g-C3N4/ZnO复合材料的制备及其光催化性能分析

以尿素和乙酸锌为前驱体,采用水热法制得不同ZnO含量的光催化复合材料石墨相氮化碳/氧化锌(g-C3N4/ZnO),采用TEM、XRD、UV-Vis、FT-IR、PL等分析方法对所得催化剂进行了表征和分析.结果表明,ZnO颗粒附着于多孔片层状的g-C3N4之上形成g-C3N4/ZnO复合材料,降低了g-C3N4的禁带宽度,增加了g-C3 N4对可见光的吸收,以及光生电子-空穴对的分离几率.以可见光驱动亚甲基蓝的降解实验为探针反应检测催化剂的光催化性能,结果表明,质量比为3∶2的g-C3N4/ZnO复合材料表现最优光催化性能,其可在120 min内降解92;的亚甲基蓝,其光催化降解速率为g-C3N4单体的2.8倍.     

g-C3N4/ZnO复合光催化剂的制备及其光催化活性

以硝酸锌、三聚氰胺、氢氧化钠为原料,采用回流法合成g-C3N4/ZnO复合光催化剂.利用傅里叶红外光谱(FTIR),X射线衍射(XRD),扫描电子显微镜(SEM),紫外可见漫反射光谱(UV-Vis DRS)及N2吸附-脱附(BET)等技术对所合成样品的组成和形貌进行表征.在模拟太阳光条件下,以亚甲基蓝为模拟污染物评价催化剂的活性.结果表明,g-C3N4加入量为5wt;,煅烧温度500℃,煅烧时间2 h条件下制备的复合光催化剂具有最佳的光催化活性.5wt;g-C3N4/ZnO复合光催化剂在反应40 min时对亚甲基蓝的降解率可达到98.5;,其光催化降解速率为纯ZnO的2.8倍.     

一步法合成ZnO/BiVO4复合光催化剂及其光催化性能研究

以硝酸锌、硝酸铋、偏钒酸铵等为主要原料,采用水热法一步合成ZnO/BiVO4复合光催化剂,研究了ZnO复合量对合成产物性能的影响,利用X射线衍射(XRD)、扫描电子显微镜(SEM)、紫外-可见分光光度计等分析测试手段对样品的组成、形貌和光吸收特性进行表征.以亚甲蓝的脱色降解为模式反应,考察了样品的光催化性能.结果表明:ZnO的复合对产物的组成和形貌影响显著,与纯BiVO4相比,ZnO/BiVO4复合光催化剂的光催化性能有所提高.当ZnO的复合量为5;(质量百分比,下同)时,产物的光催化性能最佳,在高压汞灯照射240 min条件下,对亚甲蓝的降解率达87.4;,而同条件下纯BiVO4对亚甲蓝的降解率为82.2;.     

水热法合成ZnO/BiVO4复合光催化剂及其光催化性能

采用水热法制备ZnO/BiVO4复合光催化剂,研究了ZnO复合方式(直接和原位)对合成ZnO/BiVO4光催化剂性能的影响.利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、BET、紫外-可见分光光度计等检测手段对产物的晶体结构、微观形貌、比表面积和光吸收特性进行了表征.结果表明:ZnO的复合对产物的组成及形貌均有影响,复合产物中有V2 O5、Bi2 O3生成,但仍以单斜BiVO4为主.与纯BiVO4相比,复合后的BiVO4结晶度变差、粒度变小,但光催化性能提高.采用直接复合法制备的ZnO/BiVO4光催化性能提高更明显,在高压汞灯照射240 min时,亚甲蓝的降解率达90.4;,相同条件下纯BiVO4对亚甲蓝的降解率仅为82.2;.     

Fe掺杂对改善g-C3N4结构提升光催化活性的影响

石墨相氮化碳已经成为光催化领域、特别是光催化材料领域的研究热点.本文以尿素为原料,引入少量的硝酸铁改性,制备了不同含量的Fe掺杂的g-C3N4催化剂.采用SEM、XRD、IR、XPS、UV-Vis、PL等手段对催化剂样品表征.结果表明,Fe的掺杂有利于g-C3N4的剥离,影响了g-C3N4的能带结构,增强了其对可见光的吸收,提高电子-空穴对的分离效率.并以罗丹明B水溶液模拟废水,在可见光下考察催化剂的光催化降解性能,发现当Fe掺杂量为0.3;时效果最佳,降解速率是g-C3N4的1.62倍,且研究发现超氧自由基与空穴是该体系下的主要活性物种.     

