反应时间对钨酸铋材料形貌及其可见光催化性能的影响

采用水热法在不同反应时间下制备了钨酸铋(Bi2WO6)碟状结构的光催化剂,对Bi2WO6的晶体结构、组成成分、形貌、光吸收特性和可见光催化活性等进行了表征。结果表明,反应时间影响Bi2WO6样品的形貌。水热反应6 h时,Bi2WO6样品处于非晶态,随着反应时间的增加,Bi2WO6由二维盘状结构逐渐堆积成三维碟状结构,水热反应48 h后可形成完整的微米碟。180℃水热反应48 h后制备出的Bi2WO6纳米材料具有较高的羟基自由基生成速率和较强的可见光催化活性,反应时间过长或者过短都不利于Bi2WO6可见光催化性能的提高。同时分析了不同Bi2WO6样品的可见光催化效率存在差异的原因,并且提出了不同反应时间下Bi2WO6材料的微观生长机理。     

WO3颗粒修饰TiO2纳米锥的制备及其光催化性能研究

采用水热法、浸渍法后退火的方法制备WO3-Ti O2纳米锥薄膜。紫外-可见光谱结果表明生成的WO3-Ti O2纳米锥薄膜的吸收边延长到可见光范围,达到480 nm。光催化结果表明,样品WO3-Ti O2纳米锥薄膜比纯Ti O2纳米锥薄膜具有更好的光催化性能,经过10次循环降解实验后,其降解率仍然能够达到96.8%,显示其具有良好的循环稳定性。     

Ag@AgBrH2WO4异质结光催化剂的制备及其可见光催化降解盐酸莫西沙星性能

采用超声辅助沉淀-沉积及光致还原法制备可见光响应的Ag@AgBrH2WO4异质结型光催化剂。采用X射线粉末衍射、扫描电镜和紫外-可见漫反射光谱对其进行表征。以盐酸莫西沙星为模型污染物,对该催化剂在可见光(λ>420 nm)下的催化活性和稳定性进行了评价,并分别以KI、甲醇、碳酸氢钠为空穴和自由基捕获剂研究了Ag@AgBrH2WO4的光催化反应机理。实验结果表明异质结型Ag@AgBrH2WO4光催化剂在可见光下光照20 min时对盐酸莫西沙星的降解率高达94.8%,样品经4次循环使用后催化活性基本保持不变。催化机理研究表明空穴和.O2-是光催化反应中主要的氧化性物质。     

n-n异质结Ag3PO4/Bi2WO6的制备及其增强的可见光活性

以片状Bi2 WO6为前驱体,采用沉淀法制备n-n异质结Ag3 PO4/Bi2 WO6复合材料.通过多种技术,像X射线衍射(XRD)、X射线光电子能谱(XPS)、N2吸附-脱附、扫描电镜(SEM)、透射电镜(TEM)和紫外-可见漫反射吸收光谱(UV-vis/DRS)考察所制备样品的组成、结构、形貌和光吸收性质.Ag3 PO4/Bi2 WO6复合材料由球形Ag3 PO4和片层Bi2 WO6相互交织组成,形成n-n异质结.随后,以染料罗丹明B(RhB)和苯酚(Phen)为模型分子来评价光催化剂Ag3 PO4/Bi2 WO6的可见光催化性能.与单体相比,Ag3 PO4/Bi2 WO6复合材料显示出增强的可见光催化活性.n-n异质结的形成可扩宽可见光吸收范围,促进光生电子-空穴对的分离,进而提高复合材料的可见光催化效率.     

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.     

