硼酸钾锶晶体的高温溶液法生长研究

以摩尔比为3∶1的NaF和H3 BO3为复合助熔剂,采用高温溶液法生长出了尺寸达7×4 ×3 mm3的较透明的KSr4B3O9单晶,并探讨了生长KSr4B3O9晶体助熔剂体系的选择.该晶体属正交晶系,空间群为Ama2,晶胞参数为:a=109.87(2) nm,b =119.48(2) nm,c =68.865(2) nm.该晶体结构是由KO10基团,SrOx(x=8,9)基团和独立的BO3三角形相互连接构成的三维网络结构;UV-Vis-NIR漫反射光谱说明KSr4B3O9化合物在紫外区230 nm左右才表现为全吸收;粉末倍频测试结果表明该化合物总的倍频效应与KH2PO4 (KDP)相当.     

稀土正硅酸盐-Y2SiO5单晶体的提拉法生长

用提拉法晶体生长工艺已成功地生长出正硅酸盐-Y2 SiO5单晶体.使用设备是一台中频感应加热炉.文中讨论了高光学质量掺Eu离子Y2 SiO5单晶体的生长工艺,已生长的晶体毛坯直径达35mm,长130mm、质量为460g、光学质量良好.     

有机分光晶体季戊四醇的生长研究

本文采用多次重结晶的方法提纯季戊四醇(PET)原料,用高效液相色谱进行分析研究.通过目测法和吊籽晶法,测定了PET生长的亚稳区宽度.研究了溶液的pH值、过热时间和过热温度等因素对溶液亚稳区和诱导期的影响.采用紫外-可见光谱、红外光谱研究了长时间高温下溶液被氧化的特性.用溶液降温法在2L的生长槽中生长出30 nm×30 mm× 30 mm的PET单晶体.     

Ba3(VO4)2晶体的生长和拉曼性质的研究

采用提拉法生长了尺寸为φ22mm×50 mm的Ba3(VO4):晶体.室温下测试了Ba3(VO4)2晶体不同激发配置下自发拉曼散射光谱.另外测试了该晶体在532 nm、25 ps脉冲下的受激拉曼散射,观察到3阶斯托克斯线(625.5 am)和1阶反斯托克斯线(506.8 nm),并估算了Ba3(VO4)2晶体的稳态拉曼增益系数.     

[(CH3)2NH]3[H3PMo12O40]的合成、结构及表征

通过水热合成法,成功合成了化合物[(CH3)2NH]3[H3PMo12O40],并通过单晶X射线衍射,IR,XRD,元素分析和电化学分析对该化合物进行表征.该化合物中,Keggin型磷钼酸之间通过氢键形成二维折叠层,这些层按照ABCD沿c轴方向堆积.二甲胺分子分布在层间,通过氢键连接相邻的来自不同层的两个Keggin型磷钼酸,将二维折叠层进一步拓展成三维超分子骨架.     

4-(2,5-二甲基-3,4-二乙酰基)-1-吡咯基苯甲酸的合成及其晶体结构

在强酸性介质中,3,4-二乙酰基-2,5-己二酮与对氨基苯甲酸作用,满意地得到了4-(2,5-二甲基-3,4-二乙酰基)-1-吡咯基苯甲酸,用IR、1H NMR、高分辩质谱等对其进行了表征,用X射线衍射测定了晶体结构.该晶体属三斜晶系,P1空间群,a＝0.80950(10)nm,b＝0.81910(10)nm,c＝1.1900(2)nm,α＝101.600(10)°,β＝98.820(10)°,γ＝104.960(10)°,Z＝2,Dc＝1.364×103kg/m3.拟合了苯环平面和吡咯环平面的平面方程,并求出两平面之间的二面角为68.11°.     

绿柱石晶体的水热法生长及特征研究

采用温差水热法,以分析纯的Al(OH)3和BeO以及无色纯净的石英为原材料,球形和//s(1121)的片状无色绿柱石为籽晶,在复杂的盐酸混合溶液中生长了无色透明的绿柱石晶体.利用双圈反射测角仪、电子探针、X射线衍射仪和红外光谱仪等仪器,对合成绿柱石晶体的形态、成分及晶体结构进行了详细的研究.结果表明,合成的绿柱石晶体为六方短柱状,主要发育平行双面c{0001}、六方柱m{1010}、a{1120}和六方双锥p{1011}四种单形.合成的绿柱石晶体的成分中(Na2O+ K2O)的质量分数约为0.59;,且c0/a0值为0.9988,可归属于"正常"绿柱石向"四面体"绿柱石的过渡范畴.在中性或弱碱性环境体系中,通过调整绿柱石中各成分的百分含量,有望在更低的温度、压力条件下合成出高质量的板柱状绿柱石晶体.     

一种改性的TGS:Be2+热释电单晶体

本文报道了在TGS中掺入适量的金属铍离子的新晶体生长特性,晶体形貌分析,同时测定了新晶体的热释电系数(P)、介电常数(ε)、居里温度(Tc).实验表明,在TGS中掺入金属铍离子生成的TGAS:Be2+晶体的优值比明显提高.     

