Formation of an internal bias field in chromium-and L, α-alanine-doped triglycine sulfate crystals

The unipolar state of a chromium-and L, α-alanine-doped ferroelectric triglycine sulfate (TGS) crystal has been studied. The experimental data on the distribution of internal bias fields with respect to a seed are considered. The possible mechanisms of the formation of an internal bias field during the growth of TGS crystals with a low impurity concentration are considered.     

Growth of TGS crystals using uniaxially solution‐crystallization method of Sankaranarayanan‐Ramasamy

The recently discovered crystal growth method called uniaxially solution‐crystallization method of Sankaranarayanan–Ramasamy (SR) is modified in some aspects and used for growth of triglycine sulphate (TGS) crystals. The modification leads to the simplicity, reduction of cost and avoided the temperature fluctuations. The 〈010〉 direction of TGS is very important and used for fabrication of infrared detectors. Using this method, the 〈001〉, 〈010〉 directional crystals of TGS were successfully grown in a glass crystallizer. The grown crystal was characterized by HRXRD, UV‐Visible and dielectric studies. The results prove the suitability of the modified SR method for oriented TGS crystal. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Modification of pyroelectric crystal TGS using thermodynamic theory

Based on the Devonshire thermodynamic theory, the relationship λ/χ = Ps/C can be regarded as a method to increase the pyroelectric material figure of merit of ferroelectric crystals. Several modified TGS crystals doped with urea or co-doped with urea and other dopants have been grown. The effect of the urea dopant on crystal growth and pyroelectric properties was investigated. The pyroelectric figures of merit M (λ/ε) of the doped TGS crystals are obviously higher than those of pure TGS. Furthermore, the variations of λ/χ and Ps/C as a function of temperature for these doped TGS single crystals were measured, and analyzed according to the Devonshire thermodynamic model.     

Study on the Growth of Triglycinsulphate Single Crystals

Crystallization of TGS at 52.0°C - above the transition point - has been studied in a wide range of supersaturation of the solution (σ = 0 to 10⁻²). The rates of growth of {110} and {001} faces were measured as a function of supersaturation at constant hydrodynamical conditions (Re = 3.4 · 10⁻³). Further, the influence of hydrodynamical conditions on the growth of {110} faces at constant supersaturation (σ = 4.2 · 10⁻³) was established. The parameters of the experimentally found dependences are determined on the basis of the surface-diffusion model of BURTON . CABRERA and FRANK . From these dependences follows that the growth rate of the {110} faces is already almost limited by the volume diffusion of TGS molecules towards the crystal surface, while in the case of {001} faces the surface diffusion mechanism of crystallization is clearly manifested. Dislocation densities in the crystals have been determined by means of etching technique. The number of dislocations increases with increasing supersaturation; hence, supersaturation of the solution together with the processes taking place in the regeneration zone surrounding the seed determine the number of dislocations in the crystal volume and thus the resulting structural perfection of single crystals. Investigation of the spontaneous redistribution of domains showed that the growth rate of TGS crystals influences the dielectric properties to much smaller extent than does chemical purity.     

Growing of TGS and TGSe single crystals at various pH of solution

The influence of pH of solution on growth rates of the faces (001), (010), (100) and habit of TGS and TGSe single crystals was studied. The pH-values were determined when growth of TGS and TGSe crystals was ceased. At pH < 1 diglycine sulphate (DGS) and at pH < 2 diglycine selenate (DGSe) crystals are growing. The permittivity and resistivity of DGS and DGSe were measured. The resistivity of DGSe is an order of magnitude less than of TGSe for the same temperature. The possible mechanism of change of crystal morfology vs pH, supersaturation of solution and growth temperature is proposed.     

Water-soluble ferroelectric crystals with inhomogeneous impurity distribution

Stabilization of the unipolar state via the formation of inhomogeneous impurity distribution in crystal bulk is considered. Possible growth of crystals with stable characteristics is demonstrated on triglycine sulfate (TGS) crystals with a regular inhomogeneous impurity distribution. The properties of TGS crystals with an inhomogeneous distribution of chromium ions grown above and below the Curie temperature T_C are studied. Inhomogeneous TGS crystals of three types are obtained: type-I crystals with a smooth variation of the concentration gradient along the growth direction, type-II crystals with a periodic layer variation of the impurity concentration, and type-III crystals with a sawtooth-like variation of the impurity concentration along the sample length. The TGS crystals with the regular inhomogeneous impurity distribution in the ferroelectric phase are characterized by higher values of the internal bias field E _b , unipolarity coefficient k, and pyroelectric coefficient γ than the inhomogeneous crystals in the paraelectric phase and the crystals with the statistic impurity distribution grown by the conventional method.     

