Low temperature X-ray diffraction study of CdI2 crystals

Solid state structural transformations in polytypic crystals of cadmium iodide have been investigated at low temperatures using X-ray diffraction techniques. The crystals were cooled to liquid nitrogen and liquid helium temperatures employing three different methods. The results obtained are discussed on the basis of bond dissociation energies of interlayer and intralayer bonds and the possible mode of layer displacements in MX₂-type polytypic crystals.     

Solvent effect on the polytype structure of CdI2 crystals

Single crystal platelets of cadmium iodide have been grown from alcohols: n-propyl, isobutyl and isoamyl and from their aqueous solutions. The structures of 880 crystals has been identified and the effect of solvent on the polytype structure of CdI₂ has been discussed regarding: the stability of the basic structures 2H and 4H, the structure of complex polytypes, the effect of the solvent on the structure of faults, the period of polytypes. Some relations indicating the role of the solvent in the formation of polytype structure of CdI₂ have been found.     

Micromorphology of pure and PbI2‐doped CdI2 dendritic single crystals

Undoped and PbI₂‐doped dendritic single crystals were grown by vapour growth technique. The basal surfaces of the as grown crystals were examined by optical and electron microscopy to observe wide variety of growth and defect features. Apart from typical features of dendritic growth, features of overgrowth, slip bands, growth steps and their bunching, etc. were observed. The basal surfaces of the crystals were then etched by controlled condensation of water vapour, after optimizing the etching condition, and the microscopic studies were repeated. Etch pits of hexagonal and triangular shape, both symmetric and asymmetric, and of different density, were observed in the case of undoped and doped crystals, respectively. In some cases, crystallographic hillocks were also observed. The crystals were also examined by X‐ray diffraction for their polytypism and related behaviour. The results are analyzed to elicit information on the correlation of structure, defects and surface features of the crystals. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

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.     

A speculation concerning the origin of long-range crystallographic order in polytypic and related crystals

It is suggested that long-range crystallographic order may be mediated by acoustic vibrations which have their origin in thermoacoustic phenomena and on which structural details exert a filter effect.     

Analysis of X‐ray extinction in crystals with inhomogeniously distributed dislocations

The secondary extinction theory of Zachariasen for mosaic crystals as well as the formalism of Becker&Coppens have been used for substructure analysis (lattice disorientations, block size, density of excess dislocations, etc.) in crystals with inhomogeniously distributed dislocations in the Bragg case of diffraction geometry. In the case of large crystals D_S ≫ Λ_hkl the mean total density ρ_D of randomly distributed dislocations was also estimated taking into account additionally the primary X‐ ray extinction treatment. In this connection two cases are considered: I) pure secondary extinction related to arrangement of dislocation walls and II) mixed extinction in crystals with large subgrains related to randomly distributed dislocations and arrangement of dislocation walls. In order to check the considerations, the experimental and calculated data were compared for Be (model I) and Cu (model II) single crystals. The weakly distorted single crystals of Be and Cu were experimentally investigated in the Bragg case of diffraction geometry using Cu Kα₁ radiation by means of double crystal diffractometer. A new experimental procedure was proposed. Using alternative technique for substructure analysis (for instance EBSD) the reliability of analysis based on extinction phenomenon in weakly distorted single crystals has been checked. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structure perfection of some molecular crystals grown from the melt

Single crystals of anthracene, naphthalene, phenazine and anthracene sym. trinitrobenzene (TNB) were examined using X-ray topography. Low-angle boundaries were observed and misorientation vectors of adjacent mosaic blocks have been estimated. Using an X-ray camera with oscillating film dislocation density in crystals has been evaluated. Anthracene-TNB crystals showed a much higher structure perfection than the other crystals.     

X‐ray Rotation‐Tilt‐Method — First Results of a new X‐ray Diffraction Technique

That from us as X‐ray Rotation‐Tilt Technique (XRT Method) designated procedure principle represents a world innovation and overcomes essential disadvantages of comparable diffraction techniques known up to now. Starting from the origin and the informational content of the XRT interferences a realization of a special equipment and selected examples of some first applications are presented.     

Growth imperfections in oriented grown KDP crystals by X‐ray topographic analysis

Potassium dihydrogen phosphate (KDP) crystals were restrained to grow in two dimensions only, using a specially designed platform. This enables us to grow the blanks of frequency conversion elements that satisfy type‐II phase matching direction out of a type‐II phase‐matched seed crystal. Synchrotron radiation topography was used to study the growth mechanism of these profiling grown KDP crystals. It is found that both dislocation growth mechanism and layer growth mechanism were involved in the growing process. Inclusions, growth striations and dislocations were the main defects that influenced the crystalline quality of these crystals. High‐resolution X‐ray diffraction was employed to study the lattice integrality of the crystal.     

Optical defects in barium—strontium niobate single crystals

The distributions of edge dislocations and residual mechanical stresses in Ba_xSr_1-xNb₂O₆ (BSN) crystals are investigated and the explanation of the nature of the “growth column” is proposed. The “growth column” is a defect zone going through all of the crystal and usually repeating in its cross-section the contour of the seed crystal. The “growth column” boundary is the closed contour with extremely high edge dislocation density. These dislocations are connected with thermal stresses due to seed-melt contact or abrupt crystal widening. Under proper crystal seeding and widening conditions one can obtain the BSN crystals with dislocation densities less than 10 cm⁻² and without the “growth column”. The method of chemico-mechanical polishing of BSN crystals not forming a defect layer on the surface of the crystals have been developed. The high temperature diffusion annealing is shown to eliminate the growth striae in BSN crystals.     

