微波法合成纳米MnO_2及其电化学性能研究

采用微波法制备了不同形貌的MnO2纳米粉体。通过X射线衍射、扫描电子显微镜对MnO2的微观结构和形貌进行了表征。结果表明:制备的MnO2为α-MnO2和γ-MnO2的混晶,随着微波反应时间的增加,其形状由花瓣状过渡为棒状,并且其晶型越来越完整。电化学测试结果表明,合成的MnO2在2 mol/L的(NH4)2SO4中具有较好的电化学性能,在2 mA/cm2的电流下放电时的比容量为240 F/g。     

邻菲咯啉铜微纳米棒的制备及其影响因素研究

以五水硫酸铜和1,10-邻菲咯啉为原料,采用液相沉淀法制备邻菲咯啉铜(Ⅱ)微纳米棒,研究 pH 值和温度对产物形貌和尺寸的影响.通过 XRD、SEM、UV-Vis、FT-IR、元素分析和荧光光谱表征产物的结构与性能.结果表明,硫酸铜溶液的 pH 值显著影响室温时反应产物的物相和形貌.当起始 pH 值为 2.0和5.0时,分别生成了微米级的花状和长片状的单斜品系[Cu(phen)(H2O)2]·SO4;当 pH 值上升至 9.0和11.0时,分别生成了平均直径172 nm 和253 nm 的[Cu(phen)(OH)]2SO4·5H2O 棒状结构.在 pH 值为9.0条件下,棒状产物的直径随着反应温度的降低而减小,4℃时可获得平均直径为87 nm 的纳米棒.此外,片状[Cu(phen)(H2O)2]·SO4 的荧光光谱相对于纳米棒状[Cu(phen)(OH)]2SO4·5H2O 出现蓝移和发射增强现象.     

α-MnO2和 β-MnO2一维材料的可控制备及其电容性能

将锰粉分散在K2S2O8水溶液中,分别在150℃和180℃水热处理24 h制备了两种MnO2材料.应用X-射线衍射(XRD)、扫描电镜(SEM)和N2吸-脱附技术对所得产物进行表征.结果表明,α-MnO2具有纳米线状形貌(直径为40～60 nm,长度约为4μm),β-MnO2具有棒状形貌(长度约为3μm).α-MnO2的比表面积高达87 m2/g,而β-MnO2的仅为6.2 m2/g.电化学测试结果表明,在1 mol/L Na2 SO4水溶液中,当扫描速度为5 mV/s时,α-MnO2和β-MnO2的比电容分别为121 F/g和19 F/g.扫速为20 mV/s时,α-MnO2循环2000次后的容量保持率高达99.2;.α-MnO2具有优异的电容性能.     

水热法生长棒状MnOOH和MnO2晶体

以高锰酸钾(KMnO4)和硫酸铵((NH4)2SO4)为主要原料,在150℃反应16h,水热法生长了棒状MnOOH晶体,然后以合成的棒状MnOOH晶体为前驱物,在硫酸溶液中,130℃水热反应12h,生长了棒状MnO2晶体.探索了KMnO4和(NH4)2SO4的用量以及反应温度对合成棒状MnOOH晶体的影响.利用X射线粉末衍射(XRD)、透射电子显微镜(TEM)和选区电子衍射等(SAED)等手段对产物进行了表征.结果表明,产物MnOOH为单斜结构的纯相,呈现棒状形貌,其平均直径约为72nm, 长度近9.2μm,显示单晶特性;产物MnO2为四方结构的纯相,呈现棒状形貌,其平均直径约为83nm, 长度达11μm,显示单晶特性.     

模板剂对微波水热合成CdS微晶相组成、形貌及光学性能的影响

采用微波水热法,以CdCl2·H2O和Na2S2O3·5H2O为镉源和硫源,分别以柠檬酸、乙二胺四乙酸(EDTA)、六亚甲基四胺(乌洛托品)和聚乙烯吡咯烷酮(PVP)为模板剂,合成了不同微观形貌的硫化镉微晶.利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、EDS、透射电子显微镜(TEM)等对样品的物相、形貌和元素组成进行了分析.结果表明:通过添加不同模板剂制备了球形、花状和棒状硫化镉微晶,制备的硫化镉微晶结晶良好;紫外-可见吸收光谱分析表明,产物均发生了不同程度的蓝移.     

