戊二酸十八酯晶体的合成和结晶习性研究

本文合成了有机晶体材料戊二酸十八酯(OGO),对其样品进行了表征和鉴定.对OGO在多种有机溶剂中的结晶性能进行了研究,结果表明在实验的几种有机溶剂中OGO的成核趋势很强,在甲苯和苯中具有较好的结晶特性.苯和甲苯可作为晶体生长的溶剂,但不是理想的溶剂.测定了OGO在苯和甲苯中的溶解度曲线,讨论了OGO在甲苯中的晶体生长条件.     

软X射线分光晶体琥珀酸十八酯的生长研究

本文合成了软X射线分光晶体材料琥珀酸十八酯(OSO),对其样品进行了表征和鉴定.对OSO在多种有机溶剂中的结晶性能进行了研究,结果表明在实验的几种有机溶剂中OSO的成核趋势很强,在甲苯和苯中具有较好的结晶特性.测定了OSO在苯和甲苯中的溶解度曲线,并用溶液降温法进行了晶体生长的实验.     

溶剂对有机非线性光学晶体NPAN生长习性的影响

本文测定了有机晶体N-(4-硝基苯)-N-甲基-2-氨基乙腈(简称NPAN)在某些醇和酮有机溶剂中的溶解度,研究了NPAN在这些有机溶剂中的溶液热力学性质、溶质与溶剂的相互作用以及溶剂对NPAN结晶习性的影响.根据界面熵因子α值,预测了NPAN晶体在不同溶剂中低指数晶面的晶体生长机制.选择丁酮为生长溶剂,进行单晶生长实验.在35～25℃温度区间内,用溶液降温法在较高过饱和度下成功地培养出尺寸为37×7.0×7.0 mm3的棱柱状透明单晶,所得晶体的外形与预测的结果相吻合.     

反式二苯乙烯(TSB)的溶液法晶体生长

本文观测了TSB在苯甲醚等有机溶剂中的结晶习性,测定了相应的溶解度曲线和亚稳区.采用溶液降温法在50~30 ℃的温度范围内进行晶体生长,获得透明度好的厘米级TSB晶体.通过对所得晶体进行X射线粉末衍射、紫外-近红外透过光谱、吸收光谱和紫外荧光光谱等测试,表明:本实验使用的不同生长溶剂对TSB晶体结构不会产生影响,所得晶体在410~1000 nm波长范围内透过率不低于80;,而在200~360 nm范围内有吸收,在波长为272.8 nm的激发光作用下,得到较强的荧光峰,峰位为386 nm.     

磺基水杨酸锶分光晶体生长的研究

本文采用液相法合成了高纯度磺基水杨酸锶(简称SSS)多晶粉末原料,并采用热分析、红外光谱和XRD分析对多晶粉末原料进行表征。以水为溶剂分别在不同pH值下(pH=2.50、1.50和0.60)进行了SSS结晶习性实验。结果表明,在水溶液中当pH=0.60时SSS结晶性最好,实验还测定了SSS晶体在不同pH值溶液中的溶解度曲线,并进行了过饱和溶液成核机理的研究。研究结果表明,当生长溶液pH为0.60时,控制单晶生长温度在40～50℃区间,采用水溶液降温法可生长出63 mm×25 mm×3 mm的透明单晶。     

软X射线分光晶体马来酸氢十六酯

马来酸氢十六酯(HHM)是一种长碳链酯晶体,晶面间距2d=5.85 nm,对软X射线有很好的衍射性能.它在苯和甲苯溶剂中表现很好的结晶性,增大溶剂的极性时明显地不利于HHM的结晶.以甲苯为溶剂,采用溶液降温法生长HHM单晶,控制晶体生长温度为32 ℃,降温速度为0.02 ℃/d,籽晶转速为6 r/min,经过约2周的生长时间,可以生长出30 mm×16 mm×1 mm的透明单晶体.HHM分子极易形成双分子缔合体,缔合体上由2个羧基组成的局域平面有利于分子的有序排列,这是HHM所以能表现出比其它长碳链酯有更好的结晶性的主要原因.     

