长余辉发光玻璃SrAl2O4∶Dy, Eu的制备与发光性能研究

在低熔点破璃中掺杂一定量的长余辉发光粉制备了性能优良的长余辉发光玻璃。在保证发光玻璃均匀透明的基础上，发光性能随发光粉掺杂量的增加而增强，尽量降低假烧温度和减少保温时间可以保持良好的发光性能，在还原气氛制备的发光玻璃性能优于在空气中制备的。煅烧工艺对发光玻璃的微观结构有显著的影响。     

顺式-二(乙二胺)二硝基合钴(Ⅲ)苹果酸盐的晶体结构及手性识别

合成了标题化合物，并用X-射线衍射法确定了该分子的晶体结构。化合物Δ（λλ），Λ（δδ）－cis－[Co（en）2（NO2）2]2d，l-C4H4O5，Co2C12N12O13H22，Mr=657．94．晶体属单斜晶系，空间群为P21/c，晶胞参数：a=13．969（4），b=6.440（1），c＝14．408（4）A，β=94.37（1）°，V=1292．3A3，Z=2，Dc=1．69g／cm3，μ=105.833cm－1，F（000）=668.最终偏离因子R=0.066，Rw=0．085。结构分析表明晶体存在无序现象，其阴离子C4H4O52-有两种排列方式。R-构型和S-构型的几率各为50％，手性识别是通过Δ构型的阳离子与阴离子R-构型C原子上羟基氧形成氢键相互作用；Λ构型的阳离子与阴离子S-构型C原子上羟基氧形成氢键相互作用而实现的。     

Evolution of Er^3＋ Distribution in the Oxyfluoride Glass Ceramics with Heating

The distribution characteristics of Er3+ ions doped in the oxyfluoride glass ceramics containing LaF3 nanocrystals heat-treated at 650 ℃ for different durations were investigated. The results of the integral absorption cross-section analysis demonstrated that the partition fraction of Er3+ in LaF3 nanocrystals increases with prolonging of heating time. The anomalous phenomena of Er3+ emissions in the up-and the down-conversion fluorescence spectra are well explained based on the calculated results.     

高碲酸合铜（Ⅱ,Ⅲ）配合物的合成和性质

在Ｈ６ＴｅＯ６／ＫＯＨ水溶液中以臭氧为氧化剂，将二价铜化合物氧化成三价铜化合物，并获得一个新的三价铜化合物Ｂａ４Ｋ［Ｃｕ（Ｈ２ＴｅＯ６）２］（ＯＨ）４．６Ｈ２Ｏ；描述了碱性溶液中“Ｃｕ（Ⅲ）／Ｃｕ（Ⅲ）”循环伏安图。对铜（Ⅲ）化合物，Ｎａ４Ｈ［Ｈ２ＴｅＯ６）２］．１７Ｈ２Ｏ以及相应的铜（Ⅱ）配合物的电子光谱和Ｃｕ２ｐＸＰＳ进行了研究，给出了其配位场场强参数和Ｃｕ２ＰＸＰＸ的电子结合能。由于价态升高     

A Facile Synthesis of Ethyl 2,4-Dimethoxy-6-perfluoroalkyl-benzoates via Acyclic Precursors

Introduction Polysubstituted arenes are important intermediates in synthetic medicines and dyestuffs, and the fluorinated analogues are more attractive as a result of their lipo-philicity and the increment of activity.1,2 Therefore, to study the convenient and efficient synthesis of polysub-stituted arenes is valuable in organic synthetic method-ology. We have designed a simple synthesis of fluori-nated polysubstituted arenes through the intramolecular Wittig reaction of a new phosphorous ylid…     

