Yb(Cl4)3·3H2O-18C6-C2H5OH体系(25℃)的相化学研究及固态配合物的合成与性质

The solubilities of Yb(ClO₄)₃·3H₂O-18C6-C₂H₅OH ternary system at 25 were invstigated by a semimicro method for study of phase equilibrium.and the refractive indexes of saturated solutions were determined.The behavior of water in this system during the equilibrium was examined.The results indicate that there are two kinds of complexes formed in the system, their chemical compositions are: Yb(ClO₄)₃·18C6·3H₂O·2C₂H₅OH (I) and Yb(ClO₄)₃ 18C6·3H₂O·C₂H₅OH.Both are incongruently soluble in EtOH.The influences of rare earth ions and salt anions on formation of complexes were discussed.The two solid complexes have been prepared, and their composihons and properties have been investigated by chemical analysis, IR, DTG and DSC.According to the DSC, the enthalpies of some steps during the decomposition have been obtained for complexes (Ⅲ)and (Ⅳ).     

The Sialons MLn[Si4−xAlxOxN7−x] with M = Eu,Sr, Ba and Ln = Ho‐Yb – Twelve Substitution Variants with the MYb[Si4N7] Structure Type

The oxonitridoalumosilicates (so‐called sialons) MLn[Si_4?xAl_xO_xN_7?x] with M = Eu, Sr, Ba and Ln =Ho, Er, Tm, Yb were obtained by the reaction of the respective lanthanoid metal, the alkaline earth carbonates or europium carbonate, resp., AlN, “Si(NH)₂” and MCl₂ as a flux in a radiofrequency furnace at temperatures around 2100 °C. The compounds MLn[Si_4?xAl_xO_xN_7?x] are relevant for the investigation of substitutional effects on the materials properties due to their ability of tolerating a comparatively large phase width up to x ≈ 2.0(5). The crystal structures of the twelve compounds were refined from X‐ray single crystal data and X‐ray powder data and are found to be isotypic to the MYb[Si₄N₇] structure type. The compounds crystallize in space group P6₃mc (no. 186, hexagonal) and are made up of chains of so‐called starlike units [N^[4](SiN₃)₄] or [N^[4]((Si,Al)(O,N)₃)₄], respectively. These units are formed by four (Si,Al)(N/O)₄ tetrahedra sharing a common central nitrogen atom. The structure refinement was performed utilizing an O/N‐distribution model according to Paulings rules, i.e. nitrogen was positioned on the four‐fold bridging site and nitrogen and oxygen were distributed equally on both of the two‐fold bridging sites, resulting in charge neutrality of the compound. The Si and Al atoms were distributed equally on their two crystallographic sites, referring to their elemental proportion in the compound, due to being poorly distinguishable by X‐ray methods. The chemical compositions of the compounds were derived from electron probe micro analyses (EPMA).     

基于非线性偏振旋转效应的多波长掺铥锁模光纤激光器

运用非线性偏振旋转效应实现了一种掺铥锁模多波长光纤激光器.采用环形腔结构,以1 565nm半导体光源为泵浦源,3m长掺铥光纤为增益介质.利用非线性偏振旋转效应进行滤波.当泵浦功率在800mW时,通过调节光纤偏振控制器,激光器出现了被动锁模状态的脉冲输出,脉冲重复频率为3.178MHz,脉冲宽度为617ps.进一步增加泵浦功率,激光器进入多波长输出的工作状态.调节偏振控制器在室温下得到1~5个稳定的波长激光输出,边摸抑制比为40~60dB.     

无溶剂一锅法Al(ClO_4)_3催化合成α-氨基膦酸酯

以无水高氯酸铝为催化剂,将芳香醛、芳香胺及亚磷酸酯在无溶剂条件下一锅法反应,高效地合成了α-氨基膦酸酯,该催化剂优于其它已发现的催化剂[如Mg(ClO4)2,BiCl3,AlCl3等],建立了一种适用于含有钝化基团的芳香胺的α-氨基膦酸酯的新合成方法.     

