Micromorphology of as-grown surfaces of crystals

This paper describes and discusses the micromorphology of as-grown surfaces of single crystals. After a brief introduction to the methods of observation of surfaces, the mechanism of growth and development of crystals is first outlined. Here the formation of bunches and macrosteps, the relationship between the growth mechanism and the surface entropy factor, and the effect of impurities on the surface morphology are described. Common structures observed on the as-grown surfaces are then explained in relation to growth conditions of the crystals. The following growth structures are described: elementary spirals, macrospirals, hillocks of dislocation and nondislocation origin, interlacing and slip patterns, macrosteps, inclusions, block structures, growth striations and impurity striations.     

Some observations of growth hillocks and growth layers on potassium hydrogen tartrate crystals

Some observations of growth hillocks and growth layers on the as-grown surfaces of potassium hydrogen tartrate (KHT) crystals obtained at 30 °C from aqueuos solutions of different supersaturations are reported and discussed. It is found that macrospirals, isolated growth hillocks, and growth layers are typical features observed on these crystals. Bunching of rectilinear growth layers originating from growth hillocks produced parallel macrosteps on the {010} faces. In certain cases, interaction of thick rounded layers of unequal height, emitted from neighbouring strong sources, gave rise to residual steps (pseudo-interlaced steps). Isolated growth hillocks produced by microbes were also observed.     

Influence of free convection on the formation of growth defects in potassium bichromate crystals grown from aqueous solutions

The influence of free convection on the formation of inclusions, growth bands and dislocations in potassium bichromate crystals grown by self-nucleation and on freely hanging seeds from aqueous solutions in a wide range of temperature is studied. It is found that in free convection all the three types of defects appear mainly in the top sectors but in stirred solutions the slow-growing faces are more defective.     

Heterometry-induced defects and stresses in isomorphously mixed crystals of varying composition

The comparative study of the distribution and density of dislocations and cracks in isomorphously mixed potassium-rubidium biphthalate crystals grown under the conditions of discrete and continuous changes of the solution composition with time. The method is developed for calculating the heterometry-induced internal stresses and the character of their variation in a crystal during its growth. It is established that formation of dislocations, cracks, and interzonal inclusions is associated with the effect of the heterometry-induced stresses, whereas the number of defects depends on the values of these stresses varying during crystal growth.     

The crystal growth and perfection of 2,4,6-trinitrotoluene

Large crystals of TNT were grown from ethyl acetate solution by both temperature lowering and solvent evaporation. The perfection of crystals grown from seeds under carefully controlled conditions was generally higher than those prepared by uncontrolled solvent evaporation. Examination by X-ray topography revealed the crystals to have a characteristic growth induced defect structure comprising growth sectors and boundaries, growth banding, solvent inclusions and dislocations. Twins and stacking faults (SF) were also observed. Many of the defects noted in the topographs can be attributed to impurities. The influence of the highly anisotropic crystal structure on the nature of growth defects is discussed. A structural model proposed to explain twinning and SF formation is partially supported by topographic evidence.     

Natural crystallization

Natural mineral crystals grow under a broad spectrum of conditions; from vapors, from hydrothermal solutions, from magmas (high temperature solutions), or through metasomatic or metamorphic reactions. In understanding kinetic problems involved in natural crystallization, there are two ways of approach; (1) experimentally stimulating textures of rocks, and (2) decoding the paragenetic information contained in natural crystals. The latter approach is especially important, since in situ observation is impossible. Key Key features which aid in deciphering natural growth processes and conditions include external forms, surface microtopographs of crystal faces, internal inhomogeneity (growth bands, growth sectors, inclusions, twin or exsolution textures), lattice defects (plane defects, dislocations) and impurities (precipitations). Mainly based on the observations of surface microtopographs of natural crystals, characteristics of crystallization in magma, in hydrothermal solution, in vapor phase, in hydrothermal metasomatism and in regional metamorphism are analysed and reviewed in this paper. The difference and similarity between natural and synthetic crystals are also discussed.     

