Microstructures of gel-grown ammonium hydrogen tartrate single crystals

Single crystals of ammonium hydrogen tartrate (AHT) have been grown in silica gels by employing the controlled reaction between ammonium chloride and tartaric acid. Transparent AHT crystals upto 24 × 4 × 3 mm³ in size have been grown at room temperature. Optical and electron-optical studies have been made on the various surface structures of {010} faces of the grown crystals. A variety of growth striations and growth hillocks have been observed. Growth layers modified by the presence of misaligned microcrystals have been illustrated. It has been suggested that two-dimensional nucleation, spreading and pilling up of growth layers is mainly responsible for the growth of these crystals and the implications are discussed.     

Dislocation etching of tin iodide single crystals

Single crystals of tin-iodide (SnI₂) have been grown using the controlled reaction between SnCl₂ and KI by diffusion process in gel medium. As grown (010) surfaces of the crystals have been optically studied. Characteristic etch pits have been observed on them. This suggests that SnI₂ crystals might go into dissolution in the acid-set gel. By successively etching (010) surfaces in a mixture of ammonia, acetic acid, and CdCl₂ solution, it is established that the pits indicate the site of dislocations in the crystals. This is further confirmed by comparing the etch patterns before and after chemically polishing (010) surfaces. The average dislocation density in the crystals have been evaluated and found to be 3.2 × 10³ cm⁻² and the implications are discussed.     

Sub-boundaries on (002) cleavages of Li2CO3 single crystals

Linear arrays of dislocations (straight, terminating and curved) are observed on etching with 2% citric acid (002) cleavages of lithium carbonate (Li₂CO₃) single crystals, grown by zone melting technique. As the dislocations are non-uniformly spaced and disappear on successive etching, they may not be revealing low-angle grain boundary, nor slip traces as they are terminating and curved meaning crystallographically non-oriented. On the observation of experiments on successive etching and etching of matched pairs, it is concluded that the arrays of etch pits reveal dislocation walls (dislocation density 1.1 × 10⁶ — 1.5 × 10⁷ pits cm⁻²) probably created due to the localized thermal stresses released as a result of high temperature annealing of the crystal during growth. The implications are discussed.     

Dislocations of salol crystals grown by the Czochralski method

Crystals of salol were grown by the Czochralski method in three different pulling directions to examine the crystallographic orientation effect of the seed. They were characterized by the etch pit method and X-ray projection topography. It was found that the dislocation density was 2 × 10³−1 × 10⁴/cm² and that the configuration of dislocations was straight. The running directions of dislocations strongly depend on the pulling directions; i.e., [11 0] and [1 10] for the crystal grown in [100] axis, [11 0], [1 10] and [110] for the crystal pulled along [112] axis and [010] for [010] axis crystal.     

Thermal and infrared studies of calcium malate crystals grown in diffusion limited medium

Single crystals of the title compound Ca (C₄H₅O₅)₂.10H₂O are grown in silica gel using controlled chemical reaction method. Multifaceted single crystals of size up to 8 × 4 × 2 mm³ are obtained. Powder X‐ray Diffraction (XRD) pattern of the grown crystal and the Fourier Transform Infra‐Red (FTIR) spectrum in the range 400–4000 cm^–1 are recorded. The vibrational bands corresponding to different functional groups are assigned. Thermal decomposition stages observed in the Thermo‐gravimetric (TG) and Differential Thermal Analysis (DTA) studies are discussed. A six‐stage thermal decomposition scheme is proposed for the compound. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and characterization of ferroelectric magnesium hydrogen phosphate single crystals

Ferroelectric Magnesium Hydrogen Phosphate MgHPO₄ (MHP) single crystals are grown by slow diffusion of magnesium chloride in sodium metasilicate gels impregnated with orthophosphoric acid. Bright and transparent prismatic, tabular, and isometric habit MHP crystals upto 3 × 2 × 1 mm³ are obtained. Results of chemical, X-ray diffraction, EDAX, microhardness and magnetic analysis are reported. The average etch pit density is determined by chemical etching to be 7 × 10³ cm⁻². Microtopographic investigations revealed the mechanism of crystal growth.     

Flux crystallization of Pb(Mg1/3Nb2/3)O3 single crystals by the Czochralski method

Single crystals of lead magnesium niobate have been grown by flux crystallization using a modified Czochralski method. The crystals grown are free of pyrochlore impurity and have sizes of (15–28) × (20–30) × 20 mm³. The region of congruent melting of solution is determined. The PbO-B₂O₃ and PbO-B₂O₃-KBO₂ systems are chosen to be solvents.     