蔗糖辅助水热合成BiVO4及其光催化性能研究

以硝酸铋、偏钒酸铵为主要原料,蔗糖为辅助剂,采用水热法合成单斜相BiVO4.主要研究了蔗糖及其用量对合成产物性能的影响.借助XRD、SEM、紫外-可见分光光度计对合成产物的物相组成、微观形貌及光催化性能进行表征.结果表明:在水热合成过程中,蔗糖的添加对BiVO4的合成有抑制作用.在后期热处理中,蔗糖的加入可以提高产物的结晶质量.光催化降解亚甲蓝结果表明,当蔗糖添加量为60mol;时,合成产物的光催化性能达到最佳,在高压汞灯照射180 min时,亚甲蓝的降解率达95.5;,比同条件下纯BiVO4对亚甲蓝的降解率提高近40;.     

金属镍掺杂g-C3N4的制备及其光降解性能

采用浸渍法制备不同掺杂量的负载型光催化剂Ni/g-C3N4,并考察其在可见光照下对亚甲基蓝的光降解性能.利用XRD、FT-IR、SEM、TEM、XPS、N2-sorption和ICP-OES等手段表征Ni/g-C3N4样品.研究表明,Ni/g-C3N4催化剂的光催化活性随着金属镍粒子掺杂量的增加而增大,随着亚甲基蓝浓度的增大而减小,其中金属镍掺杂量4.0wt;的样品4-Ni/g-C3N4表现出优异的光催化活性和光降解稳定性.这是由于4-Ni/g-C3N4样品的光降解过程中产生了超氧自由基、羟基自由基和空穴等活性物质,其中超氧自由基起主导作用.金属Ni0离子在光生电子作用下生成Ni2+,O2分子得到电子生成O2·-自由基.这些活性物质的产生有助于光生电子-空穴对的分离和抑制其复合速率,从而实现可见光下高效催化降解亚甲基蓝.     

Z机制光催化三元复合材料RGO/WO3/g-C3N4结构及光催化性能

以一步水热法合成了还原氧化石墨烯/三氧化钨/石墨相氮化碳(RGO/WO3/g-C3 N4)三元光催化复合材料,并对其结构、形貌及光电性能进行了表征.以罗丹明B(RhB)和盐酸四环素(TC-HCl)为降解目标物,评价了三元复合材料的光催化性能.基于自由基捕获实验和光催化反应结果分析了三元复合材料的光催化机制.结果表明:三元光催化复合材料中,三种物质紧密接触形成异质结构,与WO3和g-C3 N4单体及其二元复合材料相比,其可见吸收光谱有明显的红移,具有更低的光致发光光谱强度.复合材料有效的改善了电子-空穴对的复合,具有很好的光催化活性,最优配比组成的样品为0.2;RGO/WO3/g-C3 N4,光照240 min后,对RhB降解效果高达97.58;,其光催化效果优于WO3、g-C3 N4、RGO/g-C3 N4和WO3/g-C3 N4.催化降解过程中的主要活性物种是·O2-,其次是h+、·OH,反应过程中半导体的电子转移机制符合Z机制.     

La3+,Al3+共掺杂纳米ZnO光催化降解活性艳蓝X-BR研究

采用溶胶-凝胶法制备了不掺杂和掺杂铝离子、镧离子以及两种离子共掺杂的ZnO,并用X射线衍射(XRD),高分辨透射电镜(HRTEM),紫外-可见(UV-Vis)吸收光谱对其进行了表征.用紫外灯作为光源,一定浓度的活性艳蓝X-BR溶液为光催化反应模型污染物,研究了各种离子掺杂ZnO的光催化性能,考察了掺杂量对降解率的影响.结果表明,镧离子和铝离子掺杂浓度为2 at;和3 at;的共搀杂ZnO的光催化性能最好;在室温下,加入催化剂浓度为0.1 g/L,降解时间为45 min时,对活性艳蓝X-BR溶液的降解率达到96.63;.     

氰基修饰的g-C3 N4制备及光催化产氢性能

通过简单的醋酸钠与g-C3 N4前驱体三聚氰胺共混直接在空气气氛下烧制成功制备出氰基修饰的g-C3 N4.采用XRD、SEM、FT-IR、XPS、UV-Vis、PL和EIS对所得催化剂的物相结构、形貌和光学性能进行了表征.合成的氰基修饰的g-C3N4有着高效的光催化产氢性能,比原始g-C3N4的光催化产氢性能最高提高4.5倍(λ≥420 nm),归固于氰基增强了光生电子和空穴的分离能力.另外,氰基修饰的g-C3 N4在循环光催化产氢过程中展现了良好的光催化稳定性.     

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.