氨改性二氧化钛的制备及可见光催化性能研究

以工业TiO2为原料,在不同氨气浓度下采用热处理法制备了N掺杂的光催化剂.用XRD,TEM,XPS,UV-visDRS和PL等对其结构进行了表征,以亚甲基蓝为目标化合物,评价了其可见光催化活性.结果表明,当氨气浓度为99;时,工业TiO2在500℃下煅烧3h后,具有优良的可见光催化活性,对亚甲基蓝的去除率达到93;.当煅烧温度升高到600℃后,TiO2的晶相由锐钛矿向金红石转变,随着煅烧过程中氨气浓度的增加,所制备的催化剂对亚甲基蓝的降解显著增加.     

Sm2O3/TiO2对亚甲基蓝染料的光催化降解行为研究

采用浸渍法制备Sm2O3掺杂TiO2的负载型光催化剂Sm2O3/TiO2,考察其在紫外可见光区对亚甲基蓝的光降解行为.利用XRD、N2吸附、SEM、TEM、XPS和ICP-OES等手段表征Sm2O3/TiO2样品,考察Sm2 O3掺杂量和亚甲基蓝浓度对亚甲基蓝紫外光降解活性的影响和催化剂Sm2O3/TiO2的催化稳定性.结果表明,Sm2O3/TiO2对亚甲基蓝的紫外光降解活性高于TiO2,这归因子掺杂Sm2O3引起TiO2的晶体缺陷.这种晶体缺陷作为光生电子和空穴的陷阱实现光生电子-空穴对的有效分离,从而提高Sm2O3/TiO2的光催化活性.Sm2O3/TiO2对亚甲基蓝的光降解活性随着Sm2O3掺杂量的增加先增大后减小,随着亚甲基蓝浓度的增大而减小.Sm2 O3掺杂量5.0wt;的Sm2O3/TiO2对亚甲基蓝紫外光降解的7次循环实验未出现明显失活.     

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;.     

生物质改性纳米TiO2的制备及其结构表征

采用溶胶-凝胶法制备了系列生物质改性复合纳米TiO2.以亚甲基蓝溶液为模拟污染物,考察了其可见光催化活性,并确定了最佳制备工艺.通过X射线光电子能谱(XPS)、X射线衍射(XRD)、场发射扫描电镜(FESEM)、紫外-可见漫反射光谱(UV-Vis-DRS)、荧光光谱(PL)等手段对催化剂样品进行了表征.实验结果表明,催化剂对亚甲基蓝的光催化降解适应一级反应动力学,复合TiO2和纯TiO2的反应速率常数分别为0.4990 h-1和0.0305 h-1,且复合催化剂实现了C、N、S、P、K等多元素的共掺杂.相比纯TiO2,复合TiO2的比表面积增大,结晶度升高,光生载流子复合率降低,吸收边带红移,禁带宽度窄化了0.09 eV.     

g-C3N4/ZnO复合光催化剂的制备及其光催化活性

以硝酸锌、三聚氰胺、氢氧化钠为原料,采用回流法合成g-C3N4/ZnO复合光催化剂.利用傅里叶红外光谱(FTIR),X射线衍射(XRD),扫描电子显微镜(SEM),紫外可见漫反射光谱(UV-Vis DRS)及N2吸附-脱附(BET)等技术对所合成样品的组成和形貌进行表征.在模拟太阳光条件下,以亚甲基蓝为模拟污染物评价催化剂的活性.结果表明,g-C3N4加入量为5wt;,煅烧温度500℃,煅烧时间2 h条件下制备的复合光催化剂具有最佳的光催化活性.5wt;g-C3N4/ZnO复合光催化剂在反应40 min时对亚甲基蓝的降解率可达到98.5;,其光催化降解速率为纯ZnO的2.8倍.     

多级孔TiO2/ZSM-5催化剂的孔道效应对 亚甲基蓝催化降解性能影响

以廉价凹凸棒石为原料,通过调控介孔模板剂聚乙二醇(PEG-1000)用量用水热合成法制得多级孔ZSM-5分子筛,并用溶胶-凝胶法制备了TiO2/ZSM-5光催化剂.通过FT-IR、XRD、SEM和N2吸附-脱附对多级孔TiO2/ZSM-5光催化剂的官能团、晶体结构、形貌和孔道特征进行表征,并对典型的亚甲基蓝印染废水进行光催化实验,考察模板剂用量和TiO2负载量对光催化剂孔道效应和催化性能的影响.结果表明:ZSM-5分子筛作为载体,其介孔体积与介孔模板剂PEG用量成正比,调节PEG用量可定向控制载体的孔道结构;TiO2负载量在一定程度上影响光催化效率和载体孔体积.当PEG为0.16 g,TiO2负载量为10;时,多级孔TiO2/ZSM-5具有良好光催化活性,光照40 min光催化降解率可达90;.     