Dislocation activity in single crystals of stannic iodide

Single crystals of stannic iodide (SnI₄) have been grown employing the controlled-reaction between SnCl₂ and KI solutions by diffusion process in silica gels. As-grown (111) surfaces of the crystals have been optically studied. Characteristic growth spirals and hopper growth patterns have been observed on them. By successively etching (111) surfaces in a 0.2 N HCl solution, it is established that the pits indicate the sites of dislocations in the crystals. This is further confirmed by comparing the etch patterns before and after chemically polishing (111) surfaces. The average dislocation in the SnI₄ crystals have been determined and found to be 7.3 × 10² cm⁻². Observations of polygonisations are described and the implications are discussed.     

Microhardness studies of ammonium hydrogen tartrate single crystals

Single crystals of ammonium hydrogen tartrate AHT NH₄HC₄H₄O₆ have been grown employing the controlled reaction between NH₄Cl and (CHOHCOOH)₂ by slow diffusion process in silica gels. The variation in the microhardness of AHT crystals has been determined using Vicker's microhardness indentor. The effects of annealing and quenching on the mechanical properties of these crystals have been studied. It is observed that: (i) irrespective of the relative orientation of the indentor and the crystal, the median vents initiated at the sharp indentation edges, (ii) the microhardness of the crystals depends on the applied load, (iii) the microhardness of the crystal is independent on the duration of loading, and (iv) maximum plasticity is observed in quenched crystals. The implications of this behaviour are discussed.     

Kinetics of Etching of Dislocations in Ferroelectric Ammonium Hydrogen Tartrate Single Crystals

Ferroelectric crystals of Ammonium Hydrogen Tartrate (AHT) have been synthesised using the controlled reaction between NH₄Cl and (CHOHCOOH)₂ by diffusion process in silica gel medium. (010) cleavages of AHT crystals have been etched in 1.0 M and 1.5 M solutions of SrCl₂ solution. The lateral and normal velocities of the growth of pits were measured at different temperatures. The time dependence of the growth of the pit dimensions is found to be linear, whereas the temperature dependence of the growth of pits is found to be exponential, viz. \documentclass{article}\pagestyle{empty}\begin{document}$ \[V = A\,\exp \left({\frac{E}{{kT}}} \right)\] $\end{document}. The dissolution parameters, e.g. the activation energies and the pre-exponential factors for dissolution along the surface and along the dislocation lines have been computed. It is observed that the activation energy (E₁) of dissolution along [001] direction is found to be greater than the activation energy (E_b) along [100] direction and the implications are discussed.     

Enhancement of thermoelectric efficiency in vapor deposited Sb2Te3 and Sb1.8In0.2Te3 crystals

Pure and indium doped antimony telluride (Sb₂Te₃) crystals find applications in high performance room temperature thermoelectric devices. Owing to the meagre physical properties exhibited on the cleavage faces of melt grown samples, an attempt was made to explore the thermoelectric parameters of p‐type crystals grown by the physical vapor deposition (PVD) method. The crystal structure of the grown platelets (9 mm× 8 mm× 2 mm) was identified as rhombohedral by x‐ray powder diffraction method. The energy dispersive analysis confirmed the elemental composition of the crystals. The electron microscopic and scanning probe image studies revealed that the crystals were grown by layer growth mechanism with low surface roughness. At room temperature (300 K), the values of Seebeck coefficient S (⊥ c) and power factor were observed to be higher for Sb_1.8In_0.2Te₃ crystals (155 μVK⁻¹, 2.669 × 10⁻³ W/mK²) than those of pure ones. Upon doping, the thermal conductivity κ (⊥ c) was decreased by 37.14% and thus thermoelectric efficiency was improved. The increased figure of merit, Z = 1.23 × 10⁻³ K⁻¹ for vapour grown Sb_1.8In_0.2Te₃ platelets indicates that it could be used as a potential thermoelectric candidate.     

Study on rapid growth of KH2PO4 and its characterization

Large size crystals of KH₂PO₄ (KDP) were grown by adopting rapid growth technique from point seeds in a 1500‐liter crystallizer which is used to grow KDP crystals by conventional method. The grown KDP crystal size can reach to 310 × 310 × 320 mm³ and the average growth rate was 8mm/day. The optic properties of the rapidly grown KDP crystals were characterized comparing with the KDP crystals grown by the traditional temperature reduction method. We found it that the optical quality of the KDP crystals we grown rapidly are not significantly different from those of KDP crystals grown by traditional method. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and ionic conductivity of γ-Li<Subscript>3</Subscript>PO<Subscript>4</Subscript>

Single crystals of γ-Li₃PO₄ have been grown from flux. The 4 × 8 × 9-mm crystals have the cleavage along the [010] and [120] directions. The anisotropy in ionic conductivity in the grown crystals, ((σ ‖ a)/(σ ‖ b) = 2.5 and (σ ‖ a)/(σ ‖ c) = 1.3), is explained by specific features of the γ-Li₃PO₄ structure.     

