海洋防腐用氧化石墨烯/聚苯胺/二氧化钛的制备

以氧化石墨烯为模板,在酒石酸的存在下合成了水性氧化石墨烯/聚苯胺/二氧化钛复合材料.通过TEM、SEM、XRD和IR等设备对材料进行了表征,并采用光降解和电化学手段研究了复合材料的光催化和防腐性能.结果表明,酒石酸掺杂苯胺单体在氧化石墨烯纳米片层表面聚合获得氧化石墨烯/聚苯胺(G/P)层状结构,纳米二氧化钛均匀分散在G/P前躯体表面,形成水性氧化石墨烯/聚苯胺/二氧化钛(G/P/T)层状复合材料.罗丹明B光降解试验表明,复合材料具有良好的光降解效果,提高了金属材料耐生物腐蚀性能;G/P/T改性的环氧树脂则有效地改善了铝合金的腐蚀状况,将铝合金的自腐蚀电流从10-5 A/cm2降低至约10-11 A/cm2.     

石墨烯/聚苯胺复合材料的制备及超电容性能研究进展

近年来,石墨烯/聚苯胺复合材料由于自身优异的电化学性能引起了国内外学者的广泛关注,石墨烯具有大的比表面积和双电层电容特性,聚苯胺具有高赝电容特性,二者协同作用使其复合材料的超电容性能大大提高.主要介绍石墨烯/聚苯胺复合材料的制备方法及电容性能的影响因素,总结三维石墨烯/聚苯胺复合材料的构筑方法,并对复合材料未来在超级电容器领域的发展趋势进行了展望.     

高锰酸钾对石墨烯及石墨烯-CaTi2O4(OH)2复合材料电化学性能的影响

由于CaTi2O4(OH)2导电性较差,为进一步提升CaTi2O4(OH)2电化学性能,将具有优异导电性的石墨烯材料与之复合.采用C为原料,H2 SO4为插层剂,KMnO4为氧化剂还原制得石墨烯,将两者复合制备石墨烯-CaTi2 O4(OH)2复合材料.研究高锰酸钾用量对石墨烯-CaTi2O4(OH)2复合材料电化学性能的影响.利用X射线衍射(XRD)和扫描电子显微镜(SEM)对样品的显微结构、形貌进行检测分析,采用恒电流充放电(CP)和循环伏安(CV)等技术测试其电化学性能.实验结果表明:当高锰酸钾用量5 g时,可以制备出氧化、还原程度良好,电化学性能优异的石墨烯,与CaTi2O4(OH)2复合制得样品电极,其电化学性能最优,在5 A/g的工作电流密度下,样品比电容高达394.2 F·g-1是纯CaTi2O4(OH)2电容值(162 F·g-1)的2.43倍.     

电化学法制备石墨烯基复合材料及其在超级电容器中的研究进展

石墨烯及其复合材料作为一种新型功能材料在能量存储领域受到广泛的关注.电化学制备技术相比于其他的制备手段具有安全、高效、绿色的优点.本文综述了电化学法制备石墨烯/纳米金属复合材料、石墨烯/金属氧化物(氢氧化物)复合材料、石墨烯/聚合物复合材料等的研究进展及其在超级电容器上的应用,以期为电化学制备石墨烯及其复合材料在超电领域的研究提供参考.     

高性能Si-α-SiC-β-SiC复合涂层的研究

以硅粉、石墨粉为包埋原料及MgO、Al2O3和B2O3等为促渗剂,采用二次固渗工艺在C/C复合材料表面制备了Si-α-SiC-β-SiC复合涂层.并采用X射线衍射(XRD)和扫描电子显微镜(SEM)对复合涂层进行了表征.结果表明:一次固渗后的涂层为Si-β-SiC涂层, 两次固渗后可以获得致密的Si-α-SiC-β-SiC复合涂层,涂层厚约300μm,具有致密的表面和断面结构,没有开裂和孔隙等缺陷.氧化性能测试表明:在1500℃的静态空气气氛下氧化200h后,Si-α-SiC-β-SiC复合涂层能对C/C复合材料进行有效保护,涂层试样的失重仅为4.42×10-4g·cm-2.     

氧化石墨烯/二氧化硅复合材料的制备及其在吸附领域应用研究进展

近十年来,氧化石墨烯(GO)基复合材料日益引起研究者的广泛兴趣,而氧化石墨烯和二氧化硅的复合材料是其中的一个研究热点.本文介绍了氧化石墨烯/二氧化硅(GO/SiO2)复合材料的制备及其在吸附领域的应用.其制备方法包括非共价键法和共价键法,在非共价键法中,包括阳离子表面活性剂法和二氧化硅表面改性法;在共价键法中,包括形成酰胺键(-CO-NH-)、硅酯键(-COOSi-)、碳氧硅键(-C-O-Si-).吸附领域的应用包括对重金属离子、有机物的吸附.最后,我们对氧化石墨烯/二氧化硅复合材料将来的发展进行了展望.     

