球形Cu2O修饰Bi2WO6层状微球的制备及其光催化制取氢气和烷烃的研究

采用水热法制备了Bi2WO6层状微球,通过还原沉淀法在Bi2WO6层状微球内部薄片表面修饰纳米球形Cu2O而制备Cu2O/Bi2WO6复合催化剂.利用X-射线衍射(XRD)、场发射扫描电子显微镜(FESEM)、透射电子显微镜(TEM)、紫外-可见漫反射光谱(UV-visDRS)、荧光光谱(PL)等对复合光催化剂的晶体结构、形貌、光响应性能等进行表征.在Cu2O/Bi2WO6中,100nm左右Cu2O不均匀地附着在1.5μmBi2WO6层状微球的内部的纳米薄片上.通过Cu2O的复合,可以显著提高Cu2O/Bi2WO6对紫外-可见光谱的吸收能力、光生电子-空穴对的分离效率及光催化活性.以丙酸为电子供体,考察了紫外光照射下Cu2O/Bi2WO6分解水制备氢气和烷烃的性能,结果表明:5wt;Cu2O/Bi2WO6的光催化产生氢气和烷烃的性能最佳.     

可磁分离的"核-壳"结构Fe3O4@SiO2/Bi2WO6/Ag2O催化材料的制备及光催化性能研究

采用沉淀-沉积法制备了磁性Fe3O4@SiO2/Bi2 WO6/Ag2O催化材料,利用XRD、SEM和UV-Vis-DRS光谱对其组成、形貌和光吸收特性进行表征.以氙灯模拟可见光,以罗丹明B为模拟污染物对所得催化剂进行性能评价,考察了不同Ag2O复合量对Bi2WO6光催化剂反应活性的影响.结果表明,Fe3O4@SiO2/Bi2WO6/Ag2O的光催化活性明显优于纯Bi2 WO6,当Ag2 O的复合量为0.6;时,催化剂的活性最好.催化剂的活性增强增强机理分析表明,Ag2O的复合有效地降低了Bi2WO6的光生电子-空穴复合率,增加了Bi2WO6的可见光吸收范围.此外,该催化材料可进行磁分离,易于回收重复利用.     

Bi3Ti4O12/α-Bi2O3/TiO2复合光催化剂的制备及其可见光催化活性研究

以工业二氧化钛(TiO2)、五水合硝酸铋(Bi(NO3)3·5H2O)为原料制备了Bi3Ti4O12/α-Bi2O3/TiO2复合光催化剂.采用X射线衍射(XRD)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)、傅里叶变换红外光谱(FT-IR)、紫外-可见吸收光谱(UV-Vis)、荧光光谱(PL)等表征方法对光催化剂结构进行分析,表明复合样品中形成了Bi3 Ti4 O12/α-Bi2 O3/TiO2异质结结构,其禁带宽度减小、吸收带边红移,光催化效率有明显提高.以亚甲基蓝为目标污染物评价其光催化活性,TiO2与Bi(NO3)3·5H2O质量比为1:2.5,煅烧温度为600℃,煅烧时间为5 h时,复合样品光催化活性最佳,在12 W LED灯下,180 min后对浓度为10 mg/L的亚甲基蓝溶液的去除率达96.8;.     

不同酸性助剂水热合成钨酸铋的制备及光催化性能研究

以Bi(NO3)3·5H2O、Na2WO4·2H2O为原料,NaOH为矿化剂,采用水热法合成Bi2WO6纳米晶体,并使用XRD、SEM、TEM、DRS和低温氮吸附等手段对样品进行表征,考察了其可见光降解RhB的催化性能,分析了不同酸性助剂CH3 COOH和HNO3对水热法合成Bi2WO6光催化剂的影响.实验结果表明,不同酸性助剂对Bi2WO6样品的形貌和可见光催化活性均有较大影响.HNO3的添加抑制了花状微球的形成,使Bi2WO6样品的紫外-可见光吸收边发生红移,比表面积增大.光催化测试结果表明,以HNO3为酸性助剂时所制备样品的光催化活性最高,添加CH3COOH则相对降低.     

Ag3PO4/TiO2复合催化剂的制备及光催化性能研究

为提高纳米TiO2的光催化降解性能和稳定性,采用两步水热法制备具有高催化性能的Ag3PO4/TiO2复合催化剂,采用XRD、SEM、EDS、XPS、TEM等仪器对其表面微观形貌和形态大小、表面元素组成、物相结构等进行表征,并研究了TiO2的比表面积和Ag3PO4颗粒尺寸大小对Ag3PO4/TiO2光催化性能的影响.以亚甲基蓝(MB)和苯酚为目标降解物来考察复合光催化剂的光催化性能.结果表明:1h后Ag3PO4、TiO2、Ag3PO4/TiO2对亚甲基蓝的降解率为25;、42;、92;;复合光催化剂Ag3PO4/TiO2经过5次光催化降解实验后,对亚甲基蓝的降解率仍可达78;.     

