化学计量比LiNbO3晶体的畴结构及完整性研究

本文对用助熔剂提拉法生长的两种化学计量比LiNbO3晶体进行了测试分析,并与同成分LiNbO3晶体相比较.通过差热分析和X射线粉末衍射测试,得出随着晶体中Li2O含量的增加,其居里温度变高,晶格常数变小.用酸腐蚀晶体,通过直接观察和金相照片,分析其畴结构,得出SLN11是单畴生长,首次观察出SLN19晶体在Z切面上出现了三块面积较大的对称反畴区,将其称为区域性单畴.另外,还对晶体在(001)方向抛光面的不同位置测量了其回摆曲线,得到了其中SLN19晶体有着较完整的结晶面.期望通过改变生长参数,长出完全单畴且更加接近化学计量比的LiNbO3晶体.     

富锂熔体中提拉法生长近化学计量比铌酸锂(LiNbO3)晶体

利用提拉法,在富锂(Li2O∶NbO3=58.5/41.5)熔体中生长了质量良好的近化学计量比铌酸锂单晶,其紫外吸收边位置为308nm,居里温度超过了1200℃.测量了其Z向晶片的压电系数d33,并且观察了Z向晶片的180°畴,结果证明除少数区域外,所生长晶体为单畴.     

适用于宽温度范围高稳定的Q开关LiNbO3晶体

分析了俄罗斯的Q开关LiNbO3晶体的成分,这种开关用在Nd∶YAG激光测距仪上,能够在温度-50～50℃范围内稳定工作.通过测量紫外吸收边的位置、红外振动光谱、晶格常数和居里温度的方法,测出晶体中的锂铌比([Li]/[Nb])为49.02/50.98.分析认为晶体中的锂铌比是影响LiNbO3晶体Q开关温度稳定性的主要因素.     

高温下锂离子在低掺镁铌酸锂晶体中的扩散

研究了高温富锂气氛下锂离子在低掺镁铌酸锂晶体中的扩散.采用气相输运平衡法制备了掺杂1mol; MgO的不同锂含量的铌酸锂(Mg1LN)晶体,采用热分析仪测试了晶体的居里温度.制备了一系列不同锂含量的Mg1LN多晶料,拟合了晶体锂含量与居里温度的关系.采用Boltzmann-Matano法求解了扩散方程.结果表明,扩散温度为1100 ℃时,Mg1LN晶体中锂离子扩散系数为3.2×10-9~13.0×10-9 cm2/s,当扩散温度为1145 ℃时锂离子扩散系数约是1100 ℃时扩散系数的三倍.因此,适当提高扩散温度是提高气相输运平衡法制备近化学计量比低掺镁铌酸锂晶体效率的有效办法.     

(Nd3+,Yb3+):Ca3(VO4)2晶体的极化研究

本文回顾了(Nd3+,Yb3+):Ca3(VO4)2晶体的研究历程,通过对晶体结构和对晶体激光性能研究年代的对比,认为高的泵浦阈值是由于晶体中存在的对泵浦光和激光散射很强的畴壁结构未被发现而造成的.讨论了极化的原理、建立了极化装置,采用Laue定向法和X射线定向仪定向法结合解决了(Nd3+,Yb3+):Ca3(VO4)2这种大晶格常数(c＝3.8029nm)晶体的定向问题.把晶体的抛光面放入0.5mol;的温度为30℃的硼酸中腐蚀样品1h,用显微镜可以观察到畴结构.在～1100℃和电流密度为～10μA/mm2的条件下极化2h即可完成极化.变黑的极化样品可以通过把晶体放入马福炉中升温至850℃,保持1h,然后降至室温即可消除.     

