掺希土离子Eu3+的BaTiO3超细微粉的制备及物性表征

近年来人们对材料及由材料制备的元件提出了高可靠性、多功能等要求。为了达到这种要求,人们从多种途径进行了探索,其中,对现有材料进行掺杂就是很有效的方法之一［１,２］。本文报道对ＢａＴｉＯ３超细微粉进行Ｅｕ３＋的有效掺杂并对其进行了物性表征。１实验部分１...     

溶剂萃取法制备Co(PO_3)_2超细微粉

本文用溶剂萃取法成功地制备了偏磷酸钴超细微粉并通过ＸＲＤ，ＩＲ，ＴＧ，ＤＴＡ，ＴＥＭ等实验对超细微粉的组成、结构进行了表征。     

金属团簇MoS4Cu4(SCN)2(NC5H5)6的皮秒光学非线性特性和光限幅特性研究

由于激光技术的快速发展，新型超快可调谐波长的高功率激光器更多的在民用和军事上应用。快速的非线性光学器件的需求越来越多。近10年，人们投入大量研究寻找超快光学非线性材料，同时寻找快速响应、高线性透过率和低非线性透过率以及高损伤阈值的光限幅材料，研究发现金属酞菁化合物、金属卟啉化合物以及富勒烯衍生物具有良好的光限幅效果和强的光学非线性特性。     

新型一维链状配位聚合物[Cd2(C23H14O6)2(C10H9N3)2(H2O)]n的研究

配位超分子聚合物的设计合成与应用研究一直是配位化学、超分子化学、生物无机化学及材料科学等领域的热点研究课题之一,具有微孔结构的配位聚合物吸引了许多科学家的目光,这不仅因为该类配合物具有新颖的结构,展现出多种诱人的拓扑结构,更主要的 是因为它们在离子交换、催化、磁性材料、光学材料及气体贮存领域的应用潜力[1～3].     

Zn(Oxin)2·2H2O纳米晶的固相化学反应合成及表征

随着纳米微粒研究的深入,对纳米超细微粒提出了不同的物理、化学特性需求,制备高纯、超细、均匀的纳米微粒,发展新型的纳米材料,就显得非常重要,而解决问题的关键在于研究、发展新的合成技术.通常,纳米微粒制备的要求是:表面洁净;粒子形状及粒径、粒度分布可控,防止粒子团聚;易于收集;有较好的稳定性;产率高.     

低温反应制备高纯度纳米BN包覆Al2O3和ZrO2粉体

硼酸和尿素在氮气中于650℃反应,生成t-BN-Al2O3和t-BN-ZrO2纳米包覆粉.IR分析表明,反应产物中含CH2和CN基团的杂质属尿素缩聚的复杂产物,经450℃煅烧即可除去.硼酸和尿素完全反应,得到纯净的纳米复合粉体.BN产率大于99%,在复合粉中的含量与计算值吻合.     

片状MoS2/MoS1.5Se0.5纳米复合材料的制备及其摩擦学性能研究

将钼粉与升华硫和硒粉的混合粉末按一定化学计量比混合,通过固相反应法成功制备出了均匀的片状纳米颗粒。分别使用X射线粉末衍射仪(XRD)、扫描电子显微镜(SEM)以及透射电子显微镜(TEM)对该纳米粉体进行结构表征和分析,发现该粉体为MoS2/MoS1.5Se0.5混合晶相,晶粒尺寸在300~600 nm,厚度约为5 nm的片状结构。将该MoS2/MoS1.5Se0.5纳米片作为润滑油添加剂添加到基础油中,使用UMT-2型摩擦磨损试验机对其摩擦学性能进行测试,并对摩擦机理进行了解释,结果表明MoS2/MoS1.5Se0.5纳米片作为润滑油添加剂具有良好的减摩抗磨性能。     

LaL3(NO3)3·(H2O)2·(C2H5OH)2的晶体结构和生成反应焓变

0 引言 稀土是一类具有特殊结构和性质的元素,稀土元素不仅大量用于工业,而且在农业和医学领域也有广泛应用 [1,2].其中,镧系离子以其独特的光、电、磁、催化和分析等性能而受到人们的广泛关注,并进行了大量的研究.镧系离子本身发光效率低,目前,设计并合成含有稀土离子La3+和Eu3+的超分子配合物,作为发光分子器件和荧光探针成为稀土配位化学,材料科学,超分子化学,分析化学和生物化学等研究领域的热点课题之一 [3～8].但对它们的热化学行为的研究鲜见文献报道.     

CO2超临界干燥制备超细TiO2粉体的研究

采用溶胶-凝胶法结合CO2超临界流体干燥技术制备了平均粒径为8nmTiO2粉体颗粒,并采用BET、TEM、SEM、XRD、及DTA-TG技术对制得的粉体进行了表征.结果显示出CO2超临界干燥技术在制备大孔高比表面TiO2纳米粉体时具有较大的优越性.     

