TiO2有序分级结构的制备条件对其形貌和光电转换性能的影响

采用水热法,在钛箔表面成功制备出TiO2纳米线-纳米粒子分级结构光阳极.利用XRD、SEM等表征方法系统研究了制备条件对TiO2有序分级结构物相和微观形貌的影响,讨论了TiO2纳米结构和其光电转换性能之间的关系.结果表明:由于二次水热反应将初级TiO2纳米线阵列转变为纳米线-纳米粒子分级结构,使其比表面积和光电转换性明显提高.然而晶体生长时间过长或水热反应前驱液的浓度较高,都使得生长的纳米结构相互团聚在一起,从而减少其比表面积,降低光电转换性能.最佳的条件是第一步水热反应时间10 h,草酸钛钾溶液浓度0.0075mol/L,第二步水热反应时间6h,TiC14处理液浓度0.05 mol/L,分级结构的光电转换效率达到2.01;.     

不同基底对电沉积制备ZnO纳米棒薄膜 光电转换性能的影响

选取不同的导电支撑物(FTO、ITO、不锈钢网、Ni网)作为基底,在其表面采用相同的电沉积参数制备得到ZnO纳米棒薄膜,详细探讨了不同基底物理化学性质对ZnO基光阳极形貌及光电性能的影响.研究表明:以ZnCl2与O2为前驱体,分别在未做预处理的空白FTO、ITO、Ni网、不锈钢网上施加-1.0 V的沉积电位,反应3600 s后均可得到棒状结构的ZnO纳米薄膜,但纳米棒的直径、密度以及结晶性相差较大.经紫外漫反射测试发现,虽然各基底上ZnO纳米薄膜对太阳光的响应范围相一致,但玻璃基底相较于柔性金属网基底具有较小的禁带宽度,电子跃迁所需能量较小.此外,I-V测试结果表明基于玻璃基底的ZnO基DSSC相较于柔性金属丝网基光阳极具有较大的光电转化效率,最高可达0.38;.     

钇掺杂多孔结构氧化锌纳米棒的制备与性能研究

采用两步法在二氧化锡掺氟(SnO2:F,FTO)导电玻璃基板上制备出钇(Y)掺杂多孔结构氧化锌(ZnO)纳米棒,首先利用浸渍-提拉法在FTO导电玻璃基板上制备ZnO晶种层,然后利用水热法在ZnO晶种层上生长Y掺杂ZnO纳米棒.研究了不同浓度Y掺杂ZnO纳米棒的晶相结构、微观形貌、化学组成及光学性能.实验结果表明:所制备的Y掺杂ZnO纳米棒为沿c轴择优取向生长的六方纤锌矿结构,随着Y掺杂浓度的增加,ZnO纳米棒(002)衍射峰强度先增大后减小,纳米棒的平均长度由1.3μm增加到2.6μm.ZnO纳米棒的形貌由锥状结构向柱状结构演化,纳米棒侧面的孔洞分布密度增加.所制备的Y掺杂ZnO纳米棒具有一个较弱的紫外发光峰和一个较强的宽可见发光峰.所制备样品的光学带隙随着Y掺杂浓度的增加而减小,其光学带隙在3.29～3.21 eV之间变化.利用Y掺杂ZnO纳米棒作为量子点敏化太阳能电池的光阳极可极大提高太阳电池的光电转换效率.     

CdS/TiO2纳米管阵列的制备及光催化性能

采用阳极氧化法在纯钛箔上制备出TiO2纳米管阵列,再通过化学水浴沉积法在TiO2纳米管阵列上负载CdS纳米颗粒.利用XRD、FESEM和UV-Vis分光光度计对样品的晶体结构、微观形貌和光学性质进行表征,并研究了不同含量CdS负载的复合薄膜对光催化降解气相苯性能的影响.结果表明,CdS纳米颗粒均匀沉积到TiO2纳米管阵列上,所制备的复合薄膜光吸收带边均扩展到了可见光区.CdS的修饰大幅度提高了TiO2纳米管阵列对气相苯的光催化降解活性,其中负载CdS质量分数为3;的TiO2纳米管阵列光催化活性最佳,80 min内对气相苯的去除率为80;,终产物CO2的浓度为640 mg/m3.     

籽晶辅助化学水浴沉积法制备ZnO纳米棒阵列

采用籽晶辅助化学水浴沉积法,即先用磁控溅射法在硅片上制备c轴取向的ZnO薄膜,以此作为籽晶层,利用化学水浴沉积法制备ZnO纳米棒阵列.利用扫描电子显微镜(SEM)和X射线衍射(XRD),研究了ZnO薄膜籽晶层的沉积温度、水浴温度和前驱体溶液中Zn源的初始浓度等对ZnO纳米棒阵列生长的影响,由此得到了结晶性好且几乎垂直于衬底方向的ZnO纳米棒阵列的生长条件,为制备基于ZnO纳米棒阵列的器件提供了条件.     

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 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.     

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.     

Synthesis of spinacine and spinacine derivatives: crystal and molecular structures of Nπ-hydroxymethyl spinacine and Nα-methyl spinaceamine

The natural amino acid L-Spinacine (4,5,6,7-tetrahydro-1H-imidazo[4,5-c]pyridine-6-carboxylic acid) has been synthesized following a new pathway which gives a chemically and optically pure product with an excellent yield. The crystal structures of a synthetic intermediate, N^π-hydroxymethyl-spinacine, and a spinacine derivative, N^α-methyl-spinaceamine, have been investigated through X-ray diffraction: Spi(πMeOH)·H₂O, monoclinicP2 _i,a=8.571(1),b=6.682(1),c=8.588(1) Å, and β=94.67(1)^o. Spm(αMe)·2HCl·H₂O, triclinicP l,a=7.492(4),b=10.799(3),c=7.040(2) Å, α=91.88(2), β=98.36(3) and γ=73.34(3)^o. Spi(πMeOH) crystallizes with a water molecule and displays a zwitterionic character. The carboxylate group is in equatorial position and forms a short electrostatic interaction of 2.618(2) Å between one of its oxygens and the protonated nitrogen of the tetrahydropyridine ring. The crystal packing is assured by strong O?H???O, O?H???N, N?H???N intermolecular hydrogen bonds and C?H???O close contacts. The biprotonated compounds Spm(αMe) crystallizes with two Cl^? anions and a water molecule. The positive charge on the imidazole ring is delocalized on the conjugated moiety N=C?N. The crystal is built up by clusters formed by two biprotonated Spm(αMe) molecules, four Cl^? anions and two water molecules linked together by hydrogen bonds.