Synthesis,crystal growth,structural, spectral,optical, thermal and dielectric studies of a new nonlinear optical material: 4-Hydroxy-l-proline-l-tartaric acid (1:1)

Single crystals of a new organic material, 4-hydroxy-l-proline-l-tartaric acid (HPTA) adduct, were grown by slow evaporation of an aqueous solution containing equimolar concentrations of 4-hydroxy-l-proline and l-tartaric acid at room temperature. Formation of new crystal has been confirmed by single crystal X-ray diffraction and NMR spectroscopic techniques. The single crystal XRD analysis shows that a molecule of 4-hydroxy-l-proline and a molecule of free l-tartaric acid both of which are interlinked to each other by two types of H-bonding interactions, namely O(6)–H(6)⋯O(2) and N(1)–H(1B)⋯O(10). The title compound (HPTA) crystallizes in monoclinic crystal system with non-centrosymmetric space group P2₁. The suitability of the crystal for optical applications was studied by UV–Vis–NIR spectroscopy. Fourier transform infrared (FT-IR) spectral analysis was used to confirm the presence of various functional groups in the grown crystals. The thermal stability of the compound was investigated by thermogravimetric and differential thermal analyses. The dielectric constant and dielectric loss of the crystal were studied as a function of frequency and temperature. The fluorescence spectral analysis of the title crystal shows an indigo emission. The second order nonlinear optical (NLO) property of the crystal was confirmed by the modified Kurtz–Perry powder second harmonic generation (SHG) test.     

液态丙烯腈低聚物修复聚丙烯腈基碳纤维微孔缺陷

提出一种全新的缺陷修复的方法,即将聚丙烯腈基(PAN)碳纤维T300在液态丙烯腈低聚物(LAN)中浸渍后,再进行预氧化和碳化热处理,可以将T300的拉伸强度提高25%.应用二维小角X射线散射(SAXS)法可以计算出LAN修复缺陷前后T300微孔缺陷的长度(L)、横截面尺寸(lp)、取向角(Beq)、相对体积(Vrel)的变化,结果表明碳纤维的拉伸性能越好,微孔的长度、取向角、相对体积含量越小.T300拉伸性能的提高是由于缺陷修复的结果.应用BET比表面积法、扫描电子显微镜(SEM)表征LAN修复缺陷前后T300的比表面积以及表面形貌的变化,结果表明,T300在LAN中浸渍并经过预氧化和碳化热处理,比表面积变小,表面缺陷明显减少.进一步验证LAN对碳纤维中的微孔缺陷具有修复作用.应用X射线光电子能谱(XPS)法表征LAN修复前后T300表面化学成分的变化,结果表明,LAN修复后含氧官能团(C―OH,C=O,HO―C=O)显著增加,有利于增强碳纤维与树脂基体之间的相互作用,从而提高碳纤维的力学性能.     

二氧化锡薄膜:制备及在室温下气敏性质(英文)

利用溶胶-凝胶法首先在玻璃基片上制备了氧化锡晶种膜,之后采用溶剂热法在其上生长了致密的氧化锡薄膜。利用扫描电子显微镜和X射线衍射技术对氧化锡薄膜的形貌和晶体结构进行了表征,结果表明构成薄膜的氧化锡晶粒具有四方锡石结构,尺寸在7~10 nm之间。表面活性剂在溶剂热反应过程中对薄膜生长的研究表明,十二烷基苯磺酸钠可以显著提高薄膜的质量。对所制备的氧化锡薄膜进了气敏性质研究,结果表明,在温和的测试条件下,如室温、常压、干燥的空气背景等,该氧化锡薄膜对二氧化氮气体具有良好的探测能力,检测限为0.5μL·L-1。     

Lithium ion conduction and ion-polymer interaction in poly（vinyl pyrrolidone） based electrolytes blended with different plasticizers

Poly（ethylene oxide）, poly（vinyl pyrrolidone）（PEO/PVP）, lithium perchlorate salt（Li Cl O4） and different plasticizer based, gel polymer electrolytes were prepared by the solvent casting technique. XRD results show that the crystallinity decreases with the addition of different plasticizers. Consequently, there is an enhancement in the amorphousity of the samples responsible for the process of ion transport. FTIR spectroscopy is used to characterize the structure of the polymer and confirms the complexation of plasticizer with host polymer matrix. The ionic conductivity has been calculated using the bulk impedance obtained through impedance spectroscopy. Among the various plasticizers, the ethylene carbonate（EC） based complex exhibits a maximum ionic conductivity value of the order of2.7279 10 4S cm 1. Thermal stability of the prepared electrolyte films shows that they can be used in batteries at elevated temperatures. PEO（72%）/PVP（8%）/Li Cl O4（8%）/EC（12%） has the maximum ionic conductivity value which is supported by the lowest optical band gap and lowest intensity in photoluminescence spectroscopy near 400–450 nm. Two and three dimensional topographic images of the sample having a maximum ionic conductivity show the presence of micropores.     