超亲水TiO2和TiO2-SiO2表面的动态润湿性

1997年, Fujishima研究组[1]发现TiO2表面经UV光照射能产生较强的亲水性, 同时具有较高的亲油性, 即经UV光照射后的TiO2表面具有超双亲的性质. 这种防雾和自清洁性在工业上应用广泛, 已引起了人们的极大兴趣[2～5]. 进一步的研究发现, 超亲水的TiO2表面在暗处放置会变为疏水表面. 对于这个问题, 除了可以通过UV光照[6]、氩离子或电子束溅射[6]和高温热处理[5]等恢复其超亲水性外, 还可以通过添加摩尔分数为10%～30%的SiO2有效地降低TiO2表面的接触角, 提高UV光诱导的超亲水表面在暗处的稳定性能[3]. 另外, 诱导TiO2的亲水性需要较强的UV线强度(如太阳光), 使它在室内应用受到限制. 为了在室内实现TiO2的自清洁功能, Watanabe等[4]发现在TiO2中添加WO3可使TiO2在室内的照明光下也能实现亲水性转变. 以上这些研究成果为TiO2在工业和生活上的实际应用提供了重要的科学依据. 然而, TiO2的防雾和自清洁功能的实现同时也受其动力学性质的制约.     

Crystal structure of [Mn(1,10-C12H8N2)3](B6H7)2

A new compound [MN^II(Phen)₃]²⁺(B₆H₇)₂⁻ is synthesized; its crystal structure is studied by XRD at 100 K. Crystallographic data: C₃₆H₃₈B₁₂N₆Mn, M = 739.39, triclinic symmetry, space group P , unit cell parameters: a = 10.3131(3) ?, b = 13.4839(4) ?, c = 15.1132(4) ?; α = 97.696(1)°, β = 108.324(1)°, γ = 102.211(1)°; V = 1903.9(1) ?³, Z = 2, d _calc = 1.290 g/cm³. The structure is solved by direct and Fourier methods and refined by full-matrix LSM in the anisotropic (isotropic for hydrogen atoms) approximation to the final factor R ₁ = 0.036 for 10169 I _hkl ≥ 2σ _I (Bruker-Nonius X8 APEX CCD diffractometer, λMoK _α). The structure contains two crystallographically different anions. Original Russian Text Copyright ? 2009 by T. M. Polyanskaya, M. K. Drozdova, V. V. Volkov, and K. G. Myakishev __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 2, pp. 381–385, March–April, 2009.     

Complexes of neodymium and dysprosium triiodides with amines. Molecular structures of the {Dy[Me2N(CH2)3NH2]8}I3, NdI3(PriNH2)4, and NdI3(PriNH2)5 complexes

The dissolution of DyI₂ in diamine Me₂N(CH₂)₃NH₂ (DMDA) is accompanied by the disproportionation of the salt, hydrogen evolution, and oxidation of Dy^II to Dy^III. The [Dy(DMDA)₈]I₃ complex (1) was isolated from the solution. The neodymium amide amine complex (PrⁱNH)NdI₂(IPA)₄ was produced by the reaction of NdI₂ with isopropylamine (IPA). The recrystallization of this complex from IPA afforded the NdI₃(IPA)₄ complex (2). The recrystallization of (PrⁱNH)NdI₂(IPA)₄ from a toluene-IPA mixture gave the complex with five amine ligands, NdI₃(IPA)₅ (3). The structures of compounds 1, 2, and 3 were established by X-ray diffraction. Dedicated to Academician G. A. Abakumov on the occasion of his 70th birthday. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1674–1679, September, 2007.     

[Pt2(P2O4H2)4]4-和[Pt2(P2O4CH4)4]4-基态和激发态性质的理论研究

采用从头计算MP2和CIS方法分别优化等电子双核d⁸配合物[Pt₂(P₂O₄H₂)₄]^4-和[Pt₂(P₂O₄CH₄)₄]^4-的基态和激发态结构。结果表明基态Pt-Pt距离分别为0.290 5和0.298 7 nm，与实验的0.292 5和0.298 0 nm符合。NBO计算的Pt-Pt键级以及Pt原子间伸缩振动说明Pt-Pt相互作用具有吸引本质。CIS计算揭示电子激发到Pt-Pt的σ(p_z)成键轨道使得相互作用增强。保持激发态几何，含时密度泛函理论(TD-DFT)计算的溶液发射分别为449和475 nm，与实验值512和510 nm接近。     

Inclusion compounds of cystostatic active (C5H5)2VCl2 and (CH3C5H4)2VCl2 with α-, β- and γ-cyclodextrines: Synthesis, EPR study and microbiological behavior toward Escherichia coli

The inclusion of vanadocene dichloride (VDC) and 1,1′-dimethyl vanadocene dichloride (MeVDC) into cyclodextrines (α-CD, β-CD and γ-CD) was studied by EPR spectroscopy. It was found that VDC and MeVDC with β-CD and γ-CD form true inclusion compounds, but with α-CD, VDC and MeVDC gave only fine dispersion mixtures. The inclusion was validated by anisotropic EPR spectra of solid samples. In addition, the antimicrobial was validated by anisotropic EPR spectra of solid samples. In addition, the antimicrobial behavior (against E. coli) of each of the complexes was determined. It was established that not only did VDC and MeVDC cause elongation of E. coli, but also the new vanadocene inclusion complexes were effective in this regard.     

