白光LED用新型红色荧光粉KCaY(MoO4)3:Eu3+的制备及发光性能

采用高温固相法制备了新型KCaY1-x(Mo04)3:Eux红色荧光粉.利用X射线衍射(XRD)、扫描电镜(SEM)和荧光光谱技术对粉体进行了结构、表面形貌和发光性能表征.结果表明:该系列荧光粉均为四方晶系的白钨矿结构,能够被近紫外光(394 nm)和蓝光(465 nm)有效激发,产生Eu3的5 D0→7 F2特征跃迁红光发射(613 nm).对这种荧光粉作后处理,可改善其表面形貌,并提高其发光强度.该系列荧光粉在394,465 nm的吸收与目前广泛应用的近紫外和蓝光LED芯片的输出波长相匹配.因此这种荧光粉是一种可能应用在白光LED上的红色荧光粉材料.     

流动注射光度法测定水中总磷量

采用流动注射光度法测定了水中总磷量。水样经硫酸和过硫酸钾在125℃消解后,所得样品溶液中磷(PO_4~(3-))与钼酸铵生成杂多酸,经还原成钼蓝后测定其吸光度。总磷的质量浓度在1.0mg·L~(-1)以内与其吸光度呈线性关系,方法的检出限(3S/N)为0.003mg·L~(-1),测定下限(10S/N)为0.012mg·L~(-1)。方法用于测定水样中总磷的含量,相对标准偏差(n=7)在1.5%～3.0%之间,加标回收率在95.7%～102.5%之间。     

非电解质乙二醇水溶液脱硫石膏制备高强石膏

研究了常压非电解质乙二醇-水溶液脱硫石膏制备α-半水石膏工艺,对转化过程和产物特性做了表征分析;研究了不同金属离子对于转化过程的调控作用,对调控机制作了分析。结果表明脱硫石膏在乙二醇水溶液中(乙二醇浓度80 mol%,反应温度95℃)可成功转化为α-半水石膏;微量金属阳离子K~+,Mg~(2+)的添加可显著加快转化速率,而Fe~(3+)的加入则会减缓转化;添加K~+产物α-半水石膏晶体呈梭子状,添加Mg~(2+)后可获得细长α-半水石膏晶须,而添加Fe~(3+)后则获得扁平硬币状α-半水石膏晶体;金属阳离子对于转化速率和产物形貌的调控主要通过影响溶液pH及晶体表面选择性吸附实现,确切的机理还需进一步分析表征。研究内容将有助于常压非电解质醇水溶液α-半水石膏制备技术的发展,并利于脱硫石膏的高附加值资源化利用。     

Characterization and photoluminescence properties of ultrafine copper molybdate (α-CuMoO4) powders prepared via a combustion-like process

We report a simple method for preparing copper(II) molybdate (CuMoO₄) powders via a combustion-like process. A gel was first prepared by the polymerizable complex method, where citric acid was used as a complexing and polymerizing agent and nitric acid was used as an oxidizing agent. The thermal decomposition behavior of the (CuMo)-precursor gel was studied by thermogravimetry–differential thermal analysis (TG–DTA), Fourier transform infrared spectroscopy (FTIR), and X-ray diffraction (XRD). We observed that the crystallization of CuMoO₄ powder was completed at 450°C. The obtained homogeneous powder was composed of grains with sizes in the range from 150 to 500 nm and exhibited a specific surface area of approximately 5 m2/g. The average grain size increased with increasing annealing temperature. The as-prepared CuMoO₄ crystals showed a strong green photoluminescence emission at room temperature under excitation at 290 nm, which we mainly interpreted on the basis of the Jahn-Teller effect on [MoO₄2- ] complex anions. We also observed that the photoluminescence intensity increased with increasing crystallite size.     

防水剂对石灰-偏高岭土修补砂浆性能的影响

以石灰和偏高岭土为主要材料,制备一种适用于岩土类建筑的修补砂浆.用桐油和硬脂酸钙两种防水剂来改善砂浆的耐水性,研究桐油和硬脂酸钙对砂浆强度、反应过程、吸水率和软化系数、干燥收缩的影响,并通过XRD和SEM对砂浆进行物相分析和微观形貌观测.结果表明:桐油和硬脂酸钙可以显著提高石灰-偏高岭土砂浆的耐水性,可使吸水率下降至2.5%以下;桐油和硬脂酸都会阻碍偏高岭土的火山灰反应,在一定程度上降低砂浆的强度,但28d的抗压强度仍在5 MPa以上,达到天然水硬性石灰NHL5的强度等级;桐油和硬脂酸钙会影响石灰-偏高岭土砂浆的微观形态和结构,桐油使产物的颗粒更细小、更致密,硬脂酸钙则会使产物结构比较疏松.综合考虑砂浆强度、耐水性等因素,得出桐油和硬脂酸钙的最佳掺量分别为5%和1.5%.     

ChemInform Abstract: In Search of Chemical Frustration in the Ca—Cu—Cd System: Chemical Pressure Relief in the Crystal Structures of Ca5Cu2Cd and Ca2Cu2Cd9.

Two new compounds in the Ca—Cu—Cd system of nominal composition Ca₅Cu₂Cd and Ca₂Cu₂Cd₉ are synthesized from nearly stoichiometric mixtures of the elements (1100 °C, 48 h).     

Highly Chemoselective Calcium‐Catalyzed Propargylic Deoxygenation

A calcium‐catalyzed direct reduction of propargylic alcohols and ethers has been accomplished by using triethylsilane as a nucleophilic hydride source. At room temperature a variety of secondary propargylic alcohols was deoxygenated to the corresponding hydrocarbons in excellent yields. Furthermore, for the first time, a catalytic deoxygenation of tertiary propargylic alcohols was generally applicable. The same protocol was suitable for an efficient reduction of secondary as well as tertiary propargylic methyl, benzyl and allyl ethers. Substrates containing an additional keto‐, ester or secondary hydroxyl function were reduced with exceptional chemoselectivity at the propargylic position.