离子液体辅助合成Fe3O4纳米粒子及其性能研究

采用离子液体1-丁基-3-甲基咪唑双(三氟甲烷磺酰)亚胺盐([Bmim][TFSI])辅助合成了Fe3O4纳米粒子,研究了其磁、电化学方面的性能,并利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)等对样品进行了表征.实验结果表明:以该离子液体为稳定剂合成的Fe3O4纳米粒子平均直径约为20 nm,且形貌均一,在室温下表现出超顺磁性,饱和磁化强度为68.13 emu/g.将所得Fe3O4纳米粒子应用于锂离子电池负极材料,在电流密度为0.1 A/g条件下,首次充放电比容量分别高达1025 mAh/g和1428 mAh/g.     

离子液体对硫化镉粒径和光催化性能调控研究

以氯化镉和硫代乙酰胺为原料,分别以水,离子液以及两者的混合液为溶剂,用超声法成功合成了不同粒径的硫化镉纳米粒子.用XRD,SEM,IR以及UV-Vis等手段对所制备样品的晶型、形貌和光学特性进行了表征;以紫外光为光源、甲基橙为目标降解物评价了硫化镉纳米粒子的光催化活性.结果表明,离子液的引入使硫化镉纳米粒子的粒径明显变小,带隙能量变大,光催化性能测试表明,离子液介质中合成的CdS纳米粒子具有更高的光催化活性.离子液体对比实验还表明,三乙烯四胺型离子液体中合成的硫化镉具有更高的光催化活性.     

离子液体[Bmim]BF4辅助制备超顺磁性Fe3O4纳米粒子

以七水硫酸亚铁(FeSO4·7H2O)与六水三氯化铁(FeCl3·6H2O)为原料,离子液体1-丁基-3-甲基咪唑四氟硼酸盐([Bmim] BF4)为添加剂,70℃下反应2h制备了Fe3O4纳米粒子.通过X射线衍射仪(XRD)、傅里叶红外光谱(FT-IR)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)以及热重分析(TG)等方法对样品的结构和形貌进行表征,并测试了所合成样品的磁性能.实验结果表明:离子液体辅助制备的Fe3O4纳米粒子形貌较为均一,呈近似球状,平均直径约为14 nm,产品在室温下表现出超顺磁性,饱和磁化强度为60.66 emu/g.利用密度泛函理论(DFT)计算模拟了Fe3O4分别与离子液体和水相互作用的电子结构,发现离子液体通过阴离子的桥联,更易吸附在Fe3O4晶粒表面.     

长径比可控的CdS纳米棒制备及光催化性能研究

采用溶剂热法制备了长径比可控的纤锌矿CdS纳米棒;以3CdSO4·8H2O、CH4 N2S为原料在180℃、24 h溶剂热反应条件下,通过改变Cd/S物质的量比和保温时间等因素来调节CdS纳米棒的长径比.利用扫描电镜(SEM)、X射线衍射(XRD)、紫外可见吸收光谱(UV-Vis)、光催化分别对其形貌、结构和光催化性能进行了表征和分析.结果表明:Cd/S摩尔比对CdS棒的生长起到关键作用,随着镉硫比的减小,CdS纳米棒的长径比逐渐增大.当Cd/S摩尔比为1∶6时,制备的CdS为长径比较大且表面光滑的纳米棒,纳米棒的尺寸大约为长800 nm、直径70nm.通过降解亚甲基蓝溶液测试了CdS纳米材料的可见光照射下的光催化性能,结果表明具有大长径比的CdS纳米棒表现出优异的光催化活性.     

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.     

光敏化La2O3/TiO2催化剂的制备及其光催化性能研究

采用溶胶-凝胶法和水热法制备了La2O3/Ti O2复合物,将此种La2O3/Ti O2复合物利用叶绿素提取液浸泡后,制得了光敏化La2O3/Ti O2复合物,并采用透射电子显微镜、X-射线衍射仪、比表面积测定仪和紫外-可见分光光度计等对样品进行了表征。结果表明:La2O3/Ti O2催化剂的颗粒粒径在3~10 nm之间,BET比表面积为173.53 m2/g,光敏化La2O3/Ti O2复合物具有较好的可见光响应性能。在可见光下研究了几种光催化剂对水中六价铬离子的光催化还原效果,光催化结果表明:以光敏化La2O3/Ti O2复合物为催化剂,在可见光下光催化还原含Cr6+废水180 min后,Cr6+脱除率达到78.7%。     

可磁分离TiO2/BiOI复合纤维的制备及光催化性能

本工作合成了一种可磁分离TiO2/BiOI复合纳米纤维(TiO2/Fe3O4/BiOI),并研究了其可见光催化性能.通过静电纺丝技术获得TiO2纳米纤维,采用溶剂热法在TiO2纳米纤维表面生长Fe3 O4纳米颗粒,最后,在磁场辅助下,通过连续离子吸附反应(SILAR)法在TiO2/Fe3O4表面生长了BiOI纳米片.结果表明,Fe3O4纳米颗粒直径均一,均匀分布在TiO2纳米纤维表面.BiOI纳米片呈交错状垂直沉积在TiO2纳米纤维表面,BiOI纳米片的负载量可以通过SILAR的循环次数控制.光催化测试表明,由于BiOI对可见光吸收的增加,以及与TiO2间形成的半导体异质结,TiO2/Fe3 O4/BiOI复合纳米纤维的光催化效率均高于TiO2/Fe3 O4纳米纤维.此外,TiO2/Fe3 O4/BiOI对外磁场有强的响应,易于进行磁分离回收.     

Fe3O4/LDHs复合结构的制备及吸附性能研究

分别采用两种方式(一步合成法和二步合成法)在Fe3O4表面生长层状双金属氢氧化物(LDHs),得到了Fe3O4/LDHs复合材料.利用X-射线衍射、电子显微分析、红外光谱和交变梯度磁强计等测试方法研究了LDHs和Fe3O4的复合方式对复合材料形貌、粒径、结晶性、磁性能和吸附性能的影响.同时对比分析了LDHs和Fe3O4/LDHs复合材料对Cr(Ⅵ)离子的平衡吸附规律.结果表明,采用一步合成法制备的Fe3O4/LDHs复合材料具有良好的磁性能和吸附性能.     

常压干燥法制备铁掺杂二氧化钛气凝胶

以钛酸四丁酯(TRIP)为原料、硝酸铁为掺杂剂、冰醋酸为催化剂、甲酰胺为干燥控制化学添加剂,采用溶胶-凝胶法制备Fe3+掺杂TiO2醇凝胶,并结合常压干燥工艺,实现了Fe3+掺杂TiO2气凝胶的常压干燥法制备.采用XRD、BET、SEM、IR等对样品进行检测.结果表明:制备态Fe3+掺杂TiO2气凝胶密度为0.24 g/cm3,比表面积为529.17 m2/g,平均孔径约为20.10 nm,晶型为无定形;经850℃空气气氛下煅烧2h后,样品转变为锐钛矿型结构,平均孔径增大到22.32 nm,比表面积为136.22 m2/g.通过甲基橙溶液光催化降解实验,相比未掺杂二氧化钛气凝胶,掺入nFe∶nTi=0.05时,样品具有更高的光催化性能.     

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.     

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.