Y_2O_3添加对Nb_2O_5低膨胀陶瓷结构与性能的影响

采用高温固相烧结法制备了Y2O3改性Nb2O5低膨胀陶瓷材料。研究了Y2O3添加量对Nb2O5陶瓷的物相组成、微观结构、气孔率、热膨胀性能、抗弯强度和抗热震性能等的影响。结果表明,经1390℃保温2 h烧成,纯Nb2O5陶瓷样品存在开裂现象,表现出低的抗弯强度和差的抗热震性能。添加2~10%Y2O3后,样品主晶相为单斜相Nb2O5,还生成了YNbO4晶相。通过添加适量Y2O3改性,可抑制Nb2O5陶瓷烧成过程中的晶粒增长和避免开裂现象,形成致密的微观结构,样品的抗弯强度和抗热震性能显著提高。Nb2O5陶瓷的热膨胀系数随Y2O3添加量的增加而逐渐增大。Y2O3添加量为6%时,样品的热膨胀系数和抗弯强度分别为1.9×10-6/℃和103.4 MPa,表现出良好的抗热震性能。     

Ce掺杂ZnO纳米晶的光催化性能研究

以Zn(NO3)3.6H2O、Ce(NO3)3.6H2O为原料,明胶为模板分散剂,采用凝胶模板燃烧法制备纯ZnO和Ce/ZnO纳米晶,利用XRD、TEM、BET、UV-Vis漫反射进行表征。以染料罗丹明B为目标降解物考察了样品的光催化活性。结果表明:产物粒子形状基本为球形,结晶良好,属六方晶系结构。相比纯ZnO,Ce/ZnO对光具有更高的吸收利用率,在紫外和可见光下对罗丹明B的降解能力均有明显提高;随Ce掺杂量的增加,样品的粒径减小,比表面积增大,罗丹明B的降解率相应增大,在紫外和可见光下降解率分别可达98.6%、78.3%,其原因在于Ce掺杂有利于在ZnO纳米粒子中心和表面之间产生电势差,实现光生电子-空穴对的有效分离。     

蛋挞状Bi_2WO_6催化剂的制备及其光催化性能

以Bi(NO3)3·5H2O和Na2WO3·2H2O为原料,CTAB为结构导向剂,在混合溶剂热法条件下合成了由纳米片组成的蛋挞状Bi2WO6晶体的新颖结构。采用XRD、FESEM、HRTEM、Raman、BET、UV-DRS等对产品进行表征。结果表明,产物为正交晶系钨铋矿型结构的蛋挞状Bi2WO6晶体,结晶度良好,其直径约为0.5~1μm。相比未添加CTAB制备的片状Bi2WO6颗粒,蛋挞状Bi2WO6样品的拉曼光特征峰、紫外-可见光吸收边发生红移,其能带隙减小至2.48 eV,比表面积增大。可见光催化降解甲基橙溶液的结果表明,蛋挞状Bi2WO6光催化效率高,可见光或太阳光照射15 min、浓度为10 mg·L-1甲基橙溶液的脱色率为100%,COD去除率为98.2%,循环使用5次之后其光催化活性并没有明显降低。     

WO3薄膜的电致变色与响应时间机理研究

采用直流反应磁控溅射方法制备了纳米WO3薄膜,研究了溅射气压对WO3薄膜的表面形貌和微结构的影响.利用X射线衍射仪和扫描电子显微镜对WO3的微结构进行了表征.采用紫外-可见分光光度计和循环伏安测试系统对样品的电致变色及响应时间性能进行了研究.结果表明,纳米WO3薄膜的微孔结构特征具有较大的比表面积,有利于改善其电致变色性能.当溅射气压为4Pa时,WO3薄膜在可见光区的电致变色平均调色范围达到了71.6％,并且其着色响应时间为5 s,漂白响应时间为16 s.     

纳米Y2O3悬浮液流变性能及注浆成型研究

以比表面积为18.1 m2/g的纳米粉体Y2O3为原料,柠檬酸铵(TAC)作为分散剂制备Y2O3悬浮液,研究TAC含量、pH值、球磨时间及固相含量对Y2 O3悬浮液流变性能的影响.结果表明:加入2.2;(质量分数)的TAC,调节悬浮液的pH值为9.4～11.5,球磨8 h可以获得分散稳定的Y2 O3悬浮液;悬浮液的粘度随固相含量的增加而增大,对不同固相含量的悬浮液进行注浆成型,发现固相含量为33;(体积分数)的悬浮液致密度最高.与传统的模压成型工艺相比,注浆成型得到的坯体中粉体颗粒分散均一.     

