用电沉积法在氧化铝模板中制备氧化锌纳米线的研究

利用直流电沉积法在阳极氧化铝模板的有序孔洞中生长了氧化锌纳米线,首次在氧气氛围中将锌氧化成氧化锌.用场发射扫描电子显微镜(FE-SEM)和X射线衍射仪(XRD)对其形貌及成分进行表征和分析.结果表明,氧化铝模板的有序孔洞中填充了高致密、均一连续的锌纳米线.在氧气氛围中,800 ℃下氧化2 h,氧化铝中的锌纳米线己全部氧化成氧化锌纳米线.光致发光光谱表明,氧化锌纳米线在496 nm处有较强蓝绿光发射.     

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.     

不同形貌氮化硅纳米结构的制备与表征

分别通过VLS和VS生长机制得到了Si3N4纳米线和纳米带.产物经X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)等表征手段进行了分析.FTIR图谱表明它们在800～1100cm-1的波数范围内有一个宽的吸收带,这是Si-N键伸缩振动模式的典型吸收带.它们的室温光致发光图谱显示,在420nm左右都有一很强的发射带,表明其将在纳米光电器件中有潜在应用.另外,Si3N4纳米线发光峰与纳米带的发光相比有少许蓝移(蓝移约4nm),这可能和晶须尺寸的少许差别有关.至于纳米带的发光强度大于纳米线的原因,可能是纳米带的比表面积相对较大,有利于悬键的形成,从而导致材料结构内缺陷的浓度较大.     

温度对Ga掺杂ZnS纳米结构的形貌及光致发光性能的影响

分别以Zn粉和S粉为原材料,Ga为掺杂剂,Au纳米颗粒为催化剂,采用低温化学气相沉积法(CVD),在Si(l00)衬底上制备了Ga掺杂的ZnS纳米结构.利用X射线衍射仪(XRD)、能量弥散X-ray谱(EDS)、场发射扫描电子显微镜(SEM)和光致发光光谱(PL)等测试手段对样品的结构、成分、形貌和发光性能进行了分析.结果表明:随着温度的升高(450～ 550℃),Ga掺杂ZnS纳米结构的形貌发生了从蠕虫状纳米线到光滑纳米线再到纳米棒的演变,所制备的Ga掺杂的ZnS纳米结构均为六方纤锌矿结构,分别在波长为336 nm和675 nm处存在一个较强的近带边紫外发射峰和一个Ga掺杂引起的微弱红光峰,而其它发光峰均是缺陷引起的.此外,本文还对Ga掺杂ZnS纳米结构的形成过程进行了探讨,并提出了可能的形成机理.     

聚乙烯醇对ZnO纳米棒结构和光学性能的影响

以六水硝酸锌为锌源,聚乙烯醇(PVA)为分散剂,制备了纳米氧化锌(ZnO).利用X射线衍射(XRD)和电子扫描电镜(SEM)对氧化锌的晶体结构、形貌和尺寸进行了表征.利用吸收光谱对氧化锌的吸收率进行了测量.结果表明,所制备的氧化锌属于六方纤锌矿单晶结构,呈棒状结构.通过改变PVA含量,氧化锌纳米棒的长度可以从400nm到2μm可调.吸收光谱表明,随着PVA含量增加,吸收光谱发生红移.讨论了PVA作用下氧化锌纳米棒的形成机理.     

钒酸铜纳米线的制备及光吸收性能

以CuCl2和NH4VO3为原料,采用水热法制备了α-CuV2O6纳米线.采用X射线衍射(XRD)研究了所得α-CuV2O6纳米线的晶相特征,采用场发射扫描电镜(FE-SEM)及透射电镜(TEM)观察产物的微观形貌,利用X-射线能谱(EDS)及X-射线光电子能谱(XPS)对样品的组成进行了分析,并采用紫外-可见漫反射(UV-vis DRS)测定了样品的光吸收性能.紫外-可见漫反射测试显示α-CuV2O6纳米线具有较宽的紫外-可见光吸收范围.     

Al催化剂辅助直流电弧法合成α-Si3N4纳米线

采用等离子体辅助直流孤光放电技术,以SiO2粉和Si粉为反应原料,制备了大量纯度高α-Si3N4纳米线.通过X射线衍射(XRD)、能量色散X射线光谱(EDS)、透射电子显微镜(TEM)、傅里叶红外光谱(FTIR)对α-Si3N4纳米线的形貌和组分进行表征与分析.TEM和SEM分析显示合成的α-Si3N4纳米线直径为30~100 nm,长达几十微米,其生长沿着α-Si3N4的[001]方向生长,生长机制气-液-固(VLS)机制所控制.α-Si3N4纳米线光致发光光谱(PL)表明其具有一宽的发光带,具有良好的发光性能.     