马来酸氢十六酯(HHM)在过饱和溶液中的成核过程

本文研究了马来酸氢十六酯(HHM)在以甲苯为溶剂的过饱和溶液中的成核过程.测定了以诱导时间表示的成核速率.用经典的成核理论计算了固-液表面张力、成核自由能和临界成核半径.指出HHM晶体在甲苯为溶剂的过饱和溶液中的成核速率随着温度和过饱和比的提高而增大.溶剂的性质也将改变成核速率的大小.     

添加剂对硝酸钾结晶习性影响的研究

研究了Fe3+、Bi3+、pb2+、EDTA、柠檬酸、季铵盐和十二烷基磺酸钠共7种添加剂对硝酸钾结晶习性的影响,对不同添加剂在晶体表面的吸附机制进行了初步探讨.结果表明,随金属离子Bi3+、pb2+和EDTA浓度的增高,硝酸钾晶体c轴方向生长速度增大,晶体呈棒状;当柠檬酸添加量为100mg/L时,硝酸钾变为长片状;其他添加剂对硝酸钾结晶习性的影响效果则不明显.尽管某些添加剂可以改变硝酸钾的结晶习性,但粉末衍射和单晶衍射分析进一步证明,添加剂并未改变其晶胞参数及结构.     

水热体系中不同前驱物对合成镁铝水滑石微结构的影响

以不同的镁源、铝源组合为前驱物,利用XRD、SEM及EDS比较研究了水热体系中不同的前驱物组合对合成镁铝水滑石(Mg-Al-LDHs)晶体微结构及晶体生长的影响,同时利用生长基元的配位体理论对其生长机理进行了初步探讨.研究结果表明:当固定体系的pH =12,水热温度120℃、水热时间18h的条件下,不同的前驱物组合均可以合成结晶度较好的镁铝水滑石晶体;但不同的镁源、铝源组合对产物的物相、分散性、结晶规整性、厚径比、纯度、大小及微结构有一定的影响.当镁源固定为MgCl2,铝源分别为Al2O3、Al(NO3)3、AlCl3时,不溶性氧化铝合成的LDHs规整性、分散性及纯度较差,晶体发育不完整;当铝源分别为溶解度较好Al(NO3)3、AlCl3时,合成产物LDHs晶体的结晶度、规整性、分散性及纯度较好,但由于溶解度和相连阴离子极性的不同,造成产物微结构的微小差异;当镁源固定为溶解度较大的Mg(NO3)2时,铝源分别为Al(NO3)3、AlCl3时,同溶解度较小MgCl2相比,更有利于合成结晶度、规整度、尺寸更小的镁铝水滑石晶体.溶解度较大的镁源、铝源前驱物组合合成的镁铝水滑石有更高的结晶度和规整度.EDS分析证实,溶解度较差的Al2O3合成的镁铝水滑石纯度较差.溶解度较好的不同镁源、铝源前驱物组合合成的镁铝水滑石不含有任何其它阴离子杂质,平均镁铝比约为3,非常接近LDHs的理论值.     

超快闪烁晶体碘化亚铜的生长研究

在氮气保护的条件下,采用恒温蒸发法,在乙腈溶液中生长超快闪烁晶体碘化亚铜,获得了尺寸为3 mm×2 mm×2 mm的单晶体.测定了CuI在乙腈中的溶解度曲线和结晶度曲线.利用紫外-可见光谱对CuI的乙腈溶液中的碘离子存在形式作了判断和分析,对溶液中的黑色沉淀物氧化铜进行了IR和XRD表征.通过结晶实验,研究了温度、氧气和还原剂对晶体结晶形态的影响.实验表明:晶体生长温度应在45 ℃以上,铜粉具有很好的还原性能.     