Crystal growth of NdAl3(BO3)4 from K2O/MoO3/Nd2O3/B2O3/KF flux

NdAl₃(BO₃)₄ single crystals were grown by the flux method and the TSSG technique using a K₂O/3MoO₃/B₂O₃/0.5Nd₂O₃/KF flux system. Light-violet clear crystals could be obtained. The effects of fluoride on the growth of NAB crystals were investigated. As the content of KF was gradually increased, the growth form of NAB was changed from the equant to the columnar and the primary crystalline region of NAB was shrinked. At the ratio of KF/K₂O = 0.75, NAB crystals could not be grown.     

一种新的非线性光学材料—Na3Sm2（BO3）3

本文采用固相反应法合成了一种新的硼酸盐化合物Na3Sm2(BO3)3,以Na2CO3-H3BO3为助熔剂,用悬挂铂丝法获得了3mm×2mm×0.5mm的透明单晶,X射线粉末衍射分析表明,该化合物属正交晶系,晶胞参数a=0.50585nm,b=1.10421nm,c=0.70316nm.红外光谱测量证实晶体结构中含有BO33-基团,粉末倍频效应测试表明该化合物具有非线性光学效应,粉末倍频信号强度接近KDP.     

Synthesis and crystal structure of oxonitrate complexes Cs[VO2(NO3)2], Cs[MoO2(NO3)3], and MoO2(NO3)2

Cs[VO₂(NO₃)₂] (I), MoO₂(NO₃)₂ (II), and Cs[MoO₂(NO₃)₃] (III) complexes have been obtained by crystallization from nitric solutions and studied by single-crystal X-ray diffraction. Complexes I and II contain infinite zigzag chains of similar compositions, [VO₂(NO₃)₂]⁻ and [MoO₂(NO₃)₂], in which V and Mo atoms form, respectively, trigonal- and pentagonal-bipyramidal polyhedra. Each of these polyhedrons also contains one terminal and two bridge O atoms and two terminal NO₃ groups which are monodentate and bidentate in complexes I and II, respectively. Complex III has an island structure and consists of Cs⁺ cations and [MoO₂(NO₃)₃]⁻ anions, in which the Mo atom is surrounded by one bidentate NO₃ group and two monodentate NO₃ groups and two terminal O atoms in the cis-positions; oxygen atoms form a polyhedron in the form of distorted octahedron. According to the ab initio calculation of isolated MoO₂(NO₃)₂ molecules in the gas phase and solution, the coordination environment of the Mo atom, similarly to the Cr(VI) atom in CrO₂(NO₃)₂, is formed by two bidentate nitrate groups and two terminal O atoms (polyhedron- twisted trigonal prism).     

Precipitation of In2O3 nano-crystallites from glasses in the system Na2O/B2O3/Al2O3/In2O3

Glasses in the system Na₂O/B₂O₃/Al₂O₃/In₂O₃ were melted and subsequently tempered in the range from 500 to 700 °C. Depending on the chemical composition, various crystalline phases were observed. From samples without Al₂O₃, In₂O₃ could not be crystallized from homogeneous glasses, because either spontaneous In₂O₃ crystallization occurred during cooling, or other phases such as NaInO₂ were formed during tempering. The addition of alumina, however, controlled the crystallization of In₂O₃. Depending on the crystallization temperature applied, the crystallite sizes were in the range from 13 to 53 nm. The glass matrix can be dissolved by soaking the powdered glass in water. This procedure can be used to prepare nano-crystalline In₂O₃-powders.     