Growth and etching of calcite crystals

Single crystals of calcite (CaCO₃) have been grown by the method employed by GRUZENSKY , using an aquoeus solution of CaCl₂ and a solid (NH₄)₂SO₃, The chemical reaction takes place according to the following equation: CaCl₂ + (NH₄)₂SO₃ CaCO₃ + 2 NH₄Cl The crystals grown by this method are about 0.2 to 0.8 mm in edge dimensions. Synthetic calcite crystals have been cleaved along (100) planes and the cleavage surfaces have been studied by multiple beam interferometry. The interferograms have revealed that the cleavages are quite flat. The cleavage faces have also been chemically etched and the etch patterns studied optically. By etching a cleavage successively for three different periods it was found that the bottoms of the point-bottomed pits follow a linear etch path. By etching a cleavage pair, one face in one etchant and the other face in a different etchant and by comparing the etch patterns produced, before and after polishing a cleavage face it has been shown that the etch pits nucleate at the sites of dislocations in the crystal. The etch patterns have also been compared with those produced on the cleavage faces of natural crystals. The density of dislocations in the syntheitc calctie crystals was generally less than the density of dislocations in the natural calcite crystals. The implications have been discussed.     

Studies of helical dislocations,polygonization and pile-ups of dislocations in magnesium orthosilicate single crystals

(010) cleavages of magnesium orthosilicate crystals have been etched in concentrated hydrochloric acid and in its vapour at room temperature and also in the melts of sodium and potassium hydroxides at 400 °. Evidences of helical dislocations with their axes along [100] and [001] directions as revealed by etching is reported. Observations of polygonizations and pile-ups of dislocations are described and the implications are discussed.     

Microhardness studies on as‐grown (111) faces of some alkaline earth nitrates

Single crystals of Sr(NO₃)₂, Ba(NO₃)₂ and Pb(NO₃)₂ are grown from their aqueous solutions at a constant temperature of 35 °C by slow evaporation technique. Crystals of size 8 to 10 mm along one edge are obtained in a period of 10 days. Chemical etching technique has been employed to study the dislocations in these crystals. The dislocations are randomly distributed and the dislocation density is about 10⁴ to 10⁵ /cm². Microhardness studies are made on as–grown (111) faces of these crystals upto a load of 100 g. The hardness of the crystals increases with an increase in load and thereafter it becomes independent of the applied load. These results are discussed on the basis of reverse indentation size effect. Meyer index number n for these crystals is estimated at both low and high load regions. An analysis of hardness data of these crystals as well as some other cubic crystals like alums and alkali halates are discussed using Gilman–Chin parameter H_v/C₄₄, where H_v is the microhardness and C₄₄ is the shear constant. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Dislocations in magnetic garnet crystals

1. Dislocations in magnetic flux-grown garnet crystals (Y₃Fe₅O₁₂ and others) have been observed. As a rule, {110} growth pyramids have more defects than {211} ones. 2. The highest content of defects (dislocation density 10³–10⁴ cm⁻²) is observed in Y₃Fe₅O₁₂ that grows on crucible walls adjacent to the free surface of the solution where the flow of heat is not uniform to the greatest degree. Bottom grown crystals usually have less dislocations. Far fewer dislocations are in wall grown crystals, least of all dislocations are contained in crystals that grow inside the solution. The solution pouring off at the end of the crystallization period increases dislocation density by some dozens. 3. Heat treatment decreases dislocation density. The less dislocation content and the lower ordering are in the initial crystal, the higher heat treatment effectiveness.     

Growth of α-NiSO<Subscript>4</Subscript> · 6H<Subscript>2</Subscript>O crystals at high rates

The high-rate growth of nickel sulfate hexahydrate NiSO₄ · 6H₂O (α-NSH) crystals up to 120 × 120 × 65 mm³ in size is described for the first time. The data on the distribution of related impurities in the {011} and {001} growth sectors of α-NSH crystals grown at different rates are reported. The transmission spectra of both growth sectors of these crystals are obtained. The structural quality and the optical properties of rapidly and slowly grown α-NSH crystals are compared. It is established that the {011} growth sector of crystals grown at rates exceeding 5 mm/day shows the best characteristics for application in UV filters.     

Growth and characterization of nonlinear optical zinc hydrogen phosphate single crystal grown in silica gel

Good optical quality single crystals of zinc hydrogen phosphate (ZnHPO₄) having dimensions up to 8×2×2 mm³ have been grown with the aid of sodium meta silicate gel. Single crystal XRD studies confirm that the crystal belongs to the orthorhombic system with space group P2₁2₁2₁. The functional groups present in the crystals were confirmed using FTIR technique. Optical absorbance shows very low absorption in the entire visible region. Differential thermal and thermo gravimetric analysis confirmed that the crystal is stable up to 193°C. Photoconductivity study reveals positive photoconductivity in the presence of photo active centers formed by trap energy levels. The NLO activity of the crystal was confirmed by Kurtz powder technique. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)