等径控制系统的改进及在光学级铌酸锂生长中的应用

分析了提拉法晶体生长过程中影响滞后变化的因素,采用传统PID调节器和计算机辅助控制相结合的办法,解决了铌酸锂晶体生长过程中的精确等径控制问题,并在大直径铌酸锂晶体生长应用中取得了满意的效果.生长的76mm直径的铌酸锂晶体,生长条纹问题得到很大改善,光学均匀性提高了一个量级以上.     

8英寸铌酸锂晶体生长研究

铌酸锂单晶薄膜(LNOI)在新一代信息技术中关键通信器件领域的作用日益显著,随着铌酸锂单晶薄膜制备技术和光子集成技术的发展,降低芯片成本、增加芯片集成度是光子集成芯片永恒不变的发展方向,因此迫切需求大尺寸铌酸锂晶体。本文讨论了大尺寸坩埚中熔体自然对流随着液面下降的变化规律,研究了8英寸(1英寸=2.54 cm)铌酸锂Z轴、X轴两个提拉方向的生长特点,获得等径尺寸大于φ210 mm×50 mm的8英寸Z轴、X轴铌酸锂晶体。1 mm厚X轴铌酸锂晶圆的透过率显示波长380～3 300 nm光谱的透过率超过了70%,晶片纹影图像显示晶体中存在折射率脉理缺陷。     

近化学计量比铌酸锂晶体的研究进展

本文总结了近化学计量比铌酸锂晶体的不同生长方法及它们各自的特色,分析了锂铌摩尔比对晶体性能的影响及Li含量的各种表征方法.通过比较看出,采用K2O助熔剂生长近化学计量比铌酸锂晶体是一种较为实用的途径.基于此,我们采用K2O助熔剂提拉法和助熔剂-坩埚下降法生长了近化学计量比铌酸锂晶体,所得晶体的最大尺寸分别达到45mm×60mm和25mm×40mm.     

大尺寸近化学计量比铌酸锂晶体的制备

研究了扩散法制备近化学计量比铌酸锂晶体的工艺,从原料配比、合成方式、晶片放置方式和扩散工艺等方面进行了工艺优化.对不同厚度和切割方向的铌酸锂晶体进行扩散处理,对三英寸Z-cut铌酸锂晶体进行了批量扩散试验,并对扩散后的晶体进行了组分和均匀性测试.结果表明,厚度为3.1 mm的Z-cut晶体组分达到近化学计量比,光学质量达到实用化要求,而XYZ=5.1 mm×5.1 mm×21.0 mm的晶体光学质量较差,同时厚度达1.8mm的Z-cut三英寸近化学计量比铌酸锂晶片可实现批量制备.     

掺镝近化学计量比铌酸锂晶体的光谱性质

利用提拉法,在锂铌比为58.5/41.5的富锂熔体中生长了质量良好的掺镝近化学计量比铌酸锂(Oy:NSLN)单晶,生长晶体的尺寸为φ25mm×35 mm.测量了晶体的室温吸收谱,并根据Judd-Ofeh理论,拟合出Oy3 离子的晶体场唯象强度参数:Ω2=4.8130×10-20,Ω4 =2.6140 × 10-20, Ω6=2.2448×10-20.计算了各能级的跃迁辐射几率A1,1,振子强度P1,1, 辐射寿命r,荧光分支比β1等,并根据这些光学参量讨论了该晶体的部分性能和应用前景.     

高温度稳定性系列铌酸锂电光调Q开关的研制

通过对影响铌酸锂电光调Q开关工作温度稳定性的原因分析,认为晶体自身的应力是导致铌酸锂电光调Q开关温度稳定性差的主要原因.而减小晶体自身应力的关键主要取决于晶体光学质量的均匀性,同时,组分的波动也会使晶体产生应力.为此利用前期大尺寸铌酸锂晶体质量大幅提高的结果,配合适当的热处理工艺,研制出了系列铌酸锂调Q开关,通过在1064 nm、1318 nm、2128 nm等激光器中应用,这些调Q开关均能稳定工作,完全能够满足激光雷达等脉冲激光器的使用.     