以偏钛酸浆料制备氮掺杂纳米二氧化钛及其可见光催化性能研究

以工业偏钛酸为前驱体、尿素为氮源,混合煅烧制备了不同氮含量的TiO2光催化剂(记为TiO2-xN-温度).用傅里叶红外光谱(FT-IR)、X射线光电子能谱(XPS)、X射线衍射(XRD)、透射电子显微镜(TEM)、荧光光谱和紫外-可见光漫反射吸收光谱(UV-Vis/DRS)等对催化剂进行了表征.以亚甲基蓝为目标污染物,评价了样品的可见光光催化活性.结果表明,当催化剂中尿素与TiO2质量比为3∶1,煅烧温度为400℃(即TiO2-3N-400℃)时制得的样品活性最高.500 W的长弧氙灯照射4h,对亚甲基蓝降解率达到93.9;.     

Ag掺杂Sm2O3/TiO2对甲基橙光降解性能的影响

采用光沉积法制备Ag掺杂的光催化剂Ag-Sm2 O3/TiO2,并对其在紫外光区对甲基橙的光降解行为进行了研究.采用XRD、FT-IR、N2吸附、SEM、TEM和XPS等手段对样品Ag-Sm2 O3/TiO2进行了表征,考察了Sm2 O3和Ag掺杂量对甲基橙紫外光降解活性的影响和催化剂Ag-Sm2 O3/TiO2的催化稳定性.结果表明,Sm2 O3/TiO2在紫外光照射下对甲基橙的光降解活性随着Sm2 O3的增大而减小;与样品Sm2 O3/TiO2相比,催化剂Ag-Sm2 O3/TiO2对甲基橙具有更好的紫外光降解活性,其催化活性随着Ag掺杂量的增加而减小.Ag和Sm2 O3掺杂量均为3.0wt;的催化剂Ag(3)-Sm2 O3(3)/TiO2对甲基橙紫外光降解的活性最高,在相同条件下的6次循环实验未出现明显失活.     

芦苇杆炭负载N掺杂TiO2的制备及光催化活性研究

以钛酸丁酯、乙酰丙酮、盐酸为原料,通过溶胶凝胶法合成芦苇杆炭(经酸处理)负载N掺杂TiO2,利用X射线衍射(XRD)、扫描电子显微镜(SEM)、激光粒度仪等技术对样品的形貌和结构进行分析表征,以亚甲基蓝作为底物,氙灯光照下的光催化降解实验评测其光催化活性.实验证明,当N/Ti=1at;,退火温度350℃时,退火3h后的芦苇杆炭负载TiO2 1N对亚甲基蓝光降解性能可达92;,同时,该复合光催化剂对苯酚、对氯甲苯及硝基苯都具有一定的光催化效果.     

ZnFe2O4的制备及光催化性能研究

以乙二醇作为溶剂,采用溶剂热法制备ZnFe2O4,进一步通过控制煅烧温度获得具有不同晶粒尺寸的ZnFe2O4晶体.XRD和SEM分析表明,ZnFe2O4是由纳米尺寸的微晶构成的球状颗粒,粒径约200 nm,属于正尖晶石结构.UV-vis测定表明ZnFe2O4在紫外及可见光范围均有吸收,禁带宽度为1.60 ～2.18 eV,制备的温度条件对禁带能隙产生一定的影响.进一步以亚甲基蓝染料为研究对象考察了不同温度条件下制备的ZnFe2O4光催化活性,实验结果表明500℃煅烧的ZnFe2O4具有较高的染料降解率,当染料初始浓度10 mg/L,初始pH为11,催化剂用量为0.04 g/L,300 W汞灯照射2h,亚甲基蓝的降解率可达到96.8;,降解反应符合一级动力学.由于制备的ZnFe2O4具有磁性,重复使用三次亚甲基蓝的降解率仍可达到83.3;.     