石墨烯/Fe2O3纳米复合材料的制备及其储锂性能研究

采用软化学方法控制氧化石墨表面含氧官能团的数量,一步完成了石墨烯/Fe2O3纳米复合材料的控制合成.采用XRD和Raman光谱分析及TEM表征复合材料的组成、结构和微观形貌特征,并对石墨烯/Fe2O3复合负极的电化学储锂性能进行了研究.结果表明,石墨烯/Fe2O3复合材料作为锂离子电池负极材料具有较高的储锂容量和倍率性能,充放电循环性能稳定.在100 mA/g的电流密度下循环100次,可逆容量为606 mAh/g,放电效率保持在91;;在2 A/g下放电容量是其在250 mA/g下放电容量的58.2;.     

硅藻土/TiO2/氧化石墨烯复合材料的制备及其光催化性能研究

本文以硅藻土为载体,硫酸氧钛为前驱体,在硅藻土表面原位水解形成二氧化钛纳米颗粒,后经氧化石墨烯修饰改性,得到硅藻土/TiO2/氧化石墨烯三元复合光催化材料.通过SEM、XRD、XPS、IR对样品的晶体结构、形貌及元素形态等进行了表征,研究了复合催化剂对罗丹明B溶液的光催化降解性能.结果表明,硅藻土/TiO2/氧化石墨烯三元复合材料在2 h的光降解率高达99;,比同时间的硅藻土/TiO2二元复合材料高出10;,比硅藻土高出73;,硅藻土作为载体有效的避免了二氧化钛颗粒的团聚,同时氧化石墨烯的高导电性能有效分离光生载流子,从而提高TiO2的光催化活性和反应效率.     

还原氧化石墨烯/MoS2与碳纳米管/MoS2作为润滑油添加剂的摩擦学性能研究

通过水热法成功制备出还原氧化石墨烯/MoS2(RGO/MoS2)与碳纳米管/MoS2(CNTs/MoS2)纳米复合材料,采用XRD,SEM以及TEM分别对纳米复合材料样品进行了分析和表征,结果表明所制备的复合材料中MoS2与还原氧化石墨烯、碳纳米管很好地结合在一起.用UMT-2多功能摩擦试验机测试其作为液体石蜡添加剂的摩擦磨损性能,并对其摩擦机理进行了分析.研究发现,与纯的MoS2相比,一定比例的RGO/MoS2纳米复合材料作为润滑油添加剂的摩擦系数降低了18;,相对磨损量减少55;;与碳纳米管增强的纳米复合材料相比,RGO/MoS2纳米复合材料具有更好的摩擦磨损性能.     

六方短棒状ZnO/氧化石墨烯复合材料的制备及其光催化性能

以乙酸锌为锌源,NaOH溶液作为沉淀剂,采用水热法结晶得到六方短棒状ZnO颗粒.再以化学氧化法制备的氧化石墨烯为改性剂,在ZnO颗粒合成过程中加入不同量的氧化石墨烯(GO)分散液.在水热条件下ZnO颗粒与氧化石墨烯片发生自组装形成ZnO/GO复合材料.通过X-射线衍射仪(XRD)、扫描电子显微镜(SEM)、傅里叶变换红外光谱(FT-IR)与紫外-可见漫反射光谱(DRS)对样品的物相组成、显微形貌、官能团特征及光学性质进行表征.在紫外光和可见光照条件下,分别研究了ZnO及不同GO含量的ZnO/GO复合材料对亚甲基蓝(MB)的光催化降解活性.结果表明:合成的ZnO为六方短棒状形貌,且GO的加入量对样品的形貌产生较大影响,同时GO可以有效促进光生电子和空穴的分离,所得ZnO/GO复合材料在紫外光光照条件下对MB具有良好的光催化降解性能,而在可见光光照下光催化活性很低,从而推测ZnO极性面与非极性面的暴露比例对复合样品的光响应范围及其光催化性能产生重要影响.     

CsI-LiCl共晶材料的坩埚下降法生长与闪烁性能研究

本文采用坩埚下降法,在真空密封的石英坩埚中成功生长出CsI-LiCl与CsI-LiCl:Na共晶闪烁体。通过扫描电子显微镜(SEM)观察晶体微结构表明该共晶中LiCl相与CsI相存在周期性的层状排列,CsI相的厚度在5 μm左右。共晶样品的X射线激发发射谱显示在CsI-LiCl和CsI-LiCl:Na共晶样品存在缺陷发光,在CsI-LiCl样品中还观察到了纯CsI的自陷激子(STE)发光。CsI-LiCl样品在α粒子激发下的多道能谱中观察到明显的全能峰,这一结果证明CsI-LiCl共晶可用于热中子探测的潜力。     