Structure of 2-methyl-1,3-cyclohexanedione crystals

The crystal structure of 2-methyl-1,3-cyclohexanedione, C₇H₁₀O₂, has been determined by X-ray methods. The finalR=0.039 for 513 observed reflections and 74 refined parameters. The molecules are present in the enolized form in the crystal. Hydrogen bonds-OH--O=, in stereochemical conformation [anti-anti]anti, of 2.590(2)Å link the molecules into planar chains along [010]. The molecules have a mirror-plane symmetry. The molecular ring is in a half-chair conformation. Two methylene groups C(4)H₂ and C(5)H₂ are dynamically disordered each in two sites on opposite sides of an otherwise planar molecule. An onset of ordering of the methylene groups would break the symmetry of mirror plane and induce a phase transition changing the space group symmetry of this crystal.     

Thermal behavior of biogenic apatite crystals in bone: An X‐ray diffraction study

The thermal behavior of the bovine bone mineral and synthetic stoichiometric hydroxyapatite was investigated by X‐ray diffraction. The bone samples in solid (planar oriented pieces) and in powder form were examined to elucidate how the microstructural and textural properties of bone mineral are modified under heating. As could be expected, the thermal behavior of the bone mineral depends not only on the structural distortions, but also on the crystal habit, texture and ordering of biocrystals in tissue. The temperature growth of biogenic apatite crystals, unlike synthetic hydroxyapatite, is seen to be nonmonotonic and multi‐staged. At 600 to 700°C the biomineral crystallites grow rapidly due to disappearance of the mosaic structure as the lattice imperfections are annealed. After heating between 700°C and 900°C the bone mineral appears to be composed of roughly equidimensional ≥200 nm crystals. The further growth of the crystals in the range from 900 to 1300°C occurs by the mass transport mechanism, supporting the idea that the bone mineral is not a discrete aggregation of crystals, but rather a continuous mineral phase with direct crystal‐crystal bonding. Estimates are presented to show the important role of the surface mass transport mechanism in the growth of apatite crystals. The material obtained by heating a cortical bone fragment between 900°C and 1300°C turns out to be composed of two crystal types: crystals oriented along the bone axis (major morphology) and those of differing shape and orientation (minor morphology). The heating‐induced variations in the longitudinal and transverse dimensions of differing‐morphology crystals are found to be coherent. Small amounts of CaO, MgO and other crystalline phases are seen to be formed in the bone mineral under heating. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Dielectric Properties of Superionic System AgBr—PbI2—Ag2O—B2O3

Dielectric properties of the system AgBr—PbI₂—Ag₂O—B₂O₃ has been studied for various temperatures and frequencies. Conductivity of the sample has also been measured and it is found that at 160 °C it attains the value 5.9 × 10^—3 (Ohms cm)^—1 and the activation energy calculated from the Arrhenius is found to be 0.16 eV.     

Investigation of InAs—InSb solid solution heteroepitaxial layers and structures

The results of investigations concerning the peculiarities of obtaining InAs—InAs_1−xSb_x heterostructure and of its properties revealed that the quality of epitaxial layers as well as photoelectric and electroluminescent device structure characteristics are to a great extent determined by a disagreement magnitude of heterostructure materials. — To decrease the magnitude of disagreement at the layer-substrate boundary and to achieve the composition with x > 0.1 at some distance the method of layer-by-layer growth (ANDREWS et al.) and the obtaining a graded heterojunction with optimization of component distribution along epilayer thickness seems to be promising.     

Microtip roughness of erosion-induced disturbed layers in silicon carbide crystals

The defect structure of a disturbed layer formed in the process of erosion cutting of bulk silicon carbide crystals has been studied experimentally. The characteristic features revealed are discussed in terms of the erosion-front interaction with growth defects and of the partial electrical volume breakdown in SiC.     

Contribution of Z1-centers in radiation hardening of NaCl: Sm2+ crystals — a study

Microhardness studies on X-irradiated NaCl and NaCl:Sm crystals are studied with varying times of X-irradiation in pre-quenched and quenched crystals. The contribution of Z₁-centers in radiation hardening studies is discussed.     

Re‐Investigation of the Structure of 7Bi2O3 · 2WO3 by Single‐Crystal X‐ray Diffraction

The structure of the oxygen‐deficient compound 7Bi₂O₃ · 2WO₃, a fluorite‐derivative phase considered a candidate for electronic applications because of its high ionic conductivity, is investigated by singlecrystal X‐Ray diffraction employing Ag‐Kα radiation (λ = 0.5608 Å) to minimize the effect of the absorption by the heavy metals. The space‐group type is I4₁, the acentric subgroup of I4₁/a that was previously suggested from powder‐diffraction data and precession‐camera photographs. Lattice parameters are a = 12.513(2), c = 11.231(4) (Z = 2.5). The sample is twinned by syngonic merohedry, class I, with volume ratio of the individuals 0.58/0.42. The ordering of W partly confirms previous models, with one W fully occupying one of the sites on special position. However, the remaining W goes in a site on general position, which shares with Bi, resulting thus more diluted in the structure. The oxygen vacancies are partly ordered in three of the ten anion sites.     

Spontaneous break of symmetry in molecular crystals

The structural dissymmetry of crystals with coordinated groups of atoms performing some motion in the crystal is described in terms of the theory of hindered molecular motion based on the dynamic principles of invariance for the extended angular jump model. The spontaneous break of the symmetry in the ordered ammonium chloride phase is discussed with the invocation of the proton-relaxation data.