声化学法制备ZnS: Mn纳米晶及其光学性能

以无水氯化锌,四水氯化锰以及硫代乙酰胺为原料,采用声化学法成功制备了锰掺杂的ZnS(ZnS: Mn)纳米晶.采用透射电子显微镜镜(TEM)、X射线能谱仪(EDS)、X射线粉末衍射(XRD)和光致发光谱(PL)对所制得的纳米进行了表征.结果表明:所制备ZnS: Mn为立方闪锌矿结构,纳米粒子的形貌接近于球形.平均晶粒尺寸为10 nm左右.PL光谱分析表明:所制备试样有两个主要的发射峰,分别位于在480 nm和570 nm左右,后者与体材料ZnS: Mn相比发生了明显蓝移,但仍表现为橙黄色发光.Mn2+掺杂浓度对ZnS: Mn的光致发光性能有显著影响,原料中Zn: Mn: S(物质的量比)为3: 1: 4,Mn2+掺杂浓度为2.64 at;时,光致发光光谱发射峰强度达到最大值.     

ITO玻璃衬底上生长的Zn0.9Mg0.1S多晶薄膜特性研究

以ZnS和Mg粉末为原料,采用真空蒸镀技术在ITO玻璃上成功地制备了宽禁带三元化合物Zn0.9Mg0.1S多晶薄膜.原子力显微镜和X射线衍射研究表明:薄膜生长形貌和结晶性能良好,为择优取向的立方闪锌矿结构,晶粒直径约20nm,薄膜的X射线衍射峰较之ZnS的衍射峰向大角度方向移动了0.46°;室温下的拉曼谱峰相对于ZnS的拉曼谱峰出现蓝移,且347.67cm-1谱峰比较强;光致发光谱显示,Zn0.9Mg0.1S薄膜在410nm处有一个较强的发光峰.良好的结晶质量和发光特性为开发多功能材料和器件提供了可能性.     

ZnS:Mn/CdS核壳结构纳米微粒的制备及光学特性

采用微乳液法制备了掺Mn的ZnS纳米微粒并用CdS对其进行了表面修饰,以XRD、紫外吸收和发射光谱对其结构及光学性质进行了表征和研究.制得的纳米微晶粒径为4～6nm,为立方纤锌矿结构.与未经包覆的ZnS:Mn纳米微粒相比,核壳结构的ZnS:Mn/CdS纳米微粒中Mn2+发射峰的强度增强了很多,适当厚度的壳层的修饰可减少其表面态发射和非辐射跃迁,增强了Mn2+离子的4T1-6A1的能量传递和ZnS的带边发射,提高了发光效率;讨论了ZnS核中Mn掺杂浓度对ZnS:Mn/CdS纳米微晶的光学性能的影响,发现当掺Mn浓度为4;时Mn2+发射峰的强度最大.     

在脉冲纳米锌晶种上水热合成ZnS薄膜及其光学性能研究

用水热法在脉冲电沉积纳米Zn晶种的衬底上,制备了ZnS薄膜.利用XRD、SEM、EDS对ZnS薄膜结构进行了表征,通过UV、PL研究了ZnS薄膜的光学性质.结果表明,Zn晶种的存在、形貌控制剂(5-磺基水杨酸)的添加对ZnS薄膜显微形貌有重大影响.所制备出的ZnS薄膜为沿(106)晶面生长的六方纤锌矿结构,薄膜组成均匀而致密,光学禁带宽度变宽,发蓝紫光.     

预制层中Zn和ZnS对CZTS薄膜太阳电池的影响

采用磁控溅射后硫化的方法制备Cu2 ZnSnS4 (CZTS)薄膜,分别用Zn和ZnS作为锌源,在镀钼的钠钙玻璃衬底上以Zn(或ZnS)/Sn/Cu的顺序制备出不同的CZTS薄膜预制层.首先对预制层进行低温合金,然后以硫粉作为硫源进行高温硫化,得到CZTS薄膜.通过X射线衍射仪(XRD)、扫描电镜(SEM)及能谱仪(EDS)分别对所制备薄膜的晶体结构、表面形貌和薄膜组分进行分析表征;并用拉曼光谱表征了CZTS相的纯度.最后用CZTS薄膜制备了太阳电池,发现在预制层中以ZnS作为锌源得到的太阳电池有较高的性能参数,其开路电压:V =651 mV,短路电流密度:Jsc=11.4 mA/cm2,光电转换效率达到2.8;.     