Growth kinetics on the (100) and (001) faces of TGS crystals

The growth kinetics and mechanisms on the (001) and (100) faces of TGS crystals were investigated. A phase contrast microscope with a CCD camera was used to observe the growth of the crystal. We found the growth on the (001) and (100) faces at high supersaturation was mainly controlled by a BCF surface diffusion mechanism. The kinetic data for the (100) face were also fitted by the nucleation and layer growth model of two-dimension nucleation at high supersaturation. Some important growth parameters for TGS crystals, such as edge energy, activation energy, and so on, were estimated.     

Structure of the polar (010) cleavage of a ferroelectric TGS crystal from the atomic-force microscopy data

The atomically smooth polar (010) cleavage of a ferroelectric triglycine sulfate (TGS) crystal has been studied by the method of atomic-force microscopy. It is shown that the rounded 0.6-nm-high (deep) protrusions and pits with nanometer lateral dimensions revealed on the surfaces of TGS crystals are characteristic of their microrelief. These microrelief details can be formed either as a result of crystal cleavage in the ferroelectric phase or the mechanical action of a cantilever onto the crystal surface. These two-dimensional formations are relatively stable and genetically related to the layer structure of the ferroelectric phase of TGS crystals.     

Dielectric properties of triglycine sulfate crystals with defects at low and infralow frequencies

Dielectric responses of several crystals in ultraweak measuring fields at low and infralow frequencies are compared, namely, of nominally pure, Cr-and Lα-alanine-doped triglycine sulfate (TGS) crystals and TGS + Cr³⁺ crystals irradiated with X-rays. It is shown that dopant-induced bias fields give rise to crystal unipolarity, suppress the domain contribution to their dielectric response, and diffuse the phase transition. It is established that X-ray irradiation of the crystals results in “radiation annealing” of TGS + Cr³⁺ crystals, which increases their permittivity and diminishes diffusion of the phase transition.     

Investigation of the Solution Status of TGS and ATGSP Crystals

This paper reports on the solubility curves of TGS and ATGSP crystals with different pH's. The relationship of (010) growth rate in solutions with different pH varied with the supersaturation, has been studied. The influence of pH on the metastable region of solution have been measured. The experimential results are discussed with respect to the structure and viscosity of solution and the solubility of the crystals. Finally the optimum conditions for the rapid growth of TGS and ATGSP crystals is given.     

Kinetics of crystal growth of mirabilite in aqueous supersaturated solutions

The crystallization of sodium sulfate decahydrate (Na₂SO₄·10H₂O, mirabilite) from supersaturated solutions was investigated using stable supersaturated solutions seeded with mirabilite seed crystals. The experiments were done in batch, stirred reactors in which the supersaturated solutions were prepared either by dissolution of sodium sulfate anhydrous at 32 °C followed by cooling to 18 or 20 °C or by mixing equal volumes of equimolar ammonium sulfate and sodium hydroxide solutions at 20 °C. Inoculation of the solutions supersaturated only with respect to mirabilite with seed crystals was accompanied with temperature increase of the thermostated solution. Despite the fact that crystal growth was initiated with seed crystals, the process started past the lapse of induction times inversely proportional to the solution supersaturation. The rates of crystal growth were measured both from the temperature rise and from the concentration–time profiles, which were linearly correlated. The measured crystal growth rates showed a parabolic dependence on supersaturation at low supersaturations. For higher values this dependence changed to linear, a behavior consistent with the BCF spiral crystal growth model. The morphology of the crystals growing at 20 °C showed typical prismatic habit, while at 18 °C when crystallized from cooled sodium sulfate solutions changes in the crystal habit to a leaf like morphology were observed.     

Growth Kinetics and Mechanism of TGS Crystals

The growth kinetics of TGS crystals was studied at high supersaturations under the Curie temperature. The kinetics data proved that the crystal growth was mainly controlled by BCF surface diffusion model. The continuous growth was fitted to the growth rate data of (110) face. Its edge energy, Jackson factor, activity energies, kinetic coefficients were calculated.     

The influence of γ-irradiation on ferroelectric and polarization properties of TGS crystals

The experimental investigation of pyroelectric and polarization properties of TGS crystals was made. TGS crystals were grown under constant growth conditions (temperature and supersaturation of the solution) and γ-irradiated in a wide range of irradiation. The influence of γ-irradiation on the quality parameter M₂ of crystals, on the form of hysteresis loops, on size of spontaneous polarization and shifting field was ascertained.     

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.     