氧化锌纳米粒子的合成及其表面功能化修饰

以三甘醇(TEG)为溶剂,高温热分解乙酰丙酮锌合成了氧化锌纳米粒子.为改善氧化锌纳米粒子表面性能和生物应用性能,分别用硅烷偶联剂(KH550)和聚酰胺-胺(PAMAM)进行表面修饰,在氧化锌纳米粒子表面接枝了-NH2活性官能团.分别采用X射线衍射仪(XRD)、透射电镜(TEM)、红外光谱(FT-IR)、X射线光电子能谱、动态光散射(DSL)和紫外可见分光光度计(UV-Vis)对样品进行了表征测试.XRD结果表明纳米氧化锌的平均晶粒尺寸为10 nm,并具有较好的结晶性.TEM观察表明,其形貌为颗粒状和小晶粒团聚成的球状粒子.FT-IR、XPS、DSL和Zeta电位测试结果表明氨基官能团成功修饰在氧化锌纳米粒子表面,增强了粒子的表面功能.UV-Vis光谱表明,氨基活性基团修饰后的纳米氧化锌仍然具有较强紫外带隙吸收.     

建筑环境下基于ZnO纳米线甲醛气体检测传感器的研究

为了检测建筑物室内甲醛,用ZnO纳米线作为监测甲醛的目标物.以氯化锌(ZnCl2)和柠檬酸钠(C6 H5 Na3 O7)为原料,使用水热法合成ZnO纳米线,利用X射线衍射仪(XRD)、扫描电镜(SEM)和X射线能谱仪(EDS)对制备出的ZnO纳米线的晶体结构和微观形貌进行表征.结构表征结果表明,所制备出的ZnO纳米线结晶良好、纯度较高,平均直径为(39±10)nm,其长度约为400 nm,且分散良好.将所制备的ZnO纳米线涂覆在陶瓷管上,组装成气敏元件并对其进行系统的气敏特性研究.气敏检测结果表明,基于ZnO纳米线的气体传感器对HCHO气体具有优异的气敏性能.该传感器在125℃时对50×10-6的HCHO气体获得最大灵敏度15.2,同时展现出了优良的稳定性、重现性以及选择性.     

超细Si/SiOx纳米线和纳米花等离子体辅助生长及光致发光

采用等离子体辅助直流弧光放电技术,以Si粉和SiO2粉为反应原料,制备了不同形貌的超细Si/SiOx纳米线和纳米花.通过X射线衍射(XRD)、透射电子显微镜(TEM)、能量色散X射线光谱(EDS)对Si/SiOx纳米线的形貌和组分进行表征与分析.Si/SiOx纳米线紫外可见吸收光谱证实了样品的光学带隙为4.58 eV.Si/SiOx纳米线光致发光光谱(PL)表明其在305 nm、495 nm处有较强的发光峰,具有良好的发光性能.     

Triethyl ammonium salt of O,O′-bis(p-tolyl)dithiophosphate, [Et3NH]+[(4-MeC6H4O)2PS2]−

Triethyl ammonium Salt of O,O′-bis(p-tolyl)dithiophosphate and O,O′-bis(m-tolyl)dithiophosphate have been obtained by reaction of p- and m-cresol, respectively with P₂S₅ in toluene and have been characterized by elemental analysis, IR, ¹H and ³¹P NMR spectroscopy. The molecular structure of O,O′-bis(p-tolyl)dithiophosphate has been determined. Crystal data: [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻: Monoclinic, P2₁/c, a=15.2441(9) ?, b=10.415(2) ?, c=3.9726(9) ?, β=91.709(7)°, V=2217.5(1) ?⁻³, Z=4.Supplementary materials Additional material available from the Cambridge Crystallographic Data Centre (CCDC no. 600927 for [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻ comprises the final atomic coordinates for all atoms, thermal parameters, and a complete listing of bond distances and angles. Copies of this information may be obtained free of charge on application to The Director, 12 Union Road, Cambridge CB2 2EZ, UK (fax: +44-1223-336033; email: deposit@ccdc.cam.ac.uk or www:http://www.ccdc.cam.ac.uk).     