流动电势测量法表征Al2O3微滤膜的表面电荷性能

本文通过错流过滤方式下的流动电势测量对氧化铝微滤膜的电动性能进行表征,研究了过滤介质溶液pH、电解质种类和浓度等对膜的电动性能的影响.结果表明,膜流动电势大小取决于过滤溶液pH、电解质溶液种类和浓度.采用浓度为10-3M 的NaCl溶液为过滤介质时,膜的等电点为6.1,而采用相同浓度的CaCl2 和Na2SO4溶液时,由于对Ca2+和SO42-的特定吸附,膜等电点分别增大至6.8和减小至5.6.由于Ca2+和SO42-在膜孔表面存在特定吸附,溶液离子浓度提高导致膜的等电点和表面净电荷符号改变,而NaCl溶液浓度提高仅使膜流动电势逐渐减小,但等电点不变.     

棒状超顺磁性铁锰复合氧化物制备及对Pb2+吸附性能的研究

采用水热-共沉淀法,以N,N-二甲基十二烷基氧化胺(DDAO)与硬脂酸铁(Ⅲ)(STFE)组成的囊泡为软模板,FeSO4·7H2O为二价铁源,MnSO4·H2O为锰源,NaOH为碱源,制备铁锰复合氧化物.利用SEM、XPS和BET对样品进行了表征,并对复合氧化物磁性及复合氧化物对Pb2+的吸附性能进行了研究.结果表明,样品的形貌可通过不同煅烧温度进行调控,在500℃制备出样品是直径约为40 nm,长度约为150 nm棒状结构;对Pb2+吸附测试结果表明,在500 ℃制备的样品对Pb2+表现出优异的吸附性能,饱和吸附量为618.118 mg/g,重复5次使用后饱和吸附量仍在390 mg/g.特别是这种材料很好的超顺磁性(饱和磁化率为63.9814 A·m2/kg),可以实现对吸附剂有效的回收.     

感应区熔法制备Al2O3/MgAl2O4/ZrO2共晶陶瓷

利用感应区熔法制备了Al2O3/MgAl2O4/ZrO2共晶陶瓷.当坩埚壁温为2200℃、行走速度为2mm/h时,制备了φ10 mm ×62 mm表面光滑致密的陶瓷样品.扫描电镜微观组织图显示Al2O3相和MgAl2O4相为基体相,ZrO2相以棒状镶嵌在基体中.定向凝固共晶陶瓷硬度和断裂韧性达到12 GPa和6.1 MPa·m1/2,为预烧结体的2倍和1.7倍.气孔和晶界的消失及细小规整ZrO2相在基体中的弥散分布,有效提高了材料的硬度和断裂韧性.     

不同表面活性剂对纳米ZnO/ZrO2的制备和脱硫性能的影响

研究不同表面活性剂对采用共沉淀-真空冷冻干燥法制备的ZnO/ZrO2纳米催化剂的结构和物相变化的影响,并在模拟烟气中利用气相色谱仪进行脱除SO2性能的测定.结果表明,表面活性剂的引入可以降低纳米ZrO2的平均晶粒度.与吐温80、PEG-400和PVA相比,柠檬酸铵和DBS抑制晶核生长的能力更大,从而纳米ZrO2的平均晶粒尺寸更小,脱硫率更高;由于PEG-400具有络合正离子的能力,可防止纳米活性组分的团聚和长大,其催化吸收SO2的性能最好.     

类花状羟基磷灰石催化降解孔雀石绿染料废水的研究

以膨胀石墨为微反应器,通过化学沉淀法合成类花状羟基磷灰石,采用X射线粉末衍射(XRD)、扫描电子显微镜(SEM)、傅里叶变换红外光谱(FT-IR)等手段对催化剂使用前后的结构和形貌进行表征,同时考察了催化剂用量、H2O2用量、溶液初始浓度等因素对孔雀石绿去除效果的影响.根据动力学方程t/qt=1/k2q2e+t/qe,降解过程近似符合准二级动力学方程,吸附速率常数为0.0050 g·mg·min-1.当催化剂加入量为0.01 g,H2 O2体积为0.1mL,反应时间为54 min,孔雀石绿溶液(10 mg/L)脱色率达到98.7;.     

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。     

Selinidin: Crystal structure generated by C–H···O, C–H···π and π-π interactions

The title compound, 9,10-dihydro-8,8-dimethyl-2-oxo-2H,8H-benzo[1,2-b:3,4-b']dipyran-9-yl-2-methyl-2-butenoate, C₁₉H₂₀O₅, was isolated from the roots of Selinum vaginatum. The compound crystallizes into monoclinic space group P2 ₁ with unit cell parameters: a = 12.830(2) Å, b = 9.041(1) Å, c = 14.983(1) Å, β = 95.09(1)°, Z = 4. The crystal structure has been determined using direct methods and refined by full-matrix least-squares to a final R value of 0.0529 for 3142 observed reflections. There are two independent molecules, A and B, per asymmetric unit. In both the molecules, the coumarin nucleus is planar. However pronounced differences are observed in the conformation of dihydropyran ring which has a half-chair conformation with an 8β-9α orientation in molecule A and is intermediate between half-chair and sofa in molecule B. Differences also occur in the conformation of the 2-methylbutenoyloxy side chain at C9 due to the different geometry of C–H···π interactions in molecules A and B. Molecules A and B are connected by π–π interactions between their coumarin fragments forming dimers. The dimers interact through C–H···O and C–H···πhydrogen bonds.     