Role of microcrystals in the growth and development of prism faces of cultured quartz (I). Attached microcrystals

Microcrystals attached in random orientations to growing host prism faces of cultured quartz grown by the hydrothermal crystallization technique are described. The microcrystals are established to be quartz. Growth layers and pyramids initiated by the attached guest microcrystals of quartz on the growing host prism faces of bulk quartz crystals are illustrated. Also described are striations, parallel, perpendicular and inclined to the c-axis, and polygonal growth pyramids on the prism surfaces of attached guest microcrystals. Formation of the microcrystals of quartz is linked to the possibilities of creation of quartz micronuclei in the autoclaves which further establishes and solidly supports the explanation put forward by KOTRU . Effect of unoriented attached tiny crystals of quartz and impurities on the progress of growth layers on the host prism faces is dealt with. Role of attached guest microcrystals in the growth and development of the host prism faces in particular and the cultured quartz in general is discussed. Possibilities of the incorporation of quartz micronuclei inclusions and impurity inclusions in the quartz structure and its effect on the crystalline quality of cultured quartz is briefly dealth with.     

CZ法生长参数对TeO2晶体质量的影响

本文主要讨论CZ法生长TeO2晶体中温度梯度、拉速、转速等工艺参数对晶体质量的影响,分析了晶体开裂、包裹物等宏观缺陷以及位错等微观缺陷的形成机理.从晶体形态、包裹体和位错密度变化等方面探讨了晶体生长参数与晶体缺陷之间的内在关系.     

Study on rapid growth of highly‐deuterated DKDP crystals

Highly‐deuterated potassium dihydrogen phosphate (DKDP) crystals were grown rapidly from point seeds under high supersaturation in a temperature range of 40‐60 °C. The growth rate was about 1‐2 order of magnitude higher than that of the traditional temperature reduction method. It was found that highly pure raw materials, overheating at high temperature, ultrafine filtration and supersaturation stability were needed to keep the solution from spontaneous nucleation at high overcooling. The effect of growth conditions on pyramid faces was different from that of prismatic faces. The tetragonal to monoclinic phase solubility transition scarcely occurred in our experiments even though the overcooling of monoclinic phase was as high as 10 °C in some cases. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Experimental and numerical investigation of buoyancy driven convection during PDAMNA thin film growth

This paper presents results from numerical simulations as well as laboratory experiments of buoyancy driven convection in an ampoule under varying heating and gravitational acceleration loadings. The modeling effort in this work resolves the large scale natural convective motion that occurs in the fluid during photodeposition of polydiacetelene films which is due to energy absorbed by the growth solution from a UV source. Consequently, the growth kinetics of the film are ignored in the model discussed here, and also a much simplified ampoule geometry is considered. The objective of this work is to validate the numerical prediction on the strength and structure of buoyancy driven convection that could occur under terrestrial conditions during nonlinear optical film growth. The validation is used to enable a reliable predictive capability on the nature and strength of the convective motion under low gravity conditions. The ampoule geometry is in the form of a parallelepiped with rectangular faces. The numerical results obtained from the solution to the Boussinesq equations show that natural convection will occur regardless of the orientation of the UV source with respect to the gravity vector. The least strong convective motion occurred with the UV beam directed at the top face of the parallelepiped. The strength of the convective motion was found to be almost linearly proportional to the total power of the UV source. Also, it was found that the strength of the convective motion decreased linearly with the gravity due to acceleration. The pattern of the convection flow on the other hand, depended on the source location.     

Atomic force microscopy studies on liquid inclusions and induced defects of cadmium mercury thiocyanate crystal

Liquid inclusions and various defects accordingly induced on a nonlinear optical material of CMTC crystal were investigated by atomic force microscopy. Liquid inclusions are chiefly caused by formation of macrosteps, which result from impurity‐induced inhibiting of step growth and meeting of step trains advancing along different directions. Liquid inclusions induce generation of dislocations and even cracks within the crystal by three‐dimensional nucleation growth. Liquid inclusions also provide screw dislocation growth sources, leading to formation of spiral hillock trains with ridged tails. Etching experiments reveal circular hollow cores, indicative of screw dislocation growth, and negative crystals resulting from further crystallization in the liquid inclusions. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

水热法KTP晶体生长与宏观缺陷研究

本文报道了水热法KTP晶体的生长工艺及晶体生长形态,系统研究了水热法KTP晶体的宏观缺陷,其宏观缺陷主要为添晶、生长脊线、裂隙和包裹体.提出了晶体生长工艺的改进措施,如提高原材料和试剂的纯度、调整籽晶的悬挂方式、减少籽晶的尺寸等,都可以减少晶体的宏观缺陷,提高晶体的质量.//(011)切向的籽晶生长的晶体质量较高,且能很好地应用于激光器件中.     