Copper(II) perchlorate complexes with antipyrine: synthesis,structure, cytotoxicity and DFT calculations

The synthesis, structure and properties of copper(II) perchlorate complexes with antipyrine (AP), [Cu(AP)₄(H₂O)](ClO₄)₂ and [Cu(AP)₅](ClO₄)₂, are described and compared with those of alternative compounds containing different AP ligands.     

Facile Fabrication of Cu-doped Carbon Aerogels as Catalysts for the Thermal Decomposition of Ammonium Perchlorate

We report a simple and effective method to produce copper-doped carbon aerogel (Cu-CA) using sodium alginate as a carbon precursor through ion crosslinking and high-temperature carbonization. Results indicate that Cu-alginate has a 3D scaffold structure with pores. The effect of using different metal salt mass ratios of Cu-CA on the catalytic thermal decomposition of AP is also investigated. The thermal decomposition temperature of AP decreases by 94.24 °C, and the activation energy of the decomposition reaction is reduced by 45.7 kJ/mol. These results demonstrate that the composite exhibits superior catalytic performance compared with a single-component transition metal salt.     

Enthalpies of transfer of amino acids from water to aqueous solutions of sodium nitrate and sodium perchlorate at T = 298.15 K

Enthalpies of solution of glycine, l-alanine and l-serine in water and aqueous solutions of NaNO₃ and NaClO₄ have been determined at T = 298.15 K with a calorimeter. Enthalpies of transfer (Δ_trH) from water to aqueous solutions of salts were derived and interpreted in terms of electrostatic interaction and structural interaction. Δ_trH decreases with increasing salt concentration in the composition range studied. The transfer enthalpies of amino acids from water to NaNO₃ solution and low concentration NaClO₄ solution vary in the sequence l-serine < glycine < l-alanine while glycine < l-serine < l-alanine in NaClO₄ solution above 2 mol kg⁻¹. The difference may be due to ion association at high concentration, weakening the interaction with l-serine more than with glycine.     

Excited states Tm spectroscopy in ZBLAN glass for S-band amplifier

We report on excited state spectroscopy measurements of Tm doped ZBLAN glass designed for fiber amplifier in the 1.48 μm wavelength range. Low temperature absorption, emission and Excited State Excitation measurements are reported to clearly identify the transitions involved in the different pump mechanisms of this Thulium Doped Fluoride fiber Amplifier. Room and low temperature Excited State Absorption spectra were recorded and quantitative determination of absorption cross sections has been obtained which allows to further proceed to a modeling of this amplifier.     

Kalman滤波法在电感耦合等离子体原子发射光谱分析中的应用 Ⅰ．测定高纯氧化铥中的14种稀土杂质

本文研究了电感耦合等离子体原子发射光谱分析Ｋａｌｍａｎ滤波法测定高纯氧化铥中的１４种其他稀土杂质的方法。Ｋａｌｍａｎ滤波法有效地消除光谱干扰，可利用受干扰的光谱灵敏线，因而可提高灵敏度，是一种在大量基体存在下测定痕量杂质的有效方法。     

Conductivity of lithium perfluorononanoate in water-poly(vinyl pyrrolidone) solutions

Conductivity measurements, focused on the counterion binding of lithium perfluorononanoate (LiPFN) micelles in pure water and in the presence of poly(vinyl pyrrolidone) (PVP), have been carried out. An abrupt decrease of the conductance of the LiPFN in pure water, due to the self aggregation of anions and to dynamic linkage of cations on the micellar surface, has been found. Analysis of the conductometric data indicates that about 50% of the stoichiometric concentration of Li⁺ interacts with the head groups of the perfluorinated anions involved in micellar assembly. Conductometric data of LiPFN-water-PVP systems reveals a favorable influence of the PVP on the micellization process modulated by the concentration and by the molecular weight of the polymer. Analysis of these data shows that in presence of PVP the degree of binding of lithium ion to the micellar assemblies linked to the polymer is smaller than in pure water. By increasing the amount of surfactant in solution up to the concentration where the polymer becomes saturated by LiPFN micelles, the binding of lithium ion in the system becomes slightly greater than that observed in LiPFN-water system. This finding can be interpreted in terms of additional binding of lithium ion to the polymer chains. Conductivity measurements carried out on LiClO₄ and KClO₄ in water + PVP support this interpretation.