Deuterated hen egg-white lysozyme crystals: Optimization of the growth conditions and morphology

Deuterated and protonated tetragonal lysozyme crystals are grown using the hanging-drop vapor-diffusion method. The size of the lysozyme crystals grown is determined as a function of the concentration of sodium chloride used as a precipitant. It is found that crystallization leads to the formation of lysozyme crystals with three different habits. Morphological and X-ray diffraction analyses of the deuterated and protonated lysozyme crystals demonstrate that, despite the different habits, all the crystals grown belong to the tetragonal crystal system. The simple forms of lysozyme crystals are revealed. It is shown that the habits of the lysozyme crystals are determined by the specific combinations of simple forms. The mechanisms responsible for the formation of lysozyme crystals with different habits are discussed.     

Influence of gel inclusions on the mechanical behaviour of Gypsum

In a single test tube system, gypsum crystals grown in alcoholic gel comprise of interpenetration twinned crystals at the interface towards the gel, whereas untwinned tabular crystals are observed at greater depths inside the gel. By indentation of the crystals with a microhardness tool and recording the indentation impressions by means of a scanning electron microscope (SEM) and a transmission electron microscope (TEM) it is found that the hardness of the tabular crystals is of the same order of magnitude as those of natural crystals of gypsum, whereas interpenetration twinned crystals show a remarkable increase in hardness. On studying the morphology of cleavage faces and on carrying out energy dispersive X-ray analysis (EDXA), it is concluded that the increase in hardness of interpenetration twinned crystals with respect to tabular and natural crystals may be due to the role of the inclusion of gel particles during the growth. The implications are discussed.     

What is a protein crystal? Can we apply the terminology of classical industrial crystallization to them?

The nature of protein crystals is discussed. Since protein crystals contain not only proteins but also other substances the usage of conventional terms (of industrial crystallization) of naming such crystals is questioned. The proof that there are other components than the protein itself in a protein crystal is given. It is suggested to use a procedure like in biotechnology to guarantee the production of the right protein crystals according to the PAT concept. It is suggested not to use other established names like “hydrates”, “solvates”, “but crystals for proteins since the definitions do not fit the nature of the protein crystals.     

A survey of research on KTP and its analogue crystals

This paper reviews the growth and properties of KTiOPOP₄ (KTP) and its analogue crystals including its isomorphous crystals and doped crystals. Based on the calculation of the refractive indices and phase matching of KTP crystals, it is shown that non-critical phase matching can be achieved theoretically. In a 4%Nb-doped KTP crystal, non-critical phase matching was obtained with a pulsed Nd:YAG laser in an efficiency of ca. 4%. Most of the isomorphous and doped KTP crystals possess similar physical, optical and nonlinear optical properties as those of KTP.RbTiOPO₄, KTiOASO₄ and RbTiOASO₄ crystals have better electrooptical figure of merit and RbTiOPO₄ crystals have a fast ion conductor character. Some doped KTP crystals have shown high second harmonic generation efficiencies and damage thresholds. But the homogeneity of KTP analogue crystals is poorer than that of KTP. On the base of damage threshold tests using a CW Argon laser, it is concluded that the best second harmonic generation crystal among all the KTP analogue crystals is still KTP itself. Special care must be taken to eliminate impurity centers to avoid the formation of gray track and photorefractive centers.     

Mechanoluminescence of halogenate crystals

Mechanoluminescence (ML) has been studied in twenty halogenate crystals. All piezoelectric crystals show ML similar to the emission from second positive group of molecular nitrogen, and all the crystals not exhibiting ML are non-piezoelectric. Some of the non-piezoelectric crystals also exhibit nitrogen emission ML which is comparable in intensity to that of piezoelectric crystals. The ML appears only during the different steps developing in the fracture region of the force versus compression curve of the crystals. No considerable change in the ML activity is found due to the number of crystallization or due to the addition of different impurities from 100 to 10.00 ppm. The ML activity per mole of the halogenate crystals varies around four orders of magnitude. It is concluded that in addition to the piezoelectrification of the newly created surfaces there exists some other process of electrification which may cause the ML exitation in halogenate crystals.     

熔体法生长大尺寸有机晶体

大尺寸有机晶体在太赫兹波产生、中子探测、微波激射等多个关系国计民生、涉及国家安全的领域具有重要应用前景.但大尺寸有机单晶生长一直是国际公认的难题,无论是在生长理论、生长方法还是生长设备方面都远远落后,在整个人工晶体领域相对小众;而且有机晶体硬度低、脆性高、易解理等本征特性为加工和后期应用带来了很多困难,制约了相关领域的...     

Growth of CdBr2 single crystals by zone refining

CdBr₂ has been purified using a 12-pass zone-refining technique. Single crystals grown from the starting material showed arcing in the X-ray oscillation photographs whereas this is absent in the crystals grown from zone refined material. These crystals are found to be 6R type. In order to study the effect of impurities, DC conductivity studies were made on the crystals at various stages of purification. Surface morphology of the crystals have been studied using an optical microscope.     