晶体材料中的常青树——铌酸锂晶体

正从上世纪70年代开始,我国科研人员就开始了铌酸锂晶体生长、缺陷、性能及其应用研究。南开大学是国内最早开展研究的单位之一,几十年来,围绕通讯、激光、国防等领域对高光学均匀性、高抗光损伤、高温度适用性光学级铌酸锂晶体的需求,将铌酸锂晶体的光学均匀性提高了近2个数量级,发明了掺镁铌酸锂晶体,将抗光损伤能力提高6个数量级以上,并实现了高光学质量近化学计量比铌酸锂晶体的实用化制备。     

名义纯及掺杂铌酸锂晶体内偏置场的实验研究

铌酸锂晶体的内偏置场对铁电应用、电光应用和非线性光学应用等均有直接影响。本工作建立了铌酸锂(LN)晶体内偏置场测试方法,对同成分铌酸锂(CLN)晶体、近化学计量比铌酸锂(nSLN)晶体、掺杂铌酸锂(doped LN)晶体的内偏置场和矫顽场进行测量。结果表明,CLN晶体内偏置场最高(E_int=2.53 kV/mm),nSLN晶体的内偏置场大幅降低,其中富锂熔体法生长和气相输运平衡(vapor transport equilibration, VTE)法结合得到的nSLN晶体的内偏置场最小,与CLN晶体相比降低了约两个数量级;掺杂铌酸锂晶体的内偏置场与CLN晶体相比也普遍降低,其中掺6.5%(摩尔分数)Mg的CLN晶体的内偏置场约为CLN晶体的四分之一,掺7%(摩尔分数)Zn的CLN晶体的内偏置场约为CLN晶体的六分之一。最后对组分和掺杂影响内偏置场的因素进行了简要分析。     

大直径、高掺镁铌酸锂晶体的生长及其紫外光折变性能研究

我们生长了掺镁量分别为3.0mol;、5.0mol;、7.8mol;、9.0mol;的76mm高掺镁铌酸锂晶体,检测了这些晶体的生长条纹情况,并利用双光耦合配置测试了这些晶体在351nm紫外光下的光折变性能.从实验结果看,采用同成分共熔点铌锂配比的高掺镁铌酸锂晶体生长条纹比较多;虽然高掺镁铌酸锂晶体在可见光波段有很好的抗光折变能力,但是在紫外光下具有良好的光折变性能,可以作为优良的紫外光折变材料使用.同时,实验结果表明,掺镁量在5.0mol;的铌酸锂晶体具有最佳的紫外光折变性能.     

近化学计量比LiNbO3晶体畴结构研究

利用提拉法,从富锂(Li2O:Nb2O5=58.5:41.5)熔体中生长了φ40mm×40mm的近化学计量比铌酸锂晶体.用同步辐射异常散射技术结合化学腐蚀法观察了晶体中的畴结构,在y方向发现存在180°反向铁电畴结构,而另外的N-SLN单晶z向切片为单畴结构,表明了所生长的近化学计量比铌酸锂晶体具有区域性单畴.     

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).     

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.     

Hydrothermal Synthesis and Morphology of Thomsonite and Edingtonite

The hydrothermal treatment of different glasses of the composition 2 Na₂O–8 CaO–10 Al₂O₃– 20 SiO₂ and 2 BaO–2 Al₂O₃–6 SiO₂ at one kilobar pressure in a temperature-range between 80 °C and 230 °C lead to the formation of the zeolite-minerals thomsonite (orthorhombic symmetry space-group Pbmn, a = 13.05 Å, b = 13.09 Å and c = 13.22 Å), and edingtonite (orthorhombic symmetry, space-group: P2,2,2, a = 9.55 Å, b = 9.67 Å and c = 6.52 Å). Under the chosen hydrothermal conditions both mineral phases are formed in the whole temperature interval.     

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.     

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.     

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.     

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.     

Simulation and Experiment in X-ray Topography and Diffractometry

X-ray double crystal topography and high resolution diffractometry reveal very small deformations of the crystal lattice. However, this information can be directly obtained from the topographs or diffractometer curves only if certain conditions are fulfilled. Generally a deformation model has to be used, that is compared to the measurements by simulation calculations based on the dynamical diffraction theory. Trial and error allow to adapt the parameters of the model. An example illustrates that with a few parameters an automatic fit is possible.