Syntheses and structures of N-phenylmaleimidetriazoles and by-products

The syntheses, properties, and structures of N-phenylmaleimidetriazole derivatives are described. Intermediates and by-products are also discussed. 1b. a = 43.997(7) Å, 5.7610(9) Å, 8.245(1) Å, = 99.339(4), C₂/c; 2a. a = 13.646(4) Å, b = 7.744(2) Å, c = 10.612(3) Å, = 91.979(6), P2₁/c. 3a. a = 22.245(1) Å, b = 22.245(1) Å, 10.010(1) Å, P42/n. 3a. a = 11.727(2) Å, b = 14.075(3) Å, c = 16.080(3) Å, = 105.859(3), = 105.331(3), = 98.187(3), P-1. 3b. a = 8.561(3) Å, b = 14.755(5) Å, c = 22.771(7) Å, = 97.006(5), P2₁/c. 3c. a = 10.500(2) Å, b = 12.189(2) Å, c = 13.040(2) Å, = 109.091(3), = 106.089(3), = 101.022(3), P-1. 8a. a = 16.389(8) Å, b = 5.749(3) Å, c = 19.316(3) Å, = 97.467(9), P2₁/n. 8b. a = 5.822(2) Å, b = 10.114(3) Å, c = 16.705(4) Å, = 84.681(5), = 82.840(5), = 75.769(4), P-1. 9b. a = 11.251(1) Å, 13.335(3) Å, 13.376(3) Å, = 102.456(4), P2₁/n. 9c. a = 15.836(3) Å, b = 8.236(2) Å, c = 5.447(3) Å, = 92.551(3), P2₁/c. 10a. a = 13.177(2) Å, b = 14.597(2) Å, c = 5.5505(8) Å, = 110.979(2), Cc. 11a. a = 14.720(2) Å, b = 13.995(2) Å, c = 38.245(6) Å, = 94.430(3), P2₁/n. 12b. a = 15.067(5) Å, b = 20.378(6) Å, c = 8.669(5) Å, = 99.16(4), = 99.32(3), = 105.23(3), P-1. 13b. a = 8.2824(6) Å, b = 10.5245(7) Å, c = 15.518(1) Å, = 92.305(1), = 100.473(1), = 100.124(1), P-1. 15a. a = 15.357(3) Å, b = 7.778(2) Å, c = 22.957(2) Å, Pbca. 16b. a = 18.0384(4) Å, b = 12.474(3) Å, c = 20.078(5) Å, Pbca.     

Sol-gel synthesis and characterization of adsorbent and photoluminescent nanocomposites of starch and silica

Using sol-gel method, mesoporous and photoluminescent silica nanocomposites of soluble starch have been synthesized and characterized. Different ratios of H₂O, TEOS and EtOH were used at fixed template (soluble starch) and catalyst (NH₄OH) concentrations to obtain materials of different performances in terms of heavy metal binding from a solution which has been monitored using Cd(II) as representative divalent heavy metal ion. Optimum material was obtained when H₂O, TEOS and EtOH were used in 14:1:2 ratio. This sample was not only an efficient metal ion adsorbent but also had an intense luminescence in ultra-violet region and potentially may be used in silicon-based UV-emitting devices. Metal binding by the material was further enhanced after calcination (at 800 °C in air) while its luminescence had a multipeak profile in UV-visible region. In a batch adsorption study, calcined hybrid composite (0.25 g/L) could remove 98.5% Cd(II) from 100 mg/L Cd(II) solution in 2 h. The chemical, structural and textural characteristics of the synthesized materials have been investigated using Fourier Transform Infrared Spectroscopy (FTIR), X-rays Diffraction (XRD), Thermal Analysis (TGA/DTA), Photoluminescence (PL), Brunauer-Emmett-Teller Analysis (BET) and Scanning Electron Microscopy (SEM).     

Crystal and molecular structures of benz-p-nitroanilide and benz-p-methoxyanilide

The crystal structures of the two carboxylic amides C₁₃H₁₀N₂O₃ (I) and C₁₄H₁₃NO₂ (II) have been determined by direct methods and refined by full-matrix least squares. The predominant structural feature is the hydrogen bonding (N-H?O=C) which influences the conformations of both structures.     