Crystal structure of Zn4Na(OH)6SO4Cl·6H2O

The structure of Zn₄Na(OH)₆SO₄Cl·6H₂O, a secondary mineral from Hettstedt, Germany, was determined by single-crystal X-ray diffraction. The crystals are hexagonal,a=8.413(8),c=13.095(24) Å, space group $P\bar 3$ , Z=2. The structure was refined to R=0.0554 and R_w=0.0903 for 970 reflections with I≥3σ(I). The structure can be described as zinc hydroxide layers perpendicular toc, from which sulfates and chlorides extend. The layers are held together by a system of hydrogen bonds involving hexaaquo Na⁺ ions which occupy the interlayer space.     

Synthesis and Crystal Structure of 5-[2-(6-bromonaphthalenyloxymethyl)]-3-(4-morpholinomethyl)-1,3,4-oxadiazole-2(3<Emphasis Type="Italic">H</Emphasis>)-thione

Abstract  The title compound, C₁₈H₁₈BrN₃O₃S, a derivative of 1,3,4-oxadiazole, crystallizes in the triclinic space group P-1 with unit cell parameters a = 6.8731(3), b = 8.9994(4), c = 15.7099(6) ?, α = 92.779(3)°, β = 130.575(3)°, γ = 107.868(4)°, Z = 2. The dihedral angle between the mean planes of the planar naphthyl and morpholine (chair) rings with the planar oxadiazol ring is 50.1(8) and 76.8(6)°, respectively. The planar naphthyl ring is twisted 52.2(5)° with the mean plane of the morpholine ring. A group of four intermolecular close contacts are observed between a bromine atom and hydrogen atoms from the closely packed naphthyl, morpholine and oxy–methyl groups in the unit cell. These molecular interactions in concert with an additional series of π–π stacking interactions that occur between the center of gravity of the two 6-membered rings of the naphthalene group influence the twist angles of each of these three groups. A MOPAC AM1 calculation of the conformation energy of the crystal structure [226.0128(9) kcal] compared to that of the minimum energy structure after geometry optimization [29.9744(1) kcal] reveals a significantly reduced value. The twist angles of the three groups above also change after the AM1 calculation giving support to the influence of both intermolecular C–H···Br short-range interactions and Cg π–π stacking interactions on these angles which therefore play a role in stabilizing crystal packing. Graphical Abstract  Crystal structure of 5-{[(6-bromonaphthalen-2-yl)oxy]methyl}-3-(morpholin-4-ylmethyl)-1,3,4-oxadiazole-2(3H)-thione, C₁₈H₁₈BrN₃O₃S, is reported and its geometric and packing parameters described and compared to a MOPAC computational calculation. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Crystal structure of irisolidone from the flowers of Pueraia lobata

Irisolidone (5,7-dihydroxy-6,4′-dimethoxyisoflavone) was isolated from the flowers of Pueraia lobata and its crystal structure was examined by X-ray single crystal diffraction. The crystal structure of irisolidone is monoclinic, space group P2₁/c with a = 15.491(9) ?, b = 7.895(4) ?, c = 13.321(7) ?, β = 110.546(9)° and Z = 4. Hydrogen bonding and aromatic π–π stacking assemble the title compound into a three-dimensional networking structure.     

Synthesis of spinacine and spinacine derivatives: crystal and molecular structures of Nπ-hydroxymethyl spinacine and Nα-methyl spinaceamine

The natural amino acid L-Spinacine (4,5,6,7-tetrahydro-1H-imidazo[4,5-c]pyridine-6-carboxylic acid) has been synthesized following a new pathway which gives a chemically and optically pure product with an excellent yield. The crystal structures of a synthetic intermediate, N^π-hydroxymethyl-spinacine, and a spinacine derivative, N^α-methyl-spinaceamine, have been investigated through X-ray diffraction: Spi(πMeOH)·H₂O, monoclinicP2 _i,a=8.571(1),b=6.682(1),c=8.588(1) Å, and β=94.67(1)^o. Spm(αMe)·2HCl·H₂O, triclinicP l,a=7.492(4),b=10.799(3),c=7.040(2) Å, α=91.88(2), β=98.36(3) and γ=73.34(3)^o. Spi(πMeOH) crystallizes with a water molecule and displays a zwitterionic character. The carboxylate group is in equatorial position and forms a short electrostatic interaction of 2.618(2) Å between one of its oxygens and the protonated nitrogen of the tetrahydropyridine ring. The crystal packing is assured by strong O?H???O, O?H???N, N?H???N intermolecular hydrogen bonds and C?H???O close contacts. The biprotonated compounds Spm(αMe) crystallizes with two Cl^? anions and a water molecule. The positive charge on the imidazole ring is delocalized on the conjugated moiety N=C?N. The crystal is built up by clusters formed by two biprotonated Spm(αMe) molecules, four Cl^? anions and two water molecules linked together by hydrogen bonds.     