YAl3(BO3)4: Crystal growth and characterization

The growth and characterization of YAl₃(BO₃)₄ (YAB), a potential nonlinear optical crystal for the fourth harmonic generation of Nd:YAG laser, was reported. Using top-seeded solution growth method, a YAB crystal with the dimensions of 16×16×18 mm³ was obtained from B₂O₃–Li₂O flux system. The advantages of this flux system and the growth process were discussed in detail. The as-grown YAB crystal was verified by powder X-ray diffraction. The transparency spectra indicated that the cut-off edge of the as-grown YAB was 170 nm. The fourth harmonic generation of a frequency doubled Nd:YAG laser, from 532 to 266 nm, was carried out with a YAB crystal doubler for the first time. Output pulse power obtained was 2.4 mW at 266 nm and the conversion efficiency from 532 to 266 nm was about 15.6%.     

Fluoride glasses in the ZrF4BaF2YF3AlF3 quaternary system

The quaternary system ZrF₄BaF₂YF₃AlF₃ has been investigated in order to determine the nature of the vitreous domain. Addition of aluminium fluoride to the basic ZrF₄BaF₂YF₃ ternary system results in an increase in the size of the vitreous area and a lowering of the crystallization rate.The change of density, refractive index and T_G with respect to composition has been studied. It has been shown that the substitution of Zr⁴⁺/Al³⁺ involves a change in the cationic distribution rather than in the anionic packing.     

Synthesis and X-ray diffraction study of (Cs0.5Ba0.25)[UO2(CH3COO)3] and Ba0.5[UO2(CH3COO)3]

Uranyl triacetate complexes (Cs_0.5Ba_0.25)[UO₂(CH₃COO)₃] (I) and Ba_0.5[UO₂(CH₃COO)₃] (II) are synthesized for the first time and their structures are determined by X-ray diffraction. Both compounds crystallize in the cubic crystal system. The crystal data are as follows: a = 17.3289(7) ?, V = 5203.7(4) ?³, space group I2₁3 and Z = 16 (I); a = 17.0515(8)?, V = 4957.8(4) ?³, space group I $ \bar 4 $ \bar 4 3d, and Z = 16 (II). In I and II, as in all uranyl triacetates studied earlier, the coordination polyhedron of the uranium atom is a hexagonal bipyramid whose vertices are occupied by the oxygen atoms of the uranyl and three acetate groups. The uranium-containing group belongs to the AB ₃⁰¹ (A = UO₂²⁺, B ⁰¹ = CH₃COO⁻) crystal chemical group of uranyl complexes. It was found that compound II is isostructural to the (Rb_0.50Ba_0.25)[UO₂(CH₃COO)₃] studied earlier.     

Synthesis and crystal structure of (NH4)3[UO2(CH3COO)3]2[UO2(CH3COO)(NCS)2(H2O)]

Single crystals of the compound (NH₄)₃[UO₂(CH₃COO)₃]₂[UO₂(CH₃COO)(NCS)₂(H₂O)] (I) are synthesized, and their structure is investigated using X-ray diffraction. Compound I crystallizes in the monoclinic system with the unit cell parameters a = 18.3414(6) ?, b = 16.3858(7) ?, c = 12.4183(5) ?, β = 92.992(1)°, space group C2/c, Z = 4, V = 3727.1(3) ?³, and R = 0.0253. The uranium-containing structural units of crystals I are mononuclear complexes of two types with an island structure, i.e., the [UO₂(CH₃COO)₃]⁻ anionic complexes belonging to the crystal-chemical group (AB ₃⁰¹ = UO₂²⁺, B ⁰¹ = CH₃COO⁻) of the uranyl complexes and the [UO₂(CH₃COO)(NCS)₂(H₂O)]⁻ anionic complexes belonging to the crystal-chemical group AB ⁰¹M₃¹ (A = UO₂²⁺, B ⁰¹ = CH₃COO⁻, M ¹ = NCS⁻ or H₂O).