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.     

不同生长方向的GaN纳米线的可控制备与性能表征

采用化学气相沉积法,通过改变催化剂和衬底,以Ga2 O3和GaN的混合粉末为镓源制备出了不同生长方向的GaN纳米线,制备的平躺于衬底的GaN纳米线的直径约为60 nm,长度为10 μm到30 μm之间.垂直于衬底的GaN纳米线阵列的直径约为300 nm,长度约为5μm.使用扫描电子显微镜(SEM)、X射线衍射(XRD)、光致发光谱(PL)和透射电子显微镜(TEM)对样品进行了分析表征,结果表明所得样品为六方纤锌矿结构的GaN单晶纳米线.通过改变催化剂和衬底等生长条件,研究了衬底和催化剂对纳米线生长方向的影响,为以后的大量制备以及纳米器件的制作提供了依据.     

纳米非晶碳薄膜的制备及其场致电子发射特性

采用微波等离子体增强化学气相沉积(MPECVD)法,在涂有FeCl3的硅衬底上制备出了纳米非晶碳薄膜.通 过SEM、XRD和拉曼光谱分析了薄膜材料的形貌和结构.并研究了薄膜材料的场发射特性.结果表明:薄膜的开启电场仅为0.39 V/μm;当电场强度为1.85 V/μm时,电流密度高达3.06 mA/cm2;且场发射点均匀、密集、稳定.迭代法计算表明薄膜材料的功函数为3.1 eV,发射点密度约为1.7×105个/cm2.这些均表明该薄膜是一种性能优良的场发射阴极材料.     

无电镀沉积于硅衬底上铜纳米晶的场发射性能

采用无电镀沉积技术在经过机械抛光的单晶硅衬底上沉积了铜纳米晶.利用X射线衍射数据,估算出所沉积铜纳米晶的平均粒径大约为40nm.对120s无电镀沉积样品的场发射测试表明,该样品的开启场强为～5.5V/μm,在场强达到9.26V/μm时的场发射电流密度可达到62.5μA/cm2.对相应的沉积过程和场发射机理进行了分析.结果表明,无电镀沉积技术有可能成为制备具有较好场发射性能的金属/硅冷阴极的一种可供选择的方法.     

ZnO纳米线/纳米棒混合阵列的制备及其光致发光性能研究

使用无催化剂热蒸发法,在ZnO/Si薄膜衬底上制备了ZnO纳米线/纳米棒混合阵列.其中,纳米线的直径为10～20nm,纳米棒的直径为60～160 nn,二者混合在一起垂直生长于衬底表面.从衬底的上游到下游位置,混合,阵列中纳米线的含量逐渐下降,纳米棒逐渐增多.室温光致发光测试发现尺寸较小的纳米线阵列的紫外光发光强度比大尺寸纳米棒阵列高约5倍.持续激发光照射下,纳米线阵列的发光强度逐渐上升,停止光照后又逐渐下降到初始值,这可以用纳米线表面O2分子的解吸附和吸附过程来理解.     

TiO2纳米花的合成及其在染料敏化太阳能电池中的应用

采用水热合成技术,以盐酸、去离子水和钛酸丁酯为反应前驱物,在透明导电玻璃(FTO)衬底上合成TiO2纳米花薄膜.采用扫描电子显微镜(SEM)、高分辨透射电镜(HRTEM)和X射线衍射(XRD)对其形貌和结构进行了分析.结果表明在FTO衬底上形成的纳米花是由四方形柱状结构的纳米棒构成的,纳米棒由具有金红石晶型的直径为4~6 nm的几十条单晶纳米线束聚集在一起构成的.研究了以TiO2纳米花薄膜为光阳极制备的染料敏化太阳能电池的光电性能,电池的开路电压、短路电流密度和转换效率均随着反应前驱物中钛酸丁酯的浓度的增加而变小,这是由于纳米花的比表面积随着钛酸丁酯的浓度增加而减少造成的.     

纳米石墨和纳米碳管薄膜在低电场下的稳定场发射

采用微波等离子体化学气相沉积法(MPECVD)制备出了纳米石墨和纳米碳管混合薄膜材料.通过扫描电镜(SEM)和拉曼光谱(Raman)对薄膜材料的结构和形貌进行了分析.研究了薄膜材料的场发射性能.场发射结果显示:其开启电场为0.7 V/μm1,在较低电场下(3.7 V/μm1)即可获得5.2 mA/cm2的电流密度,此电场下发射点密度可达1.6×107 cm-2,发射点均匀,亮度稳定.迭代法计算结果表明制备的纳米石墨和纳米碳管混合薄膜材料的功函数仅为3.2 eV.这些表明该薄膜材料为优良的场发射冷阴极材料.     

电化学沉淀法制备纳米结构氧化锌的场发射特性

对电化学沉淀法制备的氧化锌纳米棒阵列,通过室温下真空场发射电流密度与外加电压关系的测量,研究其场发射特性.根据测量数据,基于 Fowler-Nordheim 方程,估算了样品场发射效应的增强因子,观察到其取值随外加电压变化具有反常的两阶段性,即当外电场强度在3.3 V/μm 场发射开启值到4.3 V/μm之间时,增强因子值为1339,外加场强大于4.3V/μm 时,增强因子锐减至296;结合样品的光致发光谱和能量散射谱,应用半导体中强电场效应、掺杂半导体中温度对费米能级、载流子浓度和迁移率影响,通过场发射电流密度测量系统的串联电路等效,分析了样品缺陷态对此两阶段性的决定和影响.     

无催化两步蒸镀法制备二氧化钛纳米线

采用一种无催化、两步蒸镀的方法在石英片上生长TiO2纳米线.此方法通过高温蒸发Ti粉,沉积一层高活性的种子层,再低温通入氧气对种子层氧化形成TiO2纳米线.运用扫描电子显微镜、透射电子显微镜、激光拉曼光谱技术等表征了生长TiO2纳米线薄膜的形貌和结构.结果表明:纳米线的直径为10 ～ 50 nm,长度为1～2 μm,随着第二次蒸镀温度的增加,二氧化钛纳米线晶相从锐钛矿转变成金红石相,其相变温度点在800℃附近.最后讨论了在无催化两步蒸镀法中TiO2纳米线的生长机理.     

水热法制备Sb2Se3纳米线及其光响应性能研究

采用简单的水热方法成功合成出分散性良好、尺寸均一的Sb2Se3纳米线.研究表明,所合成出的Sb2 Se3纳米线直径约20 ～ 30 nm,长度达30 μm.与此同时,讨论了如乙二胺的浓度、反应时间和形成机制等很多反应参数.还详细研究了Sb2Se3的光响应性能.     

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 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.