[Li]/[Nb]比对Ce:LiNbO3晶体结构及光折变性能的影响

在铌酸锂(LiNbO3,LN)中掺入摩尔分数为0.1;的CeO2,以提拉法从不同[Li]/[Nb]摩尔比([Li]/[Nb]=0.750,0.850,0.946,1.100)的熔体中生长出了Ce:LN晶体.测试了晶体的晶格常数、红外光谱和居里温度.结果表明:随着[Li]/[Nb]比的增加,晶体仍为三方的LN晶体,且晶格常数和晶胞体积没有发生大的变化,v(OH-)振动峰的位置依次向长波方向移动,居里温度依次增加,结构缺陷减少.由于Ce和[Li]/[Nb]比的协同作用,[Li]/[Nb]比为1.100的Ce:LN晶体已接近化学计量比,[Li]/[Nb]比为0.850的Ce:LN晶体的居里温度近似等于纯LN晶体.利用二波耦合光路测试了晶体的衍射效率、写入时间和擦除时间,计算了晶体的光折变灵敏度及动态范围.测试了晶体的抗光致散射能力,结果表明:[Li]/[Nb]比越高的Ce:LN晶体的光折变性能越好.并分析了不同[Li]/[Nb]比Ce:LN晶体光折变性能增强的机理.     

高温下锂离子在低掺镁铌酸锂晶体中的扩散（英文）

研究了高温富锂气氛下锂离子在低掺镁铌酸锂晶体中的扩散。采用气相输运平衡法制备了掺杂1mol%MgO的不同锂含量的铌酸锂(Mg1LN)晶体,采用热分析仪测试了晶体的居里温度。制备了一系列不同锂含量的Mg1LN多晶料,拟合了晶体锂含量与居里温度的关系。采用Boltzmann-Matano法求解了扩散方程。结果表明,扩散温度为1100℃时,Mg1LN晶体中锂离子扩散系数为3.2×10~(-9)~13.0×10~(-9)cm~2/s,当扩散温度为1145℃时锂离子扩散系数约是1100℃时扩散系数的三倍。因此,适当提高扩散温度是提高气相输运平衡法制备近化学计量比低掺镁铌酸锂晶体效率的有效办法.     

Pb(Sc1/2Nb1/2)O3-Pb(Mg1/3Nb2/3)O3-PbTiO3-PbZrO3弛豫铁电晶体的生长及表征

采用高温溶液法生长了准同型相界(MPB)四元弛豫铁电单晶Pb(Sc1/2Nb1/2) O3-Pb(Mg1/3 Nb2/3)O3-PbTiO3-PbZrO3,得到较大尺寸且具有规则外形的立方单晶.研究结果表明所生长的晶体为钙钛矿结构,立方晶粒平整的暴露面均为(001)面;晶体以层状方式生长,生长机制为搭桥生长;所生长晶体的矫顽场Ec～3.52kV/cm,三方四方相变温度Tr-t～104℃,居里温度Tc～149.5℃,压电常数d33～1089 pC/N,剩余极化强度Pr～25.4 μC/cm2;随着频率增加,晶体的相变弥散度减小.     

近化学计量比LiNbO3晶体各向畴形态的研究

本文对采用双坩埚提拉法生长的近化学计量比LiNbO3晶体沿其各向切块腐蚀后通过直接观察和在金相显微镜下观察,对其各个面的畴结构进行了分析.我们发现晶体a面上由于镜相对称不反映畴结构,b面和c面上的腐蚀形貌则完全显露而且按一定的方向整齐地排列,证明我们生长的SLN晶体是完全单畴结构的晶体.     

CaTiO3掺杂PbNb2O6高居里温度压电陶瓷的研究

采用传统电子陶瓷的制备方法,系统研究了(1-x)PbNb2O6-xCaTiO3(x=0、0.01、0.02、0.03、0.04)系高居里温度压电陶瓷.XRD分析表明,x=0时,材料只能形成三方非铁电相钨青铜结构,而x在0.01～0.04 mol范围内均能形成钨青铜型固溶体,利用XRD数据计算了晶体的晶格常数随x的变化,发现随着CaTiO3含量增加,晶胞体积减小.陶瓷材料的居里温度测试结果表明该体系具有高的居里温度(Tc＞400℃).测试了不同组成陶瓷的压电、介电性能,CaTiO3的掺杂量为x=0.03时陶瓷样品的压电常数达到d33=64pC/N,平面机电耦合系数kp=0.269,材料的介电常数ε33T/ε0=293,介质损耗tanδ=0.021,居里温度Tc=570℃,该组成具有优异的压电性能,适合于高温环境下的使用.     

