Influence of vapor transport equilibration on the crystal quality and thermal-expansion coefficients of gamma-LiAlO2

gamma-LiAlO2 (LAO) single crystal has been grown by the Czochralski method. However, its quality was deteriorated due to lithium volatilization during the crystal growth. The full width at half maximum value drops from 116.9 to 44.2 arc sec after the LAO slice was treated by vapor transport equilibration at 1000, 1100, and 1200 degrees C/48 h in sequence. The treated slice shows higher optical transmission than the as-grown one in the measured wavelength range of 190-1900 nm, meanwhile, its absorption edge exhibits a blueshift. According to Raman spectra, the treated slice has homogeneous quality at different depths from surface to 0.01 mm. The expansion coefficient of the treated slice for a axis drops from 17.2398x10(-6)/degrees C to 16.5240x10(-6)/degrees C, and that for c axis drops from 10.7664x10(-6)/degrees C to 10.0786x10(-6)/degrees C.

Influence of the AlN interlayer crystal quality on the strain evolution of GaN layer grown on Si (111)

The strain evolution in metal organic chemical vapor deposition growth of GaN on Si (111) substrate with an AlN interlayer is studied. During the growth of GaN film on AlN interlayer, the growth stress changes from compression to tension. The study shows that the density of V trenches in the AlN interlayer surface and the threading dislocations generated in the AlN interlayer have a significant influence on this strain evolution process. The dislocations generated in AlN interlayer may thread across the interface and play a key role in the strain evolution process of the GaN layer grown on AlN interlayer.

Effect of in situ thermal treatment during growth on crystal quality of GaN epilayer grown on sapphire substrate by MOVPE

GaN epilayers on sapphire substrate grown by metalorganic vapor-phase epitaxy (MOVPE) in a horizontal-type low-pressure two-channel reactor were investigated. Samples were characterized by X-ray diffraction (XRD), Raman scattering, atomic force microscopy (AFM) and photoluminescence (PL) measurements. The influence of the temperature changes between low temperature (LT) deposited GaN buffer and high temperature (WT) grown GaN epilayer on crystal quality of epilayer was extensively studied. The effect of in situ thermal annealing during the growth on improving the GaN layer crystal quality was demonstrated and the possible mechanism involved in such a growth process was discussed. (C) 2001 Elsevier Science B.V. All rights reserved.

Influence of Crystal Quality on the Excitation and Propagation of Surface and Bulk Acoustic Waves in Polycrystalline AlN Films

We investigate the excitation and propagation of acoustic waves in polycrystalline aluminum nitride films along the directions parallel and normal to the c-axis. Longitudinal and transverse propagations are assessed through the frequency response of surface acoustic wave and bulk acoustic wave devices fabricated on films of different crystal qualities. The crystalline properties significantly affect the electromechanical coupling factors and acoustic properties of the piezoelectric layers. The presence of misoriented grains produces an overall decrease of the piezoelectric activity, degrading more severely the excitation and propagation of waves traveling transversally to the c-axis. It is suggested that the presence of such crystalline defects in c-axis-oriented films reduces the mechanical coherence between grains and hinders the transverse deformation of the film when the electric field is applied parallel to the surface.

Systematic study on crystal-contact engineering of diphthine synthase: influence of mutations at crystal-packing regions on X-ray diffraction quality

It is well known that protein crystallizability can be influenced by site-directed mutagenesis of residues on the molecular surface of proteins, indicating that the intermolecular interactions in crystal-packing regions may play a crucial role in the structural regularity at atomic resolution of protein crystals. Here, a systematic examination was made of the improvement in the diffraction resolution of protein crystals on introducing a single mutation of a crystal-packing residue in order to provide more favourable packing interactions, using diphthine synthase from Pyrococcus horikoshii OT3 as a model system. All of a total of 21 designed mutants at 13 different crystal-packing residues yielded almost isomorphous crystals from the same crystallization conditions as those used for the wild-type crystals, which diffracted X-rays to 2.1 angstrom resolution. Of the 21 mutants, eight provided crystals with an improved resolution of 1.8 angstrom or better. Thus, it has been clarified that crystal quality can be improved by introducing a suitable single mutation of a crystal-packing residue. In the improved crystals, more intimate crystal-packing interactions than those in the wild-type crystal are observed. Notably, the mutants K49R and T146R yielded crystals with outstandingly improved resolutions of 1.5 and 1.6 angstrom, respectively, in which a large-scale rearrangement of packing interactions was unexpectedly observed despite the retention of the same isomorphous crystal form. In contrast, the mutants that provided results that were in good agreement with the designed putative structures tended to achieve only moderate improvements in resolution of up to 1.75 angstrom. These results suggest a difficulty in the rational prediction of highly effective mutations in crystal engineering.