溶剂蒸汽退火辅助微距升华法制备C8-BTBT单晶

有机半导体单晶由于具有内部长程有序的分子排列结构、缺陷及晶界少等优点,表现出优异的光电性能,是实现有机半导体器件实用化的一种重要材料。目前,研究者们已经发展出多种可应用于有机单晶的生长方法,其中,微距升华法是一种可以在大气环境下采用蒸镀的方式制备有机微/纳单晶的方法。然而,当将这种方法应用于C8-BTBT时发现,由于分子的熔点较低,蒸镀得到的是分子直接从液态凝固为无定形/多晶的结构。在本工作中,通过使用溶剂蒸汽退火的方式对其进行后处理,成功地将这种无定形/多晶结构转化为分立的单晶。为了表征所得到的晶体形貌和结构,分别使用光学显微镜、X射线衍射和原子力显微镜等仪器对其进行了表征,发现所制备的晶体结构具备单晶的典型特征。     

Growth of dl-malic acid-doped ammonium dihydrogen phosphate crystal and its characterization

Single crystals of dl-malic acid-doped ammonium dihydrogen phosphate have been grown using slow evaporation method and also by Sankaranarayanan–Ramasamy (SR) method with the vision to improve the properties of the ADP crystals. The characterization of grown crystals was made by single-crystal X-ray diffraction, powder X-ray diffraction, UV–vis. spectroscopy, Fourier transform infrared spectroscopy (FTIR), differential thermal analysis (DTA), Vicker's microhardness, dielectric measurements, high-resolution X-ray diffraction (HRXRD) and second-harmonic studies. Structural difference between pure and doped crystal has been studied by XRD analysis. Functional groups were identified by FTIR spectroscopy. The grown crystals were found to be transparent in the entire visible region. Decomposition temperatures of the grown crystals were measured by DTA. Vicker's hardness study carried out on (0 0 1) face at room temperature shows increased hardness of the doped crystals and SR-method-grown crystals. Dielectric measurements reveal that SR-method-grown DLM-doped ADP crystals have low dielectric loss. Crystalline perfection of the grown crystals is analyzed using HRXRD. Preliminary measurements indicate that the second harmonic generation efficiency of the doped crystals at a fundamental wavelength of 1064 nm is roughly 1.5 times greater than that of pure ADP.     

Crystallization mechanisms of acicular crystals

In this contribution, we present an experimental investigation of the growth of four different organic molecules produced at industrial scale with a view to understand the crystallization mechanism of acicular or needle-like crystals. For all organic crystals studied in this article, layer-by-layer growth of the lateral faces is very slow and clear, as soon as the supersaturation is high enough, there is competition between growth and surface-activated secondary nucleation. This gives rise to pseudo-twinned crystals composed of several needle individuals aligned along a crystallographic axis; this is explained by regular over- and inter-growths as in the case of twinning. And when supersaturation is even higher, nucleation is fast and random.In an industrial continuous crystallization, the rapid growth of needle-like crystals is to be avoided as it leads to fragile crystals or needles, which can be partly broken or totally detached from the parent crystals especially along structural anisotropic axis corresponding to weaker chemical bonds, thus leading to slower growing faces. When an activated mechanism is involved such as a secondary surface nucleation, it is no longer possible to obtain a steady state. Therefore, the crystal number, size and habit vary significantly with time, leading to troubles in the downstream processing operations and to modifications of the final solid-specific properties.These results provide valuable information on the unique crystallization mechanisms of acicular crystals, and show that it is important to know these threshold and critical values when running a crystallizer in order to obtain easy-to-handle crystals.     

Radiation hardening studies in KBr-KI mixed crystals

Radiation hardening studies have been made in KBr, KI and in different compositions of KBr-KI mixed crystals, grown from melt by Kyropoulos technique. The irradiation hardness in mixed crystals is found to vary non-linearly with composition, attaining a minimum value at intermediate compositions. Dislocation density measurements have shown a high concentration of dislocations and grain boundaries in mixed crystals as compared to end crystals. The results obtained on radiation hardening of mixed crystals were explained in terms of dislocations present in them.     

A new technique for the growth of superconducting YBa2Cu3O6 + δ crystals completely separated from flux

Growth of completely flux-separated YBa₂Cu₃O_{6 + δ} (referred to as 123 phase) crystals using a novel technique is described. The technique employs a modification of the seed pulling method commonly used in crystal growth. The crystals are grown in the temperature range of 960–1000°C using a BaCuO₂ flux. A 123 flux ratio of 1:5 is maintained. Photographs of the crystals and photomicrograph of the surfaces are presented to show complete flux-separation of the crystals measuring 6 mm × 3 mm × 1 mm. The Raman spectra recorded on the as-grown crystals show that they are in the tetragonal phase. Magnetic susceptibility measurements on crystals annealed in an oxygen atmosphere show a superconducting transition starting at 71 K. The present technique offers a possibility of growing large, completely flux-separated crystals of 123 for superconductivity research.     