Crystal structure and single crystal EPR of (NH4)2(15-crown-5)3[Cu(mnt)2] and (NH4)2(benzo-15-crown-5)4[Cu(mnt)2]·0.5H2O

The X-ray crystal structures of (NH4)2(15-crown-5)3[Cu(mnt)2] (1) and (NH4)2(benzo-15-crown-5)4- [Cu(mnt)2]·0.5H2O (2) were determined. Two single crystals are composed of distinct structures of ammonium-crown ether supramolecular cation and [Cu(mnt)2]2- anion. The triple-decker dication in complex 1 and a sandwich dimmer in complex 2 were observed. X-Band EPR studies on the single crystals of both complex 1 and complex 2 have been carried out at room temperature, which revealed that complex 2 showed a perfect hyperfine structure of Cu whereas that of complex 1 could not be observed. The principal values and direction cosines of the principal axes of the g and A tensors were computed by a least-squares fitting procedure. The spin density of Cu(Ⅱ) was estimated according to the principal values of the A tensors and compared well with the results calculated based on DFT method.     

CCl2自由基被无机小分子猝灭的速率常数

对CCl4/Ar混合气体脉冲直流高压放电产生CCl2自由基,用541.52 nm激光将电子基态CCl2激励到A 1B1(0,4,0)振动能级上. 通过检测激发态CCl2时间分辨荧光信号,测得室温下CCl2(A 1B1和a 3B1)被O2、N2、NO、 CO2、 CS2、H2O、SO2,和SF6分子猝灭的实验结果.用我们提出的三能级模型分析处理实验数据,获得了CCl2(A 1B1)态和CCl2(a 3B1)态的碰撞猝灭速率常数kA和ka值.     

Catalytic Performance of Re/Ga2O3/WO3/ZrO2 Catalyst for n-Hexane Isomerization

A series of Re/Ga₂O₃/WO₃/ZrO₂ catalysts were prepared by the impregnation method. The crystalline structure, redox, and acid site distribution of the catalysts were characterized by X-ray powder diffraction, temperature-programmed reduction of H₂, and temperature-programmed desorption of NH₃. Their catalytic performance for n-hexane isomerization was studied. The results showed that the addition of Re greatly affected the redox properties and the acid site distribution of the catalysts. Owing to the presence of Re, n-hexane isomerization was catalyzed by metal and acid sites, and thus the conversion of n-hexane and the selectivity for 2,2-dimethylbutane were significantly increased. Under the conditions of 195 °C, 1.0 MPa, LHSV = 1.0 h⁻¹, and n(H₂)/n(C₆) = 2.0, the conversion of n-hexane over 1.0%Re/1.0%Ga₂O₃/WO₃/ZrO₂ is 84.8%, and the selectivities for 2,2-dimethylbutane, i-hexane, and cracking products (C_5-) are 20%, 97.7%, and 2.1%, respectively. The catalyst is stable during 150 h operation.     

Intramolecular Hindrances to CCl3 Reorientations in CCl3PCl4 and (CCl3)2PCl3 Crystals

The trigonal bipyramidal structure of trichloromethyl-tetrachlorophosphorane CCl₃PCl₄ and bis(trichloromethyl)trichlorophosphorane (CCl₃)₂PCl₃ molecules with apical CCl₃ groups is responsible for steric hindrances to reorientations of these groups around the C–P bond. The intramolecular barriers to CCl₃ reorientations calculated for the two phosphoranes (Hartree–Fock method using the 6-31G(d) basis set) are 105.9 kJ/mole and 106.6 kJ/mole, respectively. These internal barriers are high enough to block the reorientational motion of the CCl₃ groups, as found previously by ³⁵Cl NQR for the stated crystals.     

CCl2(A 1B 1,a3B1)自由基被烷烃类分子猝灭动力学

用放电 LIF实验装置,对CCl4/Ar混合气体放电产生CCl2自由基,再用541.52 nm激光将电子基态CCl2激励到激发态A 1B1(0,4,0)振动能级上,通过检测激发态CCl2时间分辨荧光信号,测得室温下CCl2(A 1B1)被烷烃类分子猝灭的实验结果,用我们提出的三能级模型分析处理实验数据,获得CCl2(A 1B1)态和CCl2(a 3B1)态的碰撞猝灭速率常数kA和ka值.     

一维链状配位聚合物[Pb_2(C_8H_7O_2)_4(H_2O)_2]_n的合成、晶体结构及荧光性质

<正>近年来,铅的配位聚合物以其丰富的结构与在离子交换和光学等领域中的应用前景[1-3]而引起了广泛关注。由于铅的原子半径较大,可以形成较高的配位数[4-6];另外,二价铅的6s轨道上有一对孤对