Iso-structural phase transition in tetramethylammonium nickel（Ⅱ） nitrite [（CH3）4N][Ni（NO2）3]

The title compound, tetramethylammonium nickel nitrite [（CH3）4N][Ni（NO2）3], has a hexagonal perovskite-type structure with formula ABX3. It undergoes two reversible phase transitions occurring at about 409.1 and 428.4 K, associated with dielectric transitions. DSC measurement and dielectric measurement confirm the transition. The variable-temperature X-ray structural determinations and the powder X-ray diffraction （PXRD） experiments reveal that this compound has the same space group P3ml （No. 164） at 293 K, 413 K and 438 K. The phase transitions are caused by the rotation of the [（CH3）4N]＋ cation.     

Studies on crystal transition of polyamide 11 nanocomposites by variable-temperature X-ray diffraction

Polyamide I1 （PAll） and its nanocomposites with different organoclay loadings were prepared by melt-compounding and subsequent pelletizing. The crystal phase transitions of PAl 1 and its clay nanocomposites were investigated by variable-temperature X-ray diffraction. It was found that the Brill transition of the nanocomposite was 20 K higher than that of the neat PAl 1 for both heating and cooling processes. The PAl 1 d-spacings of the nanocomposites were observed to be smaller than those of the neat PAl 1 for melt crystallization. The constraints imposed by the addition of layered clay, restricting the thermal expansion of the polymer chains, are probably responsible for such a reduction of the d-spacing.     

大气压光电离技术及其应用研究进展

大气压光电离离子源(APPI)是一种新兴的用于液质联用的软电离离子源,它是利用光化学作用将气相中样品电离的离子化技术,该技术促进了质谱技术对弱极性化合物的分析检测。介绍了液相色谱–质谱/质谱联用技术中大气压光电离的基本原理、应用优点,综述了其在定性、定量分析检测中的应用。     

使用四乙基氢氧化铵作为有机模板剂和常规硅铝源直接合成SSZ-13沸石分子筛

使用四乙基氢氧化铵作为有机模板剂, 利用常规铝源和硅源而不需要高硅Y沸石作为起始原料, 同时加入适量的沸石晶种直接合成了SSZ-13沸石分子筛. 所合成的沸石产物结晶度好, 具有良好的水热稳定性, 并在氨选择性催化还原(NH₃-SCR)反应中显示出优异的催化性能, 为其在工业上广泛应用提供了可能.     

Preparation and Characterization of Protonated Fumaric Acid

Fumaric acid was reacted with the binary superacidic systems HF/SbF₅ and HF/AsF₅. The O,O'-diprotonated [C₄H₆O₄]²⁺([MF₆]^–)₂ (M = As, Sb) and the O-monoprotonated [C₄H₅O₄]⁺[MF₆]^– (M = As, Sb) species are formed depending on the stoichiometric ratio of the Lewis acid to fumaric acid. The colorless salts were characterized by low-temperature vibrational spectroscopy. In case of the hexafluoridoantimonates single-crystal X-ray structure analyses were carried out. The [C₄H₆O₄]²⁺([SbF₆]^–)₂ crystallizes in the monoclinic space group C2/c with four formula units per unit cell and [C₄H₅O₄]⁺[SbF₆]^– crystallizes in the triclinic space group P1 with one formula unit per unit cell. The protonation of fumaric acid does not cause a notable change of the C=C bond length. The experimental data are discussed together with quantum chemical calculations of the cations [C₄H₆O₄ · 4 HF]²⁺ and [C₄H₆O₄ · 2 H₂CO · 2 HF]²⁺.     

Mononuclear High-spin Octahedral Cobalt(II) Complex with Positive Axial Magnetic Anisotropy: Synthesis,Crystal Structure,and DFT Studies

This article outlines the magnetic features of a new six–coordinate high-spin cobalt(II) complex cis-[Co^II(tmphen)₂(NCS)₂] ( 1 ) achieved via the reactions of cobalt(II) thiocyanate with 3,4,7,8-tetramethyl-1,10-phenanthroline. The complex 1 was thoroughly characterized by different analytical and spectroscopic techniques and further confirmed by single X-ray crystal diffraction pattern. Complex 1 is a neutral molecule and adopt highly distorted six-coordinate CoN₆ octahedral coordination sphere surrounded by two thiocyanate N atoms in cis locations and the equatorial plane is occupied by two imine N atoms from the two tmphen ligand while the remaining two imine N atoms reside in the axial positions. Magnetic susceptibility data of complex 1 revealed that the χ_ΜT values decrease significantly to a value of 1.49 cm³ · K · mol^–1 at 2.0 K on decreasing temperatures below 100 K, mainly ascribed to the significant spin–orbit coupling (SOC) of six-coordinate Co^II ions. Furthermore, a field-dependence measurement was performed at 2 K, which shows a positive curvature up to 27 kOe, while it becomes linear up to 2.01 Nμ_B, which authenticated the fact that only the lowest Kramers doublet of ground state is appreciably populated.