Growth and characterization of high-quality LiAlO2 single crystal

g-LiAlO2 single crystal is a promising substrate for GaN heteroepitaxy. In this paper, we present the growth of large-sized LiAlO2 crystal by modified Czochralski method. The crystal quality was characterized by high-resolution X-ray diffraction and chemical etching. The results show that the as-grown crystal has perfect quality with the full width at half maximum (FWHM) of 17.7-22.6 arcsec and etch pits density of (0.3-2.2) x 10(4) cm(-2) throughout the crystal boule. The bottom of the crystal boule shows the best quality. The optical transmission spectra from UV to IR exhibits that the crystal is transparent from 0.2 to 5.5 mu m and becomes completely absorbing around 6.7 mu m wavelength. The optical absorption edge in near UV region is about 191 nm.

TlBr raw material purification, crystal growth, annealing, detector fabrication and characterisation for gamma-ray detector applications

The research reported in this thesis dealt with single crystals of thallium bromide grown for gamma-ray detector applications. The crystals were used to fabricate room temperature gamma-ray detectors. Routinely produced TlBr detectors often are poor quality. Therefore, this study concentrated on developing the manufacturing processes for TlBr detectors and methods of characterisation that can be used for optimisation of TlBr purity and crystal quality. The processes under concern were TlBr raw material purification, crystal growth, annealing and detector fabrication. The study focused on single crystals of TlBr grown from material purified by a hydrothermal recrystallisation method. In addition, hydrothermal conditions for synthesis, recrystallisation, crystal growth and annealing of TlBr crystals were examined. The final manufacturing process presented in this thesis deals with TlBr material purified by the Bridgman method. Then, material is hydrothermally recrystallised in pure water. A travelling molten zone (TMZ) method is used for additional purification of the recrystallised product and then for the final crystal growth. Subsequent processing is similar to that described in the literature. In this thesis, literature on improving quality of TlBr material/crystal and detector performance is reviewed. Aging aspects as well as the influence of different factors (temperature, time, electrode material and so on) on detector stability are considered and examined. The results of the process development are summarised and discussed. This thesis shows the considerable improvement in the charge carrier properties of a detector due to additional purification by hydrothermal recrystallisation. As an example, a thick (4 mm) TlBr detector produced by the process was fabricated and found to operate successfully in gamma-ray detection, confirming the validity of the proposed purification and technological steps. However, for the complete improvement of detector performance, further developments in crystal growth are required. The detector manufacturing process was optimized by characterisation of material and crystals using methods such as X-ray diffraction (XRD), polarisation microscopy, high-resolution inductively coupled plasma mass (HR-ICPM), Fourier transform infrared (FTIR), ultraviolet and visual (UV-Vis) spectroscopy, field emission scanning electron microscope (FESEM) and energy-dispersive X-ray spectroscopy (EDS), current-voltage (I-V) and capacity voltage (CV) characterisation, and photoconductivity, as well direct detector examination.

The Fluid Phenomena In the Crystallization Of the Protein Crystal

This paper reports that an optical diagnostic system consisting of Mach-Zehnder interferometer with a phase shift device and image processor has been used for study of the kinetics of protein crystal growing process. The crystallization process of protein crystal by vapour diffusion is investigated. The interference fringes are observed in real time. The present experiment demonstrates that the diffusion and the sedimentation influence the crystallization of protein crystal which grows in solution, and the concentration capillary convection associated with surface tension occurs at the vicinity of free surface of the protein mother liquor, and directly affects on the outcome of protein crystallization. So far the detailed analysis and the important role of the fluid phenomena in protein crystallization have been discussed a little in both space- and ground-based crystal growth experiments. It is also found that these fluid phenomena affect the outcome of protein crystallization, regular growth, and crystal quality. This may explain the fact that many results of space-based investigation do not show overall improvement.

3D Finite Volume Scheme for Czochralski Single Crystal Growth

Czochralski (Cz) technique, which is used for growing single crystals, has dominated the production of single crystals for electronic applications. The Cz growth process involves multiple phases, moving interface and three-dimensional behavior. Much has been done to study these phenomena by means of numerical methods as well as experimental observations. A three-dimensional curvilinear finite volume based algorithm has been developed to model the Cz process. A body-fitted transformation based approach is adopted in conjunction with a multizone adaptive grid generation (MAGG) technique to accurately handle the three-dimensional problems of phase-change in irregular geometries with free and moving surfaces. The multizone adaptive model is used to perform a three-dimensional simulation of the Cz growth of silicon single crystals.Since the phase change interface are irregular in shape and they move in response to the solution, accurate treatment of these interfaces is important from numerical accuracy point of view. The multizone adaptive grid generation (MAGG) is the appropriate scheme for this purpose. Another challenge encountered is the moving and periodic boundary conditions, which is essential to the numerical solution of the governing equations. Special treatments are implemented to impose the periodic boundary condition in a particular direction and to determine the internal boundary position and shape varying with the combination of ambient physicochemical transport process and interfacial dynamics. As indicated above that the applications and processes characterized by multi-phase, moving interfaces and irregular shape render the associated physical phenomena three-dimensional and unsteady. Therefore a generalized 3D model rather than a 2D simulation, in which the governing equations are solved in a general non-orthogonal coordinate system, is constructed to describe and capture the features of the growth process. All this has been implemented and validated by using it to model the low pressure Cz growth of silicon. Accuracy of this scheme is demonstrated by agreement of simulation data with available experimental data. Using the quasi-steady state approximation, it is shown that the flow and temperature fields in the melt under certain operating conditions become asymmetric and unsteady even in the absence of extrinsic sources of asymmetry. Asymmetry in the flow and temperature fields, caused by high shear initiated phenomena, affects the interface shape in the azimuthal direction thus results in the thermal stress distribution in the vicinity, which has serious implications from crystal quality point of view.

