过饱和度对KDP晶体生长与光学性能的影响研究

在不同过饱和度的溶液中生长了KDP晶体,对生长晶体的透过率,光散射和激光损伤阈值进行了表征.研究了不同过饱和度对KDP晶体生长及光学性能的影响.实验表明:KDP晶体可以在高过饱和度(σ＞3;)溶液中实现快速生长,生长速度可大于10 mm/d;但随着溶液过饱和度的增加,KDP晶体生长溶液的稳定性降低,晶体容易出现包藏、开裂和添晶等缺陷,晶体的光学性能也随之降低.     

Fe3+对KDP晶体生长影响的研究

金属离子对KDP晶体的影响是多方面的.本文采用不同的过饱和度,在不同的Fe3+掺杂浓度的生长溶液中生长KDP晶体,定量地研究了Fe3+对KDP晶体生长的影响.实验发现,无论是在高过饱和度还是在低过饱和度下生长KDP晶体,在一定的浓度范围内,Fe3+的掺入既可以增加生长溶液的稳定性,又可以有效抑制晶体柱面的扩展,而且晶体基本不楔化,同时,对晶体光学性能的影响也不大.     

溶液降温法快速生长KDP晶体的新装置

利用溶液降温法分别在锥形底生长装置和传统晶体生长装置中进行了KDP晶体点状籽晶法快速生长实验,对KDP晶体的生长条件进行了对比,分析了不同生长装置对KDP溶液稳定性的影响,利用扫描电镜观察了KDP晶体中的包裹体,测定了晶体的透过率,对比分析了锥形瓶快速生长装置的优越性.     

pH值对KDP晶体位错结构的影响

在一定的过饱和度下,分别用点状和片状籽晶在不同pH值溶液中生长出了KDP晶体.利用化学腐蚀法对KDP晶体的不同晶面进行了腐蚀,得到了清晰的位错蚀坑.应用光学显微镜对位错蚀坑的分布特点和密度做了观察分析,发现很多位错蚀坑成线状排布.pH值对KDP晶体位错密度有较大影响,低pH值条件下生长出的晶体位错密度较大.测试了KDP晶体样本的透过率,结果表明位错密度对KDP晶体的透过率没有明显的影响.     

点状籽晶法生长KDP晶体中散射颗粒分布

在不同的溶液pH值条件下进行了点状籽晶法慢速和快速生长KDP晶体实验,发展了观察晶体中散射颗粒分布的激光层析技术,通过图像处理得到了KDP晶体内部(100)面完整的散射颗粒分部图,对不同生长速度、不同pH值条件下点状籽晶法生长的KDP晶体的散射颗粒分部做了对比.利用表面光学投影技术观察了晶体表面宏观形貌,并由此分析了不同生长条件下生长机制对散射颗粒分布的影响.测定了散射颗粒密度不同部位的晶体透过率.     

pH值对KDP晶体溶解度和溶液稳定性的影响

测定了不同pH值(2.0～5.5)生长溶液中KDP晶体(KH2PO4)的溶解度曲线,实验结果表明:随着生长溶液pH值的改变,KDP溶解度明显增大.讨论了KDP晶体溶液pH值、溶液组成和溶液饱和点温度三者之间的关系.进行了高pH值(3.8～5.6)KDP生长溶液的稳定性实验,发现高pH值生长溶液中的临界成核半径rC增大,溶液的稳定性提高.在不同pH值溶液中进行了晶体生长实验,探讨了不同pH值生长溶液中配合物对KDP晶体生长习性的影响.     

点状籽晶法生长DKDP晶体的研究

本文研究了影响溶液稳定性的因素,主要包括溶液的纯度、饱和点和过饱和度等,并对DKDP的点状籽晶法生长进行了初步研究.同时比较了不同生长速度生长的晶体质量.结果表明:经超细过滤的高纯度溶液稳定性有很大提高,而此时生长速度对晶体质量的影响不大.最后,获得了X、Y向生长速度达3.8mm/d的点状籽晶,生长出尺寸为44mm×44mm×48mm的高质量DKDP晶体,并对晶体生长的表面进行了微观观察,分析了DKDP晶体生长的微观机制.     

快速生长KDP晶体表面的光学显微实时观察

设计了一套溶液降温法晶体生长显微实时观察装置,对快速生长KDP晶体{101}和{100}表面形貌的演化过程进行了实时观测分析.测量了晶体表面生长层切向生长速度随溶液过饱和度的变化曲线,并利用台阶生长动力学方程计算了相关动力学参数.进行了Fe3+掺杂实验,结果表明Fe3+的存在会影响到不同晶面上生长层的动力学系数,从而改变KDP晶体表面生长层的切向生长速度.     

KDP晶体中包裹体形成机制的探讨

本文介绍了包裹体对KDP晶体质量的影响,并从两个方面探讨了KDP晶体生长过程中包裹体的形成机制.通过分析KDP晶体表面原子结构研究了不同杂质的吸附情况以及杂质对生长台阶的阻碍作用,通过分析晶体生长过程中流体动力学和质量输运条件的变化研究了旋转晶体的流体切应力和表面过饱和度,结果表明吸附杂质对生长台阶的阻碍和表面过饱和度的不均匀造成了生长台阶的弯曲和宏观台阶的形成,导致生长台阶形貌的不稳定是包裹体形成的重要原因.     

KDP晶体生长过程中溶液稳定性的研究

在KDP晶体生长过程中,溶液的稳定性对KDP晶体的光学质量影响较大.溶液的稳定性是多种因素共同作用的结果.本文主要研究了过饱和KDP溶液中晶胚的分布情况、降温过程中晶体生长驱动力与降温速度之间的关系,并分析了KDP晶体实际生长过程中影响溶液稳定性的主要因素.我们认为,通过改善KDP晶体生长过程中溶液的稳定性,并与其它措施和技术相结合,是提高KDP晶体光学质量的有效途径.     

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.     

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.