X-ray Crystal Structures of [Et3NH][{(CO)5Mo(P(OCH2CMe2CH2O)O)}2H] and (CO)5Mo{μ-Ph2POPPh2}Mo(CO)5, Two Complexes Derived from the Hydrolysis of Coordinated Chloro-Phosphorous-Donor Ligands

Abstract X-ray crystal structures of [Et₃NH][{(CO)₅Mo(P(OCH₂CMe₂CH₂O)O)}₂H], 3, and (CO)₅Mo{μ-Ph₂POPPh₂}Mo(CO)₅, 2, are reported. Crystallization of 3 occurs in P-1 space group with a = 9.6944(19) ?, b = 10.814(2) ?, c = 19.730(4) ?, α = 94.24(3)°, β = 92.23(3)°, γ = 113.47(3)°, Z = 4. Crystallization of 2 occurs in C2/c space group with a = 10.357(2) ?, b = 20.149(4) ?, c = 17.155(3) ?, α = 90°, β = 97.28(3)°, γ = 90°, Z = 8. Compound 2 is a bimetallic complex with a P–O–P bridging group containing bond distances similar to that of other complexes in which two metal centers are bridged by a single R₂POPR₂ ligand. Compound 3 contains intermolecular hydrogen bonded P–O–H–O–P linkages with bond distances comparable to those seen in similar structures with intramolecular hydrogen bonding suggesting that the distance is a function of the nature of the bond and not affected by the cis arrangement of the ligands about the metal center. Graphical abstract X-ray Crystal Structures of [Et ₃ NH][{(CO) ₅ Mo(P(OCH ₂ CMe ₂ CH ₂ O) O)} ₂ H] and (CO) ₅ Mo{μ-Ph ₂ POPPh ₂ }Mo(CO) ₅ , Two Complexes Derived from the Hydrolysis of Coordinated Chloro-Phosphorous-Donor Ligands Samuel B. Owens Jr., Abha A. Kaisare and Gary M. Gray X-ray crystal structures of [Et₃NH][{(CO)₅Mo(P(OCH₂CMe₂CH₂O)O)}₂H], 3, and (CO)₅Mo{μ-Ph₂POPPh₂}Mo(CO)₅, 2, have been determined.      

Preparation,spectral studies and X-ray crystal structure of 1,3,5-triphenyl-1,5-pentanedione,C23H20O2

1,3,5-triphenyl-1,5-pentanedione, C₂₃H₂₀O₂, has been prepared and characterized by spectroscopic methods and single crystal X-ray analysis. Crystals are monoclinic, space groupP2₁/n, a=28.124(4),b=5.997(1),c=10.434(1)Å, -98.42(1)Å,Z=4. The structure has been refined to a finalR-value of 0.040 for 1625 reflections withF _o>3(F _o). The compound contains the two carbonyl groups in a mutuallycis arrangement.     

Isotope Effects in Liquid Crystal Systems: I: Phase Relationships in the Dodecylamine-H2O,Dodecylamine-D2O Systems

The phase diagrams and heats of fusion and transition have been determined for the dodecyl amine (-NH₂)/H₂O and dodecyl amine (-ND₂)/D₂O systems using direct optical observation and differential scanning calorimetry.     

Spherulitic crystallization of β‐In2Te3 by physical vapour deposition

Different morphologies of indium telluride (In₂Te₃) including novel spherulites were crystallized using the physical vapour deposition (PVD) method, by varying the difference in the growth and source zone temperature (ΔT) of a dual zone horizontal furnace assembled indigenously. Whiskers and kinked needles of In₂Te₃were grown at ΔT = 250 K and 300 K respectively, maintaining the growth zone at 500 °C. At high supersaturation (Δ T = 400 K), spherulitic crystals were obtained. The stoichiometric composition of these crystals has been confirmed using energy dispersive analysis by x‐rays (EDAX). The structure of β‐In₂Te₃ spherulitic crystals is identified as zinc blende with lattice parameter a = 6.159 Å, from x‐ray diffraction (XRD) studies. The scanning electron microscope (SEM) images revealed the radial structure of the grown spherulites. The growth mechanism for the spherulitic crystallization of β‐In₂Te₃ crystals has been discussed based on the theoretical models. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)