Crystal and molecular structure of rubidium azidotrimethylaluminate,Rb[Al(CH3)3N3]

The crystal structure of rubidium azidotrimethylaluminate has been determined from three-dimensional counter data, and refined by full-matrix least-squares techniques. The crystals belong to the monoclinic space groupP2₁/n, witha= 10.003(5),b=7.497(4),c= 11.806(5) Å, = 108.70(3) °, andD _c= 1.58 g cm⁼³ forZ=4. The finalR factor for 922 observed reflections is 0.049. The compound is not isostructural with its cesium analog. The aluminum atom is coordinated in a tetrahedral fashion, and the Al-N bond length is 1.944(8) Å.     

Crystal structure and IR spectroscopic study of (CN3H6)2[(UO2)2(C2O4)(CH3COO)4]

Compound (CN₃H₆)₂[(UO₂)₂(C₂O₄)(CH₃COO)₄] is synthesized and characterized by IR spectroscopy and single-crystal X-ray diffraction [a = 8.5264(2) Å, b = 13.8438(4) Å, c = 10.7284(2) Å, β = 103.543(1)°, space group P2₁/n, Z = 2, and R = 0.0258]. The main structural units of the crystals are binuclear [(UO₂)₂C₂O₄(CH₃COO)₄]^2? groups, which belong to the A ₂ K ⁰² B ₄ ⁰¹ crystal chemical group of uranyl complexes (A = UO ₂ ²⁺ , K ⁰² = C₂O ₄ ^2? , and B ⁰¹ = CH₃COO^?). The coordination polyhedron of the uranium atom is the UO₈ hexagonal bipyramid with the oxygen atoms of the uranyl ion at the axial positions. Uranium-containing groups and guanidinium cations are connected by electrostatic interactions and by the hydrogen bond system, which involves hydrogen atoms of guanidinium cations and oxygen atoms of oxalate and acetate anions. The results of the spectroscopic study of the compound agree with the X-ray diffraction data.     

Molecular structure of AlH3[N(CH2CH2)3CH]2

Reaction of AlH₃[N(CH₂CH₂)₃CH] with hexamethyltrisiloxane, (OSiMe₂)₃, gives rise to the bis-quinuclidine complex AlH₃[N(CH₂CH₂)₃CH]₂, which has been characterized by ¹H and ¹³C NMR spectroscopy and X-ray crystallography. The molecular structure of AlH₃[N(CH₂CH₂)₃CH]₂ consists of a trigonal bipyramidal aluminum with axial coordination of the quinuclidine ligands. Crystal data: orthorhombic, space group Pbcn, a = 10.6895(9), b = 12.266(1), c = 12.3794(9) Å, V = 1623.2(2) ų, and Z = 4.     

N-亚水杨基正丁胺锌配合物的合成、谱学表征和晶体结构

以乙酸锌、正丁胺及水杨醛为原料在甲醇介质中反应,合成得到了席夫碱配合物N-亚水杨基正丁胺锌[Zn(CH3CH2 CH2CH2N=CHC6H4O)2],用元素分析、红外光谱、核磁共振氢谱和热重分析进行了谱学表征,培养了该配合物的单晶,并通过单晶X射线衍射测得其晶体结构为四方晶系, 空间点群为P-4,a=1.4380(2)nm,b=1.4380(2)nm,c=0.53803(18)nm,α=β =γ=90°,V=1.1126(4)nm3 ;Dc =1.247 g/cm3;Z=2;F(000) = 400;μ =1.12mm-1.锌离子位于变形四面体的中心,分别与两个席夫碱N原子和两个酚氧负离子形成配合物.     

Spectra and structure of organophosphorus compounds,XVIII: Infrared and Raman spectra of [(CH3)2PS]2, [(CD3)2PS]2, and [(CH3CH2)2PS]2 in the solid state

The infrared (80–3500 cm^–1) and Raman (10–3500 cm^–1) spectra of solid [(CH₃)₂PS]₂, [(CD₃)₂PS]₂, and [(CH₃CH₂)₂PS]₂ have been recorded. A complete vibrational assignment is proposed for tetramethyldiphosphine disulfide on the basis ofC _2h molecular symmetry. The observed intermolecular vibrations indicate little factor group effects, and no frequency differences were observed for the normal modes of the two different molecules which exist in the crystal as reported from the x-ray study. Most of the observed bands in the spectrum of tetraethyldiphosphine disulfide have been assigned. At least two of the three optical librational modes were observed in the Raman effect.     

Crystal Structure of Diethyl[(4chlorophenyl)(dibenzylamino)methyl]propanedioate

Abstract  

The titled new functionalized N,O,O-ligand of type diethyl[(4-chlorophenyl)(dibenzylamino)methyl]propanedioate (4) is prepared in good yield through condensation of dibenzylamine, with 2-arylidene-malonic acid diethyl esters 3. The structure of 4 was determined by spectral (IR, ¹H NMR), elemental analyses and X-ray diffraction data. The molecular conformation shows two possible pockets ready to coordinate two metal atoms.     

Crystal structures of [N(CH3)4](HSeO4) at 298, 363, and 380 K

Three crystalline [N(CH₃)₄](HSeO₄) modifications are studied by X-ray diffraction method at 298, 363, and 380 K. The high-temperature phases are characterized by disordering of HSeO₄-tetrahedra. The systems of hydrogen bonds and the mechanism of the phase transitions are considered.