CuO/SnO2/TiO2复合光催化剂的制备及光催化性能

采用硬脂酸法制备了CuO/SnO2/TiO2复合光催化剂,采用XRD及TG-DTA分析对其物相和热稳定性进行了表征,并通过苯酚的光催化降解行为对所制备催化剂的活性进行了评价.结果表明,经500 ℃热处理的CuO/SnO2/TiO2复合光催化剂属于单一的锐钛矿相,且铜、锡氧化物的引入抑制了TiO2的结晶和晶粒的生长.当催化剂组成为Cu:Sn:Ti=0.25:5:100(物质的量比),焙烧温度为500 ℃,催化剂投加量为0.5 g·L-1,溶液pH为4.0时,经3 h光催化反应苯酚的降解率达97.1;.     

Ag/Bi2S3/Bi2WO6复合催化剂合成及光催化性能研究

以硝酸铋、钨酸钠和硫脲为起始原料,采用一步水热法成功合成Bi2 S3/Bi2 WO6光催化剂,采用光还原法在Bi2S3/Bi2 WO6表面沉积贵金属Ag.采用XRD、XPS、FESEM、TEM和UV-Vis-DRS等手段对Bi2S3/Bi2WO6和Ag/Bi2S3/Bi2WO6进行表征,并以罗丹明B和苯酚作为模型污染物对其光催化性能进行研究.结果证明,耦合Bi2S3可以提高Bi2WO6催化剂的光催化活性,Ag沉积使得其光催化性能进一步提高,且Ag的沉积量与催化剂的活性关系密切,其中5; Ag/Bi2S3/Bi2WO6的光催化效果最好.此外,结合活性物种检测和能带结构分析,对Ag/Bi2S3/Bi2WO6的光催化活性增强机理进行了分析.     

Ag3 PO4量子点修饰Ag3 PO4/Bi2 WO6异质光催化剂的构筑及其可见响应活性增强机制

采用水热法制备了三维分级球形结构的Bi2 WO6,在此基础上采用沉淀-沉积法将Ag3 PO4量子点(QDs)沉积在Bi2 WO6的表面,成功获得Ag3 PO4/Bi2 WO6异质复合材料光催化剂.借助XRD、FE-SEM、TEM、UV-Vis-DRS等技术对所得Ag3 PO4/Bi2 WO6异质复合材料光吸收性能、形貌和组成进行了系统表征,并以次甲基蓝(MB)和苯酚(Ph)的光催化降解为探针反应,探讨了Ag3 PO4 QDs表面沉积对Bi2 WO6光催化性能的影响.结果表明,尺寸约为10 nm左右的Ag3 PO4 QDs均匀的沉积在Bi2 WO6的表面,二者形成新颖的Ag3 PO4/Bi2 WO6异质结构.活性实验结果表明,与纯Bi2 WO6相比异质催化剂的活性显著增强,当Ag3 PO4与Bi2 WO6复合比为1:1时催化活性最高,其降解Ph的表观速率常数(kapp/min-1)约为纯Bi2 WO6的7倍.     

水热合成Cu-Bi2WO6及其光催化性能研究

以Bi(NO3)3·5H2O和Na2WO4·2H2O为原料,NaOH为矿化剂,CuCl2和CuSO4为铜源水热法离子掺杂合成Bi2WO6粉体,并使用XRD、SEM、UV-VIS、XPS对其进行表征,分析了不同铜源离子掺杂Bi2WO6以及掺杂量对所制备样品光催化性能的影响.结果表明,以CuCl2为铜源离子掺杂Bi2WO6的样品粒径减小,吸收边红移.掺杂后的铜以中Cu2和Cu+两种电子形式存在.光催化测试结果表明,以CuCl2为铜源且掺入量为1.5mol;时所制备的Bi2WO6样品的光催化活性最高.     

α-Fe2O3/TiO2光催化剂的制备及可见光催化降解罗丹明B的研究

采用浸渍法制备不同掺杂量的负载型光催化剂 α-Fe2O3/TiO2,通过XRD、SEM-EDX、XPS和N2-sorption等手段对其进行表征,并研究其在可见光照射下对罗丹明B的降解性能.考察了不同掺杂量的复合纳米粒子、不同浓度的H2O2溶液、不同pH等条件对可见光降解罗丹明B的影响.结果表明,复合α-Fe2O3/TiO2催化剂的光催化活性均高于单一的α-Fe2O3或TiO2,其中α-Fe2O3掺杂量为6.0wt;的α-Fe2O3/TiO2的光催化活性和光降解稳定性最好.     