Effect of different solvents on the habit of meta‐nitroaniline single crystals

The habit of the organic non‐linear optical material meta‐nitroaniline (mNA) crystallized from different organic solvents such as acetone, benzene, ethyl acetate, n‐hexane, methanol and toluene were studied. Solubility of mNA in these solvents at various temperatures in the range between 288 and 323 K was determined by gravimetric method. Crystals were grown by restricted evaporation of solvents method. Solutions with different solvents having different chemical nature and polarity yielded crystals with different habits: one‐dimensional needles, two‐dimensional rhombic platelets and three‐dimensional octahedral. In addition, the mNA crystals show unidirectional growth behaviour along its polar [001] direction irrespective of the solvents used. All the grown crystals were found to be orthorhombic system with point group mm2 and space group Pbc2₁ which was confirmed by powder X‐ray diffraction study. Optical transmittance study showed that the grown mNA single crystals have optical transparency in the wavelength range between 430 and 1550 nm. SHG efficiency of the grown mNA crystal was 3 times grater than KDP. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of the New Infrared Nonlinear Optical Crystal DCNP

This paper reports on the growth of 3-(1,1-dicyanothenyl)-1-phenyl-4,5-dihydro-1 H-pyrazole (DCNP) crystals in dimethylformamide. The effect of different solvents on the growth of DCNP has been investigated. Dimethylformamide was found to be a good solvent, Transparent DCNP single crystals were grown from this solvent. They are a promising infrared nonlinear material.     

Characterization of L‐ascorbic acid single crystals grown from solution with different solvents

Single crystals of L‐ascorbic acid, popularly known as vitamin‐C, were grown from solutions with different solvents and solvent combinations by low temperature solution growth methods. The suitability of different solvents and solvent combinations such as acetone, ethanol, methanol, isopropyl alcohol, water, water + acetone (1:1), water + ethanol (3:1), water + isopropyl alcohol (3:1) and isopropyl alcohol + methanol (1:1) for crystal growth of L‐ascorbic acid was found out by assessing the solubility and crystallization behaviours. Solubility of L‐ascorbic acid in selected solvents and solvent combinations in a range of temperatures was determined by gravimetric method. Solution prepared with water, water + acetone (1:1), water + ethanol (3:1) and water + isopropyl alcohol (3:1) were yielded crystals with tabular, columnar and prismatic habits and their morphologies were evaluated by goniometry. Grown single crystals were characterized with various instrumental techniques such as powder X‐ray diffraction, Fourier infrared spectroscopy, optical transmittance study, differential scanning calorimetry and second harmonic generation studies. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of L‐valine ‐ a nonlinear optical crystal

The growth of a new nonlinear optical material L‐valine by solvent evaporation method is reported here. To grow good quality crystals pH value of growth solution has been optimized and solubility of L‐valine in different solvents and different pH values was determined. The grown crystals were characterized by IR, single crystal XRD, DTA and TGA, optical transmission and second harmonic generation (SHG) efficiency measurement. SHG efficiency of L‐valine was found equivalent to KDP and its transmission is 75%‐80% from ultraviolet to near IR region. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of high quality anthracene crystals by a simple solution technique

In recent years considerable effort has gone into the preparation and characterisation of high purity anthracene crystals, since anthracene is used as a model organic molecular crystal in studies of solid‐state properties. Studies of organic molecular crystals and their applications in optics and electronics have been increasing attractive interest. Several attempts have been made to grow single crystals of anthracene. This is the first attempt to grow high quality anthracene crystals by solution technique adopting slow evaporation method in different solvents like CS₂ and CCl₄. The harvested crystals were subjected to various characterization studies. The results of characterisation studies support the purity of solution grown anthracene crystals. The solubility of anthracene in various solvents like CS₂ and CCI₄ was determined. The crystals of anthracene were grown by systematic method of slow evaporation technique in various solvents. Different morphology is noted with varying solvents. The crystal was subjected to XRD studies, FTIR studies and thermal studies. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Shape evolution of zinc oxide from twinned disks to single spindles through solvothermal synthesis in binary solvents