Chemistry and Electrocrystallization of Organic Metals and Superconductors

Abstract

Considerable variation in the conditions of electrochemical crystal growth of TMTSF₂X (i.e., constant current versus constant potential, ambient versus inert atmosphere, etc.) and in the purity of the constituents (donor, electrolyte, solvent) does not significantly affect the unusual low-temperature properties of this class of materials. Our results suggest that the electrocrystallization procedure may be self-purifying by selecting for conducting crystal phases with constituents having specific oxidation potentials and solubility properties. However, doping solutions with structurally and chemically similar constituents (i.e., TMTTF, and IO^? ₄ in CIO^? ₄) leads to their incorporation in the crystal structure where they have a profound effect. Several mole percent of these dopants suppress superconductivity in the PF^? ₆ and CIO^? ₄ salts, and increase and broaden the metal-insulator phase transition.     

晶体中负离子配位多面体结晶方位、形变与晶体压电、铁电性

本文研究了压电、铁电晶体中负离子配位多面体的结晶方位与形变,提出了压电晶体中同一种负离子配位多面体的结晶方位是一致的.在铁电晶体中,负离子配位多面体发生形变,伴随着晶体发生顺电-铁电相变,并从这一基本过程出发,对铁电体相变的形成机理进行了讨论.     

Structural and spectral studies of N-trans-cinnamylidene-m-toluidine and N-trans-cinnamylidene-m-chloroaniline

N-trans-cinnamylidene-m-toluidine (1) C₁₆H₁₅N, and N-trans-cinnamylidene-m-chloroaniline (2) C₁₅H₁₂NCl form isomorphous crystals which are monoclinic, space group P2_l/c, with unit cell dimensionsa=5.967(2),b=13.793(3),c=15.048(5) Å, =91.97(3)° anda=5.868(2),b=13.788(4),c=15.191(4) Å, =91.87(3)°, respectively. The single-crystal X-ray structure determinations of the title compounds revealtrans structures. Ring (A) C_10–15 and ring (B) C_1–6, are practically planar in both structures with dihedral angels of 61.3(3) and 63.6(2)°, respectively.¹H nmr, u.v. and i.r. spectra are also reported.     

Melting and short-range order in liquids and glasses

A theory is proposed to explain two-dimensional melting based on the gauge-invariant Lagrangian with spontaneous breaking (Higgs mechanism) or the SU(2) gauge field to U(1) symmetry. The first-order phase transition in two-dimensional melting may be strongly related to the asymptotic freedom-like interaction of the SU(2) gauge field in the case when the distance between each excited disk is shorter than a critical length, 2/ boxv;mboxv, near the melting temperature.     

Biocrystallization in Bacterial and Fungal Cells and Spores

A series of X-ray diffraction experiments were performed for the first time to study stress-induced biocrystallization (structural response to stress) in the bacteria E. coli, the spore-forming bacteria Bacillus cereus, and in cells and spores of the mycelial fungus Umbelopsis ramanniana. High-intensity areas with spacings of 90 and 44 Å are indicative of a periodically ordered arrangement (most likely nanocrystalline) of the bacterial nucleoid. For the starved bacteria Bacillus cereus, a peak at a spacing of 45 Å is also assigned to nanocrystalline complexes of DNA with the Dps protein. The spores of the fungus Umbelopsis ramanniana VKM F-582, as well as the spores of Bacillus cereus, form ordered arrays of DNA molecules with DNA-condensing acid-soluble proteins SASPs. Starved dehydrated mycelial cells of the fungus Umbelopsis ramanniana form ordered structures with spacings from 27 to 55 Å. A series of peaks reflect the formation of a number of ordered protein arrays, apparently with DNA, with continuously varying characteristic interplanar spacings.     

Preparation and characterization of PbSe nanopowder and quasi-ceramics

By means of the reduction of Pb(II) and Se(IV) with hydrazine, oval monodispersed PbSe nanoparticles characterized by sizes ～100 nm and the cubic symmetry were obtained. Their compaction and sintering into quasi-ceramic state were performed. The samples were investigated by means of scanning electron microscopy, X-ray diffraction and FTIR spectroscopy. The results obtained are discussed.     

Broken Symmetries and Hydrodynamics of Hexatic B and Snectic F and I Liquid Crystal Phases

The nature of the spontaneously broken symmetries in hexatic B and smectic F and I phases is investigated and the hydrodynamics of the associated degrees of freedom is discussed.