表面活性剂对水热法合成ZnS:Cu,Al纳米晶光致发光特性的影响

采用水热法直接合成了ZnS∶Cu,Al纳米荧光粉,并且系统研究了加入表面活性剂在不同S/Zn下,清洗样品和不清洗样品的结晶性、傅立叶红外光谱(FT-IR)及光致发光(PL)光谱.XRD和TEM测试结果表明:合成纳米晶为纯立方相结构,球形纳米晶尺寸约15 nm, 尺寸分布窄,分散性好.未清洗样品的结晶性比清洗样品的好,且加入表面活性剂和未清洗都导致粒径增大,影响纳米材料的表面态.改变[S~(2-)]/[Zn~(2+)]物质的量比、清洗和加入表面活性剂都会影响材料的PL强度.这说明其发光机理为紫外光激发材料表面的发光中心,即PL强度决定于纳米材料的表面态.     

Ag/ZnS核壳结构纳米棒的制备及其光催化性能分析

在制备的Ag纳米线的基础上,用水热法合成了Ag/ZnS核壳结构纳米棒.使用X射线衍射仪(XRD)、场发射扫描电子显微镜(FESEM)、X射线能谱仪(EDS)、高分辨透射电子显微镜(HRTEM)、紫外-可见双光束分光光度计(UV-vis)、光致发光扫描仪(PL)等检测设备对样品的成分、形貌、微结构及光学性能进行了表征.结果显示,制备的Ag/ZnS复合材料为ZnS纳米颗粒包覆Ag纳米线的核壳结构,其紫外吸收峰位于350 nm处,相对于ZnS纳米颗粒变宽并发生红移,PL发射峰位于462 nm处,相对于ZnS纳米颗粒发生了蓝移,强度明显降低.光催化结果显示,Ag/ZnS核壳结构纳米棒的光催化性能优于ZnS纳米颗粒,分析了光催化反应机理.     

L-半胱氨酸修饰的ZnS∶Co/ZnS量子点的合成及表征

选用L-半胱氨酸作为修饰剂,采用共沉淀法在水溶液中合成了ZnS∶ Co/ZnS量子点.通过X-射线粉末衍射(XRD)、透射电镜(TEM)、红外光谱(IR)、紫外可见光谱(UV-Vis)和荧光光谱(PL)对量子点的结构、形貌、组成及光谱性质进行表征.结果表明:ZnS∶ Co/ZnS量子点为立方闪锌矿结构,颗粒呈球形,分散性好,颗粒尺寸约为3.3nm1;随着ZnS壳层增厚,ZnS∶ Co/ZnS量子点的荧光发射峰强度先增大后减小,核壳比为1∶0.15时发光强度达到最大.Co2+的掺杂和ZnS壳层的形成使量子点的荧光量子产率从2.4;增加到9.8;.L-半胱氨酸分子通过其巯基与量子点表面的金属离子配位,从而修饰在量子点的表面,使该量子点具有水溶性、生物相容性和生物可偶联性.     

功能化ZnS:Mn/ZnS纳米微粒的制备及光学性质的研究

本文采用反相微乳液法制备了核壳结构的ZnS:Mn/ZnS纳米微粒.为了获得具有一定水溶性及生物相容性的纳米颗粒,巯基乙酸被直接加入到反相微乳液体系中对ZnS:Mn/ZnS纳米颗粒进行表面改性.连接上巯基乙酸的ZnS:Mn/ZnS纳米微粒在600nm处的光致发光明显增强.实验结果显示导致荧光增强的机理可能是有机分子及多核锌配合物的钝化作用.     

金属前驱体摩尔比对CZTS纳米晶微结构的影响

采用热注入法制备Cu2 ZnSnS4(CZTS)纳米晶,研究了金属前驱体摩尔比对所制备的CZTS纳米晶的晶体结构、化学组分、形貌及光学性能的影响.实验结果表明:当Cu:(Zn+Sn)前驱体摩尔比在0.8:1～1:1范围变化时,所得到的产物为纯锌黄锡矿结构CZTS纳米晶.当Cu:(Zn+Sn)≤0.7:1时,产物的XRD图谱在(112)晶面衍射峰附近出现微弱的SnS杂峰.当Cu:(Zn+Sn)前驱体摩尔比从0.9:1变化为0.8:1时,纳米晶的形貌主要为球形,少量为多边形;当Cu:(Zn+Sn)前驱体摩尔比从0.7:1减小到0.6:1时,纳米晶的形貌主要有纺锤形及少量球形.所制备样品的光学带隙随着Cu:(Zn+Sn)前驱体摩尔比的减小而增大,其带隙宽度在1.44～1.56 eV之间变化.     

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.     

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.     

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.     

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.     

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.     

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.