Growth and spectroscopic characteristics of Yb : GSO single crystal

For the first time, a high optical quality 10 at.% Yb3+-doped gadolinium oxyorthosilicate laser crystal Gd2SiO5 (GSO) was grown by the Czochralski (Cz) method. The segregation coefficient of Yb3+ was studied by the inductively coupled plasma atomic emission spectrometer (ICP-AES) method. The crystal structure has monoclinic symmetry with space group P2(1)/c; this was determined by means of an x-ray diffraction analysis. The absorption spectra, fluorescence spectra and fluorescence decay curves of Yb3+ ions in a GSO crystal at room temperature were also studied. Then, the spectroscopic parameters of Yb:GSO were calculated. The advantages of the Yb:GSO crystal include high crystal quality, quasi-four-level laser operating scheme, high absorption cross-sections and particularly broad emission bandwidth (similar to 72 nm). The results indicated that the Yb:GSO crystal seemed to be a very promising laser gain medium in diode-pumped femtosecond laser and tunable solid state laser applications when LD pumped at 940 and 980 nm.

gamma-LiAlO2 single crystal grown by Czochralski technique and modified by vapor transport equilibration (VTE) technique

Large-sized (similar to 2 inch, 50.8 mm) gamma-UA102 single crystal has been grown by conventional Czochralski (Cz) method, but the crystal ha's a milky, dendriform center. The samples taken from transparent and milky parts were ground and examined by X-ray diffraction. All diffraction peaks could be indexed in gamma-LiAlO2. The crystal quality was characterized by X-ray rocking curve. The full-width at half-maximum (FWHM) values are 116.9 and 132.0 arcsec for transparent and milky parts, respectively. The vapor transport equilibrium (VTE) technique was introduced to modify the crystal quality. After 1000 degrees C/48 h, 1100 degrees C/48 h, 1200 degrees C/48 h VTE processes, the FWHM values dropped to 44.2 and 55.2 arcsec for transparent and milky part, respectively. The optical transmission of transparent part was greatly enhanced from 85% to 90%, and transmission of milky part from 75% to 80% in the range of 190 similar to 1900 nm at room temperature. When the VTE temperature was raised to 1300 degrees C, the sample cracked and FWHM values of transparent and milky parts were increased to 55.2 and 80.9 arcsec, respectively. By combining Cz technique with VTE technique, large-sized and high quality gamma-LiAlO2 crystal can be obtained.

Growth and spectroscopic characteristics of Yb : LPS single crystal

For the first time, a high optical quality Yb3+-doped lutetium pyrosilicate laser crystal Lu2Si2O7 (LPS) was grown by the Czochralski (Cz) method. The segregation coefficient of ytterbium ion in Yb:LPS crystal detected by the inductively coupled plasma atomic emission spectrometer (TCP-AES) method is equal to 0.847. X-ray powder diffraction result confirms the C2/m phase monoclinic space group of the grown crystal and the peaks corresponding to different phases were indexed. The absorption and fluorescence spectra, as well as fluorescence decay lifetime of Yb3+ ion in LPS have been investigated. The absorption and fluorescence cross-sections of the transitions F-2(7/2) <-> F-2(5/2) of Yb3+ ion in LPS crystal have been determined. The advantages of the Yb:LPS crystal including high crystal quality, quasi-four-level laser operating scheme, high absorption cross-sections (1.33 x 10(-2) cm(2)) and particularly broad emission bandwidth (similar to 62 nm) indicated that the Yb:LPS crystal seemed to be a promising candidate used as compact, efficient thin chip lasers when LD is pumped at 940 and 980 nm due to its low-symmetry monoclinic structure and single crystallographic site. (c) 2007 Elsevier B.V. All rights reserved.

Growth, etching morphology and spectra of LiAlO2 crystal

gamma-LiAlO2 single crystal was successfully grown by Czochralski method. The crystal quality was characterized by X-ray rocking curve and chemical etching. The effects of air-annealing and vapor transport equilibration (VTE) on the crystal quality, etch pits and absorption spectra of LiAlO2 were also investigated in detail. The results show that the as-grown crystal has very high quality with the full width at half maximum (FWHM) of 17.7-22.6 arcsec. Dislocation density in the middle part of the crystal is as low as about 3.0 x 10(3) cm(-2). The VTE-treated slice has larger FWHM