Shape evolution of ZnO crystals from twinned disks to single spindles was studied through solvothermal synthesis in binary solvents N,N-diethylformamide (DEF) and methanol (MeOH). The MeOH content in DEF had large influence on the morphology of the obtained ZnO crystals. In MeOH-free DEF, well-shaped ZnO twinned disks with perfect mirror symmetry could be formed through the assembly of ZnO₄⁶⁻–julolidinium–ZnO₄⁶⁻ growth units on the (0 0 0 1) growth interfaces. For small amounts of MeOH (MeOH/DEF=0.04), elongated twinned disks were formed since the growth along the polar c-axis was enhanced. With increasing MeOH content (MeOH/DEF=0.1), twinned rods with reduced mirror symmetry were formed. When a large amount of MeOH was added to DEF (MeOH/DEF=0.5), single spindles rather than twinned disks or twinned rods were obtained. A similar shape evolution of zinc oxide was observed in binary solvents DEF and N,N-dimethylformamide (DMF), suggesting that the growth of ZnO crystals with tuneable shape and size can be controlled by the composition of the binary solvent mixture.     

Growth from Solutions and Surface Properties of Anthracene Crystals

Crystallography Reports - The influence of different solvents on the growth of anthracene crystals from solutions and on their morphological quality has been investigated. The dependence of the...     

Crystallization of the E. coli polyamine-induced protein: a novel procedure based on the concept of ionic strength reducers

Nucleation and growth of macromolecular crystals occur in supersaturated solutions the properties of which depend on numerous parameters that influence macromolecular solubility. Detailed knowledge of the effects of those parameters is essential for crystallization. The concept of the so-called “ionic strength reducers” provides insight into the changes of solubility induced by organic solvents and hydrophilic polymers in aqueous electrolytic solutions. A simple and efficient procedure is presented which exploits the properties of ionic strength reducers in the crystallization of proteins. Using this procedure in the crystallization of the E.coli polyamine-induced protein, superior crystals compared to conventional techniques have been obtained. The procedure combines microseeding with dialysis techniques and is applicable to other proteins, particularly in cases where conditions favoring both for nucleation and growth cannot be found, or in cases where excessive nucleation leads to the growth of a large number of very small crystals.     

Understanding the effect of solvent polarity on the habit modification of monoclinic paracetamol in terms of molecular recognition at the solvent crystal/interface

The habit change of monoclinic paracetamol crystallized from solutions with different solvents such as water, ethanol, methanol, acetone, isopropyl alcohol, tetrahydrofuran, cyclohexanone, acetonitrile and 1, 4 ‐ dioxane was investigated. Change in solubility, pH and nucleation time of paracetamol in these solvents at ambient condition was studied. The polymorphic form of the nucleated paracetamol was observed under in‐situ optical microscopy. Solutions with different solvents having different chemical nature and polarity yielded paracetamol crystals with different habits: columnar morphology from polar protic water and prismatic morphology from other selected polar protic, aprotic and in non‐polar solvents. The significant differences on the growth rate of various crystal habit faces of the monoclinic paracetamol grown from different solvents are attributed in context with the solubility of the solute, solvent polarity, evaporation number of the solvent, rate of generation of supersaturation and the role of hydrogen bonding interaction between the solvent molecules and protruding solute molecules on the crystal surface. Among the solution with different solvents, bulk monoclinic paracetamol single crystal was grown from ethanolic solution using seed rotation technique by controlled cooling method.     

熔体分层对BaBiBO4晶体生长的影响

研究在用助熔剂法生长BaBiBO4晶体的过程中,熔体分层对晶体生长的影响.以Li2Mo3O10作为助熔剂,采用自发成核和顶部籽晶两种方法来生长晶体.对于这两种方法得到的晶体,用X射线粉末衍射及拉曼光谱进行了表征,结果显示,在晶体生长过程中,由于熔体分层,导致通过自发成核和顶部籽晶分别得到BaMoO4多晶和LiBaB9O15单晶两种不同的物相.