Edge-defined film-fed growth of Yb:YVO4 single crystal plates

The applicability of the edge-defined film-fed growth (EFG) technique for Yb_xY_(1−x)VO₄ (x=0.05, 0.1 and 1) was approved by successful growth of crystals up to 80 mm in length as the thin plates. Low-angle grain boundaries and the crystal coloration as main defects were found. Optimal seed orientation was suggested on the strength of vanadate crystal plate morphology. Optical properties, chemical composition and the crystalline quality were investigated.     

Improvement of growth habit and optical properties of rapidly grown KDP crystal by adding diethylene triamine pentacetate acid in growth solution

By altering the concentration of a new additive ‐ diethylene triamine pentacetate acid (DTPA) in the growth solution, a series of KDP crystals were obtained by the “point seed” rapid growth method. The growth rates up to about 20 mm/day. Effects of DTPA on the growth habit and optical properties of these as‐grown KDP crystals were investigated. The results reveal that, with the increase of DTPA concentration in growth solution, the contents of impurity metal ions incorporated into crystal and aspect ratio of crystal morphology were both decreased gradually, while the UV transmittance of crystal was enhanced continually. In the presence of moderate concentration of DTPA (100–200 ppm), the solution stability was increased and optical properties of crystal (including optical homogeneity, light scattering and laser damage threshold) were all improved. However excessive doping (>500 ppm) has opposite effects. The impact mechanism was also analyzed combining with the structure of KDP crystal and chemical characteristics of DTPA molecular.     

On the growth mechanism of sodalite single crystals grown by the hydrothermal method on single crystal seeds coated with informative informative interfacial layers

The growth mechanism of the early formation stages of sodalite single crystals grown by the method of hydrothermal synthesis on single crystal seeds coated with interfacial layers of polycrystalline silver has been studied at an electronmicroscopic scale. Coating with interfacial layers leads to a very weak adhesion between the overgrown single crystal and the surface of the interfacial layer on top of the seed, thus providing a unique possibility of detaching the overgrown single crystals from seeds and investigating the very early crystallization stages by the morphology of the growth surface. In local microregions of seed surfaces coated with interfacial layers discrete particles arise differing from one another in morphology, this being primarily associated with the electrical heterogeneity of seed surfaces. During crystallization, the space between the discrete particles was filled with the hydrothermal solution which represented a liquid interfacial layer exhibiting informative properties occurred under the influence of electrically active elements of the seed surface. At the boundary separating the liquid interfacial layers with particular informative properties from the rest of the solution volume, at early crystallization stages, together with the formation of discrete particles directly on the coated seed surface, growth of a continuous sodalite single crystal took place. The informative properties of seed surfaces, which are regularly modified due to coating with interfacial silver layers, determine the occurrence on local regions of seed surfaces (under appropriate crystallization conditions) of one or the other polymorphous modification: either hexagonal – cancrinite, or cubic – sodalite.     

掺杂TGS晶体的生长及热释电性能研究

选择重稀土离子Dy3 为掺杂阳离子,DL-丙氨酸与L-谷氨酸部分取代甘氨酸分子,生长了不同掺杂配比的TGS晶体。生长和测试实验表明,掺杂TGS晶体较纯TGS晶体易于生长。将掺杂晶体生长溶液的pH值控制在1~4,可改变掺杂晶体的结晶习性。用ICP发射光谱测试了掺杂晶体中稀土元素的含量,用X射线粉末衍射法测定了晶格参数,结果表明:元素已进入晶体,晶格参数稍有变化,但掺杂晶体的对称性仍为C2-2。通过测量掺杂晶体的电滞回线,得到了内偏压场,还测量了各样品的热释电系数、自发极化强度,作了温度曲线,并分析了各掺杂剂对提高热释电性能和锁定极化的作用。结果表明:是有应用前景的热释电材料。     

Rapid growth of KDP crystals in the coniform bottom device and their characterization

The coniform bottom device was designed and used in the rapid growth process of KDP crystal. A seed support rack was also designed to be used in rapid growth of KDP crystal to avoid spontaneous nucleation on the interface of seed crystal and rack. The KDP crystals were fast grown at the growth rate of up to 25 mm/day. The optical scatter centers in KDP crystals were observed and their transmissions of different parts were measured. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

A New Modified TGS Crystal

Triglycine sulfate (TGS) crystals doped with Cr⁶⁺ have been grown from a growth solution with various Cr⁶⁺ concentrations. The structure, transmission spectrum, pyroelectric properties, and the photorefractive effect of the crystals have been measured. It has a high internal bias field and photorefractive effect.