Chromene and Imidazole Based D-π-A Chemosensor Preparation and Its Anion Responsive Effects

We have designed and synthesized the colorimetric chemosensor through the reactions of 2-(4H-chromen-4-yildene)malonitrile and 4-imidazolecarboxaldehyde. Due to its well conjugated D-π-A system and the existence of NH- fragment in structure, we expected that the chemosensor can detect anion using NH- fragment in the imidazole moiety of the structure. In this regard, UV-Vis absorption spectra were measured to investigate sensing properties of the probe toward different anions in DMSO. This chemosensor can detect both fluoride and cyanide ion with absorption change in intensity. In addition, pH sensing property was also investigated upon the addition of hydroxide ion. These properties are related to the deprotonation effect. The ICT system in this molecule was also observed by the computational approach using Material Studio 4.3 package.     

电子显微分析在表征纳米晶体化学组分中的应用

纳米材料的化学组分及含量影响其光、电、声、热、磁等物理性能,电子显微分析是表征纳米晶体化学组分的重要方法之一.本文综述了X-射线能谱(EDS)、X-射线波谱(WDS)、电子能量损失谱(EELS)和选区电子衍射(SAED)等现代电子显微分析技术在表征纳米晶体化学组分、形貌、尺寸和结构等方面的应用及其研究进展,并比较了这些分析方法存在的差异,提出了其应用中存在的不足及今后的研发方向.     

4- and 5-nitroindane

Mononitration of indane produces a mixture of 4- and 5- nitroindanes. Crystallization from mixtures occurs after distillation improves composition of a major component to above 80%. 4-Nitroindane: triclinic, space group (#2),a=7.332(4) Å,b=8.304(4) Å,c=8.358(4) Å, =61.43(4)°, =67.60(4)°, =70.15(4)°,V=405.4(4) ų,Z=2. Non-H-atoms are nearly planar, aliphatic H's are eclipsed. 5-Nitroindane: monoclinic, space groupP2₁/c (#14),a=10.946(8) Å,b=15.643(10) Å,c=9.415(6) Å, =92.34(5)°,V=1611(2) ų,Z=8. Non-H-atoms in the two molecules differ in torsion of the nitro group with respect to indane and fold of the nonbenzylic methylene group. Semiempirical calculations (PM3) suggest that distorsion from planarity may be associated with the two lowest energy vibrational modes. Uv, ir, ms, proton, and¹³C-nmr spectra are correlated with the solid state structures.     

6<Emphasis Type="Italic">S</Emphasis>,8α-Dihydroxy-14,15-Dihydrocarapin (Khayanone) from the Stem Bark of <Emphasis Type="Italic">Khaya Senegalensis</Emphasis> (Meliaceae): Isolation and its Crystal Structure

Khayanone was isolated from the stem bark of African mahogany, Khaya senegalensis (Meliaceae), and characterized as 6S,8α-dihydroxy-14,15-dihydrocarapin on the basis of spectral analysis and single crystal X-ray diffraction study. The compound crystallizes in the tetragonal space group P4 ₁ 2 ₁ 2 with unit cell parameters: a = 13.2315(19) Å, c = 29.118(6) Å, Z = 8. The crystal structure has been solved by direct methods and refined to R = 0.0375 for 4552 unique reflections. The six-membered rings A and B exist in boat conformations, rings C and D in chair conformations, and the furan ring is planar. The crystal structure is stabilized by O-H···O and C-H···O interactions. This is the first report about 6S configuration of mexicanolide revealed by X-ray diffraction analysis. The configuration of oxygenated C-6 in mexicanolide-group limonoids is discussed.     

Nuclear magnetic resonance: a powerful tool to study liquid crystals

Nuclear magnetic resonance (NMR) is a spectroscopic technique widely used to investigate materials and soft matter in particular. In this brief review, the main uses of NMR techniques to investigate different aspects of liquid crystals, such as the orientational and dynamic properties, the supramolecular structure and average molecular conformations, are described. In the second part of the paper, the case study of a ‘de Vries’ liquid crystal is reported and the main results obtained by combining different NMR techniques are discussed.     

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.     

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)