Characterization of pure and urea-doped γ-glycine single crystals grown by solution method

Pure and urea-doped gamma-glycine (γ-glycine) single crystals were grown by solution method with slow evaporation technique. When urea was added as dopant, morphological alterations were noticed in γ-glycine crystals. Structural characterization of the grown crystals was carried out by single and powder X-ray diffraction (XRD) methods and it is observed that the samples crystallize in non-centrosymmetric space groups. UV-visible transmittance studies were performed to analyse optical transparency of pure and urea-doped γ-glycine crystals and found that the crystals were transparent in the entire visible-NIR region. Density and melting point of the grown crystals were measured. Second harmonic generation (SHG) for the grown crystals of this work was confirmed using Nd:YAG laser. Thermogravimetric and differential thermal analyses (TG/DTA) thermograms reveal that the materials have good thermal stability. From Microhardness studies, it is observed that urea-doped γ-glycine crystal is harder than pure (undoped) sample.     

Effect of external forces on the dielectric and pyroelectric properties of strontium-barium niobate crystals

It is shown that high-temperature annealing of strontium-barium niobate crystals increases the mobility of domain boundaries in these crystals. This effect manifests itself in a shift of the peak of the effective permittivity of annealed samples to weaker fields. It is ascertained that the polarization of strontium-barium niobate crystals caused by annealing results in their more homogeneous single-domain state. The effect of Ce and Cr impurities on the polarization state of the surface layers in strontium-barium niobate crystals is considered.     

Effect of ammonium malate on growth rate,crystalline perfection,structural, optical,thermal, mechanical,dielectric and NLO behaviour of ammonium dihydrogen phosphate crystals

The effect of ammonium malate on the growth rate, structural, optical, thermal, mechanical, dielectric properties, crystalline perfection and second harmonic generation (SHG) efficiency of ammonium dihydrogen phosphate single crystals grown by the slow cooling method has been investigated. The lattice parameters of the grown crystals were obtained by the single-crystal X-ray diffraction analysis. Fourier transform infrared studies confirm the functional groups of the crystals. UV–vis study shows that the transparency is increased much by the dopant. Thermal analysis was performed to study the thermal stability of the grown crystals. Vickers hardness measurements reveal the higher hardness of the doped crystals. Low dielectric losses were observed from the dielectric measurements for the doped ADP crystals. The high-resolution X-ray diffraction studies show that the crystalline perfection of the crystals is good. The relative SHG efficiency measurements revealed that the dopant has enhanced the efficiency.     

Curved focusing crystals for hard X-ray astronomy

A lens made by a properly arranged array of crystals can be used to focus x-rays of energy ranging from 30 to 500 keV for x-ray astronomy. Mosaic or curved crystals can be employed as x-ray optical elements. In this work self standing curved focusing Si and GaAs crystals in which the lattice bending is induced by a controlled damaging process on one side of planar crystals are characterized. Diffraction profiles in Laue geometry have been measured in crystals at x-ray energies E = 17, 59 and 120 keV. An enhancement of diffraction efficiency is found in asymmetric geometries.     

X-ray,optical and electrical study of melt-grown CdI2 single crystals

CdI₂ has been purified using the zone-refining technique by giving 20 passes. Single crystals grown from the starting material showed arcing in the X-ray oscillation photographs whereas it is absent in the crystals grown from the zone refined material. These crystals are found to be of the 4 H type. DC conductivity studies were made on these crystals at various stages of purification. The surface morphology of these crystals have been studied using an optical microscope.     

Influence of cluster defects of variable composition on the optical and radiative characteristics of oxide crystals

It is shown that oxide crystals contain cluster defects of variable composition, which cause absorption of light in the transparency region of crystals. The model based on the presence of cluster defects in oxide crystals explains well the experimental data on the thermal and radiative coloring of these crystals. It is noted that cluster defects accumulate oxygen in oxide crystals. These defects are responsible also for the photochromic effect in them. Application of the noted model made it possible to fabricate lead tungstate scintillators at North Crystals Company for the ALICE project (CERN) with almost 100% reproducibility of their operating characteristics.     

Growth and etching of anhydrous diglycine sulfate single crystals

Single crystals of anhydrous diglycine sulfate are grown at constant temperature by evaporation method. The crystals are grown at various temperatures and their growth rate is determined. A chemical etchant for dislocation studies is reported. The perfection of the crystals grown at various temperatures has been studied using etching technique. It is found that the crystals contained inclusions of the mother liquid. The crystals grown below 28° are almost free of inclusions and the dislocation density is also low.     

Morphology of PbI2 Crystals Grown by Gel Method

The single crystals of Lead Iodide have been grown by gel method. X‐ray diffraction studies on these crystals shows that the lattice parameters of grown crystals are almost matching with reported values. The results of detailed studies made on the microstructures of Lead Iodide crystals, have been described. The observations of the faces of these crystals revealed that they have grown by layer as well as spiral mechanisms. The probable role of these parameters is explained along with the surface microstructures on these various shaped crystals.