Preparation and Properties of YIG Single Crystals

In this paper a summary is given on the reproducible preparation of large, nearly defectless yttrium iron garnet single crystals (YIG) grown in fluxes by slowly cooling with accelerated crucible rotation (ACRT) and local bottom cooling. The surface morphology of the growth faces is discussed with regard to the growth mechanism. By different methods the crystals are characterized regarding their lattice defects (impurities, growth striations, dislocations, inclusions). Ferromagnetic resonance measurements in the X-band at polished, inclusionsfree discs show that the linewidth ΔH of any crystals from different runs are less than 0.45 Oe.     

Floating zone growth and characterization of ruby single crystals

Large, high optical quality single crystals of ruby have been grown successfully by the floating zone method under air atmosphere. The size of the grown crystal is typically 60‐70 mm in length and 7‐8 mm in diameter. The obtained crystals were red and did not have any macroscopic defects such as cracks and inclusions. Grown crystals were characterized by powder X‐ray diffraction (XRD) methods, polarized optical microscopy, scanning electron microscopy (SEM). The absorption and fluorescence spectra were measured at room temperature and the dielectric constant measurements of ruby crystals were also presented. Defects occurring in single crystals of ruby during crystal growth by floating zone method are described, and their correlation with the growth parameters is discussed. The origin and control of these defects in grown crystals were studied and the optimum method was proposed. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth from the vapour by surface nucleation

The experimental conditions under which cadmium sulphide is grown from the vapour to form crystals having a (11.0) singular growth faces are calculated. This is done assuming that growth proceeds on these faces by one-dimensional surface nucleation. Calculations based on this assumption are compared with experimental observations on the habit of CdS, and the relationship between growth rate and supersaturation, and shown to be consistent with these.     

Growth of Gallium Orthophosphate Single Crystals under Hydrothermal Conditions

Gallium orthophosphate (GaPO₄) single crystals have been grown from phosphoric acid solutions under hydrothermal conditions. The crystals have been studied in terms of twinning because of the strong effect of this structural defect on the piezoelectric properties. The growth rates of individual faces have been compared to each other by considering the dipyramidal habit of the grown crystals.     

Reducing Inversion Twinning in Single Crystal Growth of GaPO4

Gallium orthophosphate (GaPO₄) single crystals were grown by the reverse temperature gradient method from phosphoric acid solutions under hydrothermal conditions. Twins after (110) were studied by etching faces having been cut perpendicular to one of the twofold axes. Based on the determination of the twin boundary position as well as on the knowledge of the growth rates of different crystallographic forms, a few faces have been chosen to be quite promising for growing high‐quality GaPO₄ single crystals if they are offered at the referring seed crystal. From the characterization of the grown crystals conditions have been found, which may lead to the reduction of the inversion twin number during the growth process.     

Growth of borax crystals by spiral mechanism

Borax crystals grown at low supersaturation values are described. A brief report about microtopographical studies of these crystals is presented. Growth spirals observed on almost all the habit faces except those in contact with the bottom of the nucleation cell are described and discussed. It is established that all these crystals have platelet form in the initial stages of crystallization and as growth proceeds they develop and grow by spiral mechanism. The conditions under which the screw dislocations play the role in the development and growth of the crystals have been worked out.     

Morphology of BBO Crystals and their Inclusions

This paper reports on the morphology and inclusions in the low temperature phase barium metaborate BaB₂O₄(BBO) crystal grown by an improved flux pulling method. The morphology of ideal BBO crystals and the relationship between the faces and the growth rate are given. The result that BBO has the symmetry L₃3P and belongs to the space group C_3v−3m can therefore be concluded. It is found that the polarity of the BBO crystal along the Z (or c) axis has a visible influence on the morphology. The investigation of the inclusions in BBO crystals shows that these have a six-fold symmetry which corresponds to the extension of flute-like facets. It is also found that most of the inclusions have a regular geometric figure and can be regarded as the negative-crystal structure which is due to the internal growth mechanism.     

On the Mechanism of Crystal Growth from Undercooled Melts

The mechanism of crystal growth from undercooled melts is studied experimentally by means of a simple capillary technique. Thymol and Na₂S₂O₃ · 5 H₂O are used as model substances. Dislocation-free crystal faces of these compounds are obtained by continuous growth in the capillary or by prolonged annealing under appropriate conditions. Two-dimensional mechanism of growth was experimentally verified on such perfect crystal planes. The conditions under which the surface nuclation mechanism operates are described accounting for the supersaturation, the influence of impurities etc. Transition from two-dimensional into spiral growth of purposedly defected crystal faces is demonstrated and investigated. The mechanism of formation of perfect crystals is discussed and further experimental evidence on the possibility of two-dimensional growth from melts is given.