(C2N2H10)2Mg(HP2O7)2·2H2O synthesis and crystal structure

(C₂N₂H₁₀)₂Mg(HP₂O₇)₂·2H₂O, is a new inorganic organic hybrid structure. It has been synthetized using wet chemistry. Its crystal structure consists of cis- and trans-edge sharing [MgO₄(H₂O)₂] octahedra resulting in chains, which are linked via [HP₂O₇] units to form [Mg(HP₂O₇)₂(H₂O)₂]⁴⁻ layers. The Mg²⁺ cations and the ethylendiammonium cations are located on centers of inversion. The ethylendiammonium cations are alternately located in the interlayer space. The cohesion of the crystal is well ensured by coulombic interactions between anions and cations and by several hydrogen bonds. The diphosphate anion shows an eclipsed conformation.     

Crystal structure of Rb2[GeO2(OH)2]·2H2O

Single crystals of Rb₂[GeO₂(OH)₂] · 2H₂O are studied by X-ray diffraction. The crystals belong to the orthorhombic system, sp. gr. Pna2₁, a = 13.523(6) Å, b = 8.143(4) Å, c = 13.407(6) Å, Z = 8, R ₁ = 0.0506. In [GeO₂(OH)₂]^2? anions, the Ge-O distances (1.71–1.73(1) Å) are shorter than the Ge-OH distances (1.76–1.80(1) Å). Anions are linked to each other by pairs of hydrogen bonds to form infinite chains. The chains are linked by hydrogen bonds involving water molecules to form a 3D structure. The assignment of the bands in the IR spectrum of the compound under study is performed.     

通过SiO2涂层改善BaSi2O2N2∶Eu2荧光粉的热性能

本文研究了SiO2涂层对BaSi2O2N2∶ Eu2蓝绿色荧光粉发光性能和热性能的影响.采用溶胶-凝胶法制备了SiO2包覆的BaSi2O2N2∶Eu2+蓝绿色荧光粉.实验结果表明,最佳镀膜量为6wt;,当镀膜量大于此值时,荧光粉亮度迅速降低.涂覆SiO2后,在150℃下BaSi2O2 N2∶Eu2荧光粉的热猝灭性能提高了2.4;,在500℃热降解后荧光粉的发光性能提高了15;.SiO2涂层显著提高了BaSi2O2N2∶Eu2+荧光粉的热稳定性.SiO2涂层的作用机理是在荧光粉表面和氧化气氛之间形成阻挡层,保护Eu2的发光中心在热加热过程中不被氧化.     

Optical properties of the germanate melilites Sr2MgGe2O7, Sr2ZnGe2O7 and Ba2ZnGe2O7

Refractive indices and their dispersion in the wavelength range from 365 nm to 2325 nm and transmission ranges of the tetragonal melilite‐type germanates Sr₂MgGe₂O₇, Sr₂ZnGe₂O₇ and Ba₂ZnGe₂O₇ were determined. The uniaxial positive crystals Sr₂MgGe₂O₇ and Ba₂ZnGe₂O₇ both offer the possibility for phase matched second harmonic generation, a detailed analysis of phase matching conditions is given. The refractive indices of Sr₂ZnGe₂O₇ show an isoindex (isotropic) point at 467 nm. The investigation was performed on Czochralski grown large single crystals. The crystal structure of all three germanates were determined by means of X ‐ray diffraction. The results corroborate unmodulated melilite‐type structures at room temperature. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Identification of a new family of diphosphate compounds, AI2BII3(P2O7)2: Structures of Ag2Co3(P2O7)2, Ag2Mn3(P2O7)2, and Na2Cd3(P2O7)2

Syntheses and single-crystal X-ray structural results are reported for three new mixed diphosphates of the family A^I ₂B^II ₃(P₂O₇)₂; Ag₂Co₃(P₂O₇)₂ (I), Ag₂Mn₃(P₂O₇)₂ (II), and Na₂Cd₃(P₂O₇)₂ (III). All crystallize in the triclinic system, space group P1 bar: (I) a = 5.351(4), b = 6.375(4), c = 16.532(4) Å, = 80.83(6) = 81.45(4), = 72.87(5)°, V = 528.9(6) ų, Z = 2, D _calc = 4.649 mg/m³, R/Rw = 0.0428/0.0548 for 3949 obs. reflns; (II) a = 5.432(7), b = 6.619(6), c = 16.51(3) Å, = 80.78(8) = 82.43(9), = 72.82(7)°, V = 557.7(13) ų, Z = 2, D _calc = 4.338 mg/m³, R/Rw = 0.0679/0.1303 for 2100 obs. reflns and (III) a = 5.67(3), b = 7.08(4), c = 7.90(4) Å, = 77.0(2), = 82.5(2), = 67.8(2)°, V = 286(3) ų, Z = 2, D _calc = 4.249 mg/m³, R/Rw = 0.0307/0.0342 for 1945 obs. reflns. (I) and (II) are isostructural but (III) is of a different type. All three structures are characterized by layers of P₂O₇ groups alternating with layers of mixed metal atoms. Differences are seen in the conglomerate bonding patterns of B atoms and in the irregular geometry of Ag in (I) and (II) compared to the octahedral bonding seen for Na in (III). The differences in structure may be understood in terms of the ratios of the ionic radii of A and B atoms.     