新铌酸盐Ba5NdTi3Nb7O30的合成与介电性能

The New Niobate Ba₅NdTi₃Nb₇O₃₀ was synthesized by solid state reaction at 1250℃ for 48h. The crystal structure and dielectric properties of Ba₅NdTi₃Nb₇O₃₀ were determined by X-ray powder diffraction and dielectric measurements. The results show that Ba₅NdTi₃Nb₇O₃₀ belongs to ferroelectric phase of tetragonal tungsten bronze structure at room temperature with unit cell parameters: a=1.24424(4)nm, c=0.39476(2)nm, calculated density 5.719g·cm^-3. Ba₅NdTi₃Nb₇O₃₀ belongs to relaxor ferroelectrics. The phase transition temperature (T_c) of Ba₅NdTi₃Nb₇O₃₀ from ferroelectric to paraelectric is found to shift toward higher temperature side at higher fre-quency, and T_c is 90℃ at 1kHz. At room temperature, the dielectric constant (ε_r) and dielectric loss of Ba₅NdTi₃Nb₇O₃₀ decrease with the increase of frequency, and Ba₅NdTi₃Nb₇O₃₀ ceramic have high dielectric constant 489 at 1kHz.     

溶胶-凝胶法制备铁酸盐超微粒子催化剂

采用溶胶－凝胶法制备了含Zn,Ni,Co的铁酸盐超微粒子催化剂，运用DTA－TG、IR、XRD以及BET比表面测试等手段对所制备的样品进行了表征。同时，考察了铁酸盐对二氧化碳选择性氧化乙苯制苯乙烯的催化性能。结果表明：制备的铁酸盐均为尖晶石型晶体，粒子的比表面积为31．9－36．3m^2/g，晶粒大小约为30－35nm，在由二氧化碳选择性氧化乙苯制苯乙烯的反应中表现出较好的催化活性。     

多晶富镉Hg_(1-x)Cd_xTe的电沉积及Hg_(0.09)Cd_(0.91)Te薄膜的光电化学行为

本文研究了在酸性CdSO_4+HTeO_2~+6HgCl_2 电解液中多晶富镉Hg_(1-x),Cd_(?),Te(x>0.5)的电沉积过程,实现了三种离子在同一电位下共沉积的技术。对在钛基底上沉积出的薄膜进行XRD,SEM和EDAX分析,结果表明薄膜为闪锌矿型的多晶结构,分布均匀连续。考察了(1—x)=0.09时多晶薄膜在多硫氧化还原电对液中的光电化学行为,光强为100mW/cm~2时,短路光电流I_(sc)=1.88mA/cm~2,开路光电压V_(oc)=0.25V,填充因子F·F=0.22。由光电化学光谱所确定出的禁带宽度E_g=1.26eV,Mott-schottky曲线给出了电极的平带电位φfb为—1.26V(vs.SCE),从而得到开路光电压V_(oc)可能达到的最大值为0.49V。因此,多晶富镉Hg_(1-x)Cd_xTe薄膜是一种很有潜力的光活性电极材料。     

Zn∶Er∶LiNbO_3单晶的坩埚下降法生长及光谱特性

报道了Zn∶Er∶LiNbO3单晶的坩埚下降法生长工艺。通过控制晶体生长固液界面的温度梯度(30~35℃.cm-1)、晶体的生长速度(0.8~1.5 mm.h-1)、密闭Pt坩埚等条件生长了宏观无缺陷的Zn2+(3%)和Er3+(0.6%)共掺的LiNbO3单晶。用X射线衍射(XRD)和差热分析(DTA)表征了获得的晶体,并测量了晶体不同部位的吸收光谱和荧光谱。从吸收光谱以及由XRD数据计算所得的晶胞参数推断,沿生长方向Er3+在晶体中的浓度分布逐步减少。光谱数据表明,晶体底部样品的吸收强度和荧光强度要比顶部大,而对应于Er3+上能级4S3/2和2H11/2跃迁至基态4I15/2的绿光发射,晶体底部却比顶部表现出更高的上转换效率。从晶体的内部结构、缺陷情况以及Er3+的分凝现象解释了产生上述现象的内在机制。