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).     

First-principles coexistence simulations of supercooled liquid silicon

We perform first-principles coexistence simulations of the low-density and the high-density phases of supercooled liquid silicon and find a negative slope for the coexisting line in the temperature-pressure plane. Electron density maps and electron-localization function plots of the two phases of silicon show marked differences. The calculated differences suggest more localized electrons in the low-density liquid compared to the high-density liquid, coming from an increased population of covalent bonds, which further explain the calculated negative slope in the two phase coexistence regime. This is consistent with the presence of a pseudo-gap in low-density liquid silicon, absent in the high-density liquid which shows a metallic behavior.     

Crystal structures of thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane

Structures of both thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane, ?C₆H₄?CH₂SCH₂?C₆H₁₀?CH₂SCH₂?, have been determined, wherecis andtrans refer to the attachments to the cyclohexane ring. Thecis form crystallizes in the monoclinic space groupP2₁/c witha=8.4299(11)Å,b=21.772(2)Å,c=8.9724(13)Å, β=116.574(11)^o, andZ=4. Thetrans isomer packs into the monoclinic space groupP2₁ witha=8.159(16)Å,b=10.185(5)Å,c=9.558(2)Å, β=112.435(18)^o, andZ=2. The cyclohexane ring of thecis isomer is in the chair conformation, while the cyclohexane of thetrans isomer is found in a twisted boat conformation.     

CTAB与SDBS对碳酸锶粒子生长形态调控及机理研究

以表面活性剂CTAB和SDBS为化学添加剂,采用化学共沉淀法对碳酸锶晶体的生长形态进行调控,成功地制备出了实心的树枝状和花瓣为空心的花状碳酸锶粉体,并用X射线衍射(XRD)、扫描电子显微镜(SEM)和傅里叶变换红外光谱(FT-IR)等分析手段对样品进行了表征;最后重点对化学添加剂可能产生的影响机理进行了初步的探讨.结果表明,CTAB和SDBS在晶体生长的过程中能起到显著的影响作用,两者对粒子分散性能的作用效果相反,而且后者对晶体(013)和(213)晶面表面能降低的贡献明显大于前者.     

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.     

Crystal structures of the cis and trans isomers of a tetrathia[3.3.3.3]cyclophane

Both the cis and trans isomers of 3,11,18,26-tetrathiatricyclo[26.2.2.1^5,9.2^13,16.1^20,24] hexatriaconta-5,7,9,20,22,24-hexene have been prepared and structurally characterized. Each of these centrosymmetric tetrathia dimers includes two cyclohexane rings in chair conformations with either 1,4-cis or 1,4-trans bonding and two meta-substituted benzene rings. The cis isomer packs into the monoclinic space group P2₁/a with a = 10.485(3)Å, b = 10.3956(18)Å, c = 14.1343(10)Å, = 105.200(13)°, Z = 2 and refined to an R factor of 0.046. The trans isomer crystallizes in the monoclinic space group P2₁/c with a = 10.7217(12)Å, b = 5.6797(7)Å, c = 25.415(5)Å, = 96.001(12)°, Z = 2 and refined to an R factor of 0.043. In the cis structure each benzene ring faces a cyclohexane ring while in the trans structure the cyclohexane rings face one another.     

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.     

电沉积法制备ZnO纳米棒阵列及其发光特性

本文以掺F的SnO2导电玻璃为基板,以硝酸锌水溶液为电解液,采用三电极恒电位体系电沉积制备ZnO纳米棒阵列,系统考察了硝酸锌浓度和沉积电位等工艺参数对ZnO纳米棒阵列的微观形貌及其发光性能的影响规律.结果表明,硝酸锌浓度和沉积电位对纳米棒阵列的形貌有显著影响,控制适宜的工艺条件可以制备出直径分布均匀、结晶性好且纯度高的六方纤锌矿ZnO纳米棒阵列.荧光光谱分析表明,电沉积制备出的ZnO纳米棒阵列在385 nm附近有一个强荧光发射峰,且发光性能稳定、对纳米棒阵列微观形貌的细微变化不敏感,使其在发光二极管和激光器等领域具有广阔的应用前景.