静电纺丝法制备CeO2微纳米纤维及其除氟性能

以聚丙烯腈(PAN)为载体,六水合硝酸铈[Ce(NO₃)₃·6H₂O]为原料,采用静电纺丝法制备了Ce(NO₃)₃/PAN纤维,在空气中热处理得到CeO₂微纳米纤维,通过XRD、BET和SEM对CeO₂微纳米纤维进行表征。采用静态吸附实验探讨了CeO₂微纳米纤维去除水溶液中氟离子的性能,考察了溶液pH值、初始氟离子浓度及共存阴离子等对吸附性能的影响。结果表明,pH=3时,CeO₂微纳米纤维对F^-的吸附性能最佳,CeO₂吸附量随着F^-浓度的增大呈上升趋势。CeO₂微纳米纤维对F^-的吸附等温线遵循Langmuir模型,二级动力学模型能很好地描述CeO₂微纳米纤维对F^-的吸附过程。CeO₂微纳米纤维的除氟性能优良,可为其实际应用提供理论参考。     

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 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.     

X-ray analysis of sideroxol from <Emphasis Type="Italic">Sideritis leptoclada</Emphasis>

Sideroxol (1), a kaurane diterpene which has the ent-7α,18-dihydroxy-15β,16β-epoxykaurane structure (MW = 320.47, C₂₀H₃₂O₃) was obtained from the acetone extract of Sideritis leptoclada plant as well as from some other Sideritis species. It crystallizes in the orthorhombic space group P2₁, 2₁, 2₁ with a = 10.967(3), b = 24.555(5), c = 6.372(4) Å, Dc = 1.240 g cm⁻³, Z = 4, and refines to R = 0.065 for 721 independent reflections. The skeleton consists of three fused six-membered rings and a five-membered ring with fused epoxide. The six membered rings exhibited slightly distorted chair conformation. In addition to sideroxol, two kaurane and five kaurene diterpenes were isolated from the hexane and acetone extracts of the studied plant.     

Photoluminescence characteristics of Mg- and Si-doped GaN thin films grown by MOCVD technique

We have studied the optical, structural and surface morphology of doped and undoped GaN thin films. The p- and n-type thin films have been successfully prepared by low-pressure MOCVD technique by doping with Mg and Si, respectively. The different carrier concentrations were obtained in the GaN thin films by varying dopant concentrations. Photoluminescence (PL) studies were carried to find the defect levels in the doped and undoped GaN thin films at low temperature. In the undoped GaN thin films, a low intensity and broad yellow band peak was observed. The donor–acceptor pair (DAP) emission and its phonon replicas were observed in both the Si or Mg lightly doped GaN thin films. The dominance of the blue and the yellow emissions increased in the PL spectra, as the carrier concentration was increased. The XRD and SEM analyses were employed to study the structural and surface morphology of the films, respectively. Both the doped and the undoped films exhibited hexagonal structure and polycrystalline nature. Mg-doped GaN thin films showed columnar structure whereas Si-doped films exhibited spherical shape grains.     

New zeotype borophosphates with chiral tetrahedral topology: (H)0.5M1.25(H2O)1.5[BP2O8]·H2O (M = Co(II) and Mn(II))

Two new isostructural open‐framework zeotype transition metal borophosphate compounds, (H)_0.5M_1.25(H₂O)_1.5[BP₂O₈]·H₂O (M = Co(II) and Mn(II)) were synthesized by mild hydrothermal method. The structure of compounds were characterized by single‐crystal X‐ray diffraction which have ordered, alternating, vertex‐sharing BO₄, PO₄, and (MO₄)OM(H₂O)₂ groups with hexagonal, P 6₁ 2 2 (No 178) space group and unit cell parameters for Co a = 9.4960(6) Å, c = 15.6230(13) Å, for Mn a = 9.6547(12) Å, c = 15.791(3) Å, Z = 1 for both of them. TGA/DTA analysis, IR spectroscopy were used for characterization. Magnetic susceptibility measurements for both of the compound indicate strong antiferromagnetic interaction between metal centers. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

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.     

Solubility of Ag2O into the Na2O–B2O3–Al2O3 system

The solubility of Ag₂O was measured for the Na₂O–B₂O₃ and Na₂O–B₂O₃–Al₂O₃ system with the rotating crucible method and static method, respectively, under air atmosphere at temperatures ranging from 1273 to 1423 K. The contamination of melts from crucibles could be avoided by the rotating crucible method, with which it became possible to measure the solubility of Ag₂O for the Na₂O–B₂O₃ system above the melting point of Ag for the first time. It was found that the addition of Na₂O decreases the solubility of Ag₂O while the addition of Al₂O₃ had little effect on the solubility. The effect of Na₂O and Al₂O₃ on the solubility of Ag₂O is expressed by interaction coefficients and is analyzed in terms of the basicity of melts. The solubility of Ag₂O in Na₂O–B₂O₃–Al₂O₃ melts increased with increased temperature. This phenomena was explained by a small enthalpy change in oxidation of silver.     

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.