Crystal structure of bis 4-benzyl piperidinium monohydrogenmonophosphate pentahydrate, [C6H5CH2CHCH2CH2NH2CH2CH2]2HPO4·5H2O

The salt bis 4-benzyl piperidinium monohydrogenmonophosphate pentahydrate is orthorhombic with the following unit cell dimensions: a = 11.235(2) Å, b = 27.924(6) Å, c = 9.321(4) Å space group Pca2₁ with Z = 4. The structure was solved by the Patterson method and refined to final R value of 0.049 for 1802 independent reflections. The flack parameter is 0.14 with an e.s.d. of 0.23. The structure consists of infinite parallel two-dimensional [110] planes built of mutually connected ions and water molecules by strong O—H,...,O and N—H,...,O hydrogen bonding. There are no contacts other than normal van der Waals interactions between the layers.     

Synthesis and characterization of (NH4)2CuBr2Cl2·2H2O crystals

Single crystals of a new compound, (NH₄)₂CuBr₂Cl₂.2H₂O, were grown from saturated aqueous solution at room temperature by slow evaporation method. The grown crystals were characterized through elemental, powder XRD, thermal and DSC analyses and FTIR and far IR spectra. The elemental analysis and the decomposition pattern formulated using the TG‐DTG studies confirm the stoichiometry of the compound. The crystallinity of the compound is confirmed from the powder XRD pattern. A preliminary single crystal X‐ray diffraction structural analysis reveals that the title compound belongs to the orthorhombic system with a = 7.7466 Å, b = 7.783 Å and c = 8.1211 Å. The low temperature DSC shows thermal anomalies at –161.1, –156.5, –152.4, –145.2, –134, –18.5, and 1.4°C during the heating run and at –4.3, –54.8, –66.1, –90.6, –109.7 and –147.2 °C during the cooling run. The thermal hysterses indicate first order phase transitions in the title compound at these temperatures. The FTIR spectra were used to assign the characteristic vibrational frequencies due to NH₄⁺, CuX₄^2– ions and other chemical bonds. The effect of substitution of two bromine atoms on the phase transitions of a closely related crystal, diammonium tetrachloro cuprate dihydrate is also discussed. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Oxygen-conducting compounds with La2Mo2O9 structure in the ternary system La2Mo2O9-Sm2W2O9-Sm2Mo2O 9 + : Synthesis and properties

Polycrystalline samples in the ternary system La₂Mo₂O₉-Sm₂W₂O₉-Sm₂Mo₂O ₉ ⁺ were synthesized in air. The region of the existence of compounds with the lanthanum molybdate (La₂Mo₂O₉) structure in this system was determined. The polymorphism of the synthesized compounds was studied. Doping with samarium or with samarium and tungsten was shown to lead to the suppression of the transition between the monoclinic and cubic phases α → β and the appearance of the transition β _ms → β between two cubic phases. In samples with a high samarium content, the phase transition β _ms → β manifests itself as significant anomalies in the temperature dependences of the dielectric permeability and electric conductivity. An increase in the concentration of samarium in the samples leads to a substantial decrease in the conductivity compared with the nondoped compound La₂Mo₂O₉.     

Structure of {Pb[S2CN(C2H5)2]2(1,10-phenanthroline)}2

Lead (II) nitrate reacts with 1,10-phenanthroline and sodium diethyldithiocarbamate in water to produce yellow bisdiethyldithiocarbamata 1,10-phenanthroline lead(II). Crystals from water are triclinic, space group $P\bar 1$ (#2),a=10.53(2) Å,b=11.050(12)Å,c=24.74 (3) Å, α=94.71 (9)⁰, β=98.15(11)^o, γ=114.11(9)^o,V=2569(6) ų,Z=2. Each lead atom has approximate pentagonal pyramid coordination geometry through the nitrogens of a phenathroline and sulfurs of two dithiocarbamates. Additionally, complexes form loose dimers in which lead atoms are weakly coordinated to a sulfur in an adjacent complex. IR and proton nmr spectrum of the complex are consistent with the solid state structure.