Formation of inclusions in CaF2 single crystals

It is reported on formation of inclusions during the Stockbarger growth of CaF₂. It the centre of this paper, hollows (gaseous or vacuum inclusions) are considered. Two different kinds of formation processes being possible under special growth conditions are discussed (segregation of gaseous impurity, entrapment of impurity-rich liquid at cell boundaries of growth cells).     

Growth of single crystals of barium iodate and strontium iodate in silica gels

Single crystals of iodates of barium and strontium grown by gel method are reported. Optimum conditions for good quality single crystals are worked out. Different habits of these crystals are reported. A brief report for characterization of these crystals by different methods is given.     

Solubility of CaO in CaF2 crystals

By means of conductivity investigations the solubility of CaO in CaF₂ crystals was estimated to be C_L(CaO) ≈︁ 3.7 exp (-0.68 eV/kT) = 3.7 exp (-7900 K/T) and the diffusion constant of O⁻ ions in CaF₂ D(O⁻) ≈︁ 3 exp (-2.2 eV/kT) cm²/s = 3 exp (-25 500 K/T) cm²/s.     

Growth of single crystals of potassium chloride from gels

The growth of single crystals of potassium chloride (KCl) in silica gels upto 3 × 3 × 3 mm³ in size is described. To crystallize KCl incorporated in the gel, hydrochloric acid has been used to crystallize the KCl in the gel media. The crystalline perfection has been studied by the chemical etch pit technique.     

Growth of octacalcium phosphate and dicalcium phosphate dihydrate crystals in silica gels

The crystallization of octacalcium phosphate (OCP) and dicalcium phosphate dihydrate (DCPD) have been studied at ambient temperature in silica gel using double diffusion system. The first stage of evolution of the OCP spherulites as well as their growth have been observed by optical microscopy. The growth rate of the OCP spherulites under stable external conditions was constant. The formation of DCPD crystals has been observed in the last stages of experiments.     

Etching and kinetics of dissolution of Mo1−x WxSe2 single crystals

The dislocation etchant has been established for single crystals of Mo_1−xW_xSe₂ system. Effect of concentration of an etchant on the etch rate has been discussed. The morphology of etch pits is also described. The etch activation energies for all the compositions of these crystals for a particular concentration (7 N) of an etchant has been found out. The etch activation energies for a particular composition (x = 0.4) of crystals with different concentrations of an etchant have been investigated and the results have been discussed.     

Influence of oxygen on electrical properties of CaF2 crystals

The O²⁻ ions appear as an unwanted impurity that contaminates the crystals of alkaline and rare earth fluorides during their preparation. The easy incorporation into the lattice and difficulties with their detection make the measurement of electrical properties problematical. In order to elucidate the influences of oxygen on CaF₂ crystals we have measured electrical conductivity. The crystals were prepared from a raw material of various moisture content, or they were doped by CaO, respectively. The measured courses exhibit equal activation energy E = 0.64 eV in the middle range. We thus conclude that synthetizing the crystal contaminated by moisture yields incorporation of O²⁻ ions only. We proved that even a two hours delay of melted raw material in gaseous products of Teflon pyrolysis does not suffice to remove oxygen. The method is effective only when applied after drying of raw material in vacuum.     

An electrolytic method to grow copper dendrites and single crystals in gels

A new electrolytic method for the growth of any metallic crystal in gel by using gel as a medium for controlled growth, is reported. Different types of large dendrites and single crystals of copper were grown by electrolytic method in the gel medium. It is found that pH of the gel medium, the concentration of the supernatant solution, the current density and the electrode material used, have considerable influence on the habits of the dendrites and the single crystals thus grown. The surface features and morphology of crystals and dendrites were studied by optical and scanning electron microscopy. Compared to other conventional electrolytic growth techniques, the present method has a number of additional parameters that can be varied, and hence a more effective controlled growth of crystals is possible.     

Etching studies of tungstenite (WS2) crystals in acids

Single crystals of tungstenite (WS₂) have been grown by direct vapour transport or sublimation method. An etchant capable of revealing the sites of dislocations has been developed. The effects of etching time, etchant concentration and temperature on the selective etch rate have been worked out. It is seen that the etch rate is independent on time, but is influenced by the temperature and concentration of the etchant. The values of activation energy determined from the etch rate against temperature plots established that the process of etching in chromic acid is chemical reaction rate controlled. The effect of addition of HF to the above etchant has led to some further interesting results.     

Crystalline quality of lysozyme crystals grown in agarose and silica gels studied by X-ray diffraction techniques

The crystalline quality of hen egg white lysozyme (HEWL) crystals grown in agarose gels and in silica gels has been characterized by measuring resolution and mosaic spread. These crystals have been compared to solution grown ones. A quasi-plane-wave X-ray topography study has also been done on some crystals. The study concerns triclinic, monoclinic, orthorhombic and tetragonal forms of HEWL. One observes that the resolution is not really changed by gelling the growth medium, even for rather high gel contents (agarose 0.5% wt/wt). On the contrary, mosaicity, characterized through reflection profile recordings allows to differentiate crystals grown by different techniques: agarose gel grown crystals are, on average, better than solution grown ones but the best crystals are obtained in silica gel. X-ray topography confirms this result.     

Vanadyl ion stability in silica gels

Silica gels doped with vanadium were prepared from tetra ethyl orthosilicate and an aqueous solution of NH₄VO₃, at a final sol pH of 1.5–2.5. Absorption and electron paramagnetic resonance (EPR) spectral studies establish that under ambient conditions the incorporated pentavalent vanadium is stabilized as tetravalent vanadyl ion in the gel monoliths. Dried gels were very stable under ambient conditions, however, transformation of V⁴⁺ to V⁵⁺ was noted during gel densification.     

Characterization of lead(II)chloride single crystals grown in silica gel

Acousto‐optical materials play an important role in acousto‐optic devices as acousto‐optic modulators. Lead(II) chloride is an acousto‐optical material, having high figure of merit approximately ten times greater than that of lead molybdate, which is an efficient acousto‐optical material. It also possesses high birefringence, low attenuation coefficient, wide transparency range and good mechanical properties. This paper discusses in detail, the growth of single crystals of lead(II) chloride in silica gel by the process of diffusion in a highly acidic medium. Needle‐type lead(II) chloride crystals have been obtained. The crystal system is confirmed to be orthorhombic by powder X‐ray diffraction analysis. To study the optical transparency of the grown crystal, the transmission spectrum has been recorded in the range 190 – 1100 nm. Thermal stability of the crystal is also studied. Results are discussed in detail. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of ytterbium tartrate trihydrate crystals in silica and agar‐agar gels and their characterization

Single crystals of ytterbium tartrate trihydrate have been grown by gel method using silica and agar‐agar gels as media of growth. The medium of growth influences the morphology of grown crystals, silica gel yielding single and polycrystalline in the form of spherulites whereas agar‐agar gel leading to growth of single and twinned crystals. Materials grown as single crystals have been characterized by using optical and scanning electron microscopy (SEM), EDAX, XRD, FT‐IR, CHN and thermogravimetric techniques. The stoichiometry of the grown single crystals is suggested to be Yb(C₄H₄O₆) (C₄H₅O₆).3H₂O. The FT‐IR spectrum shows the presence of singly as well as doubly ionized tartrate ligands. Results of thermal analysis indicate that the material is thermally stable up to a temperature of 200 °C. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Drying evolution of wet silica gels

Two kinds of porosity have been found in wet gels prepared by an esterification-controlled hydrolysis: macropores and mesopores. The textural evolution during the during shows that the most dilute gel shrinks the most rapidly. The dynamical part of the Scherer model gives a good account of this observed behavior.     

Characterization of pure and doped potassium hydrogen tartrate single crystals grown in silica gel

Growth of pure‐, sodium‐ and lithium‐ doped potassium hydrogen tartrate single crystals by gel technique is reported. Growth conditions conducive for the growth of single crystals are worked out. The crystals are characterized by using powder XRD, SEM, FTIR, AES, EDAX, CH analysis and thermoanalytical techniques. The stoichiometric composition for the grown crystals are established as KHC₄H₄O₆.H₂O, (K)_0.98(Na)_0.02.H₂O and (K)_0.94(Li)_0.06HC₄H₄O₆.H₂O. Doping of sodium and lithium in the pure potassium hydrogen tartrate single crystals is found to influence the size, perfection, morphology, crystal structure and the thermal stability of crystals. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Oxidation kinetics of BaF2 single crystals

Oxidation of BaF₂ single-crystals as a result of annealing in air in the temperature range 600° to 900 °C leads to mechanical strengthening. The process kinetics was investigated. It is shown that oxidation takes place in the bulk of crystals owing to oxygen diffusion by formation and growth of oxidation centres. These centres are precipitates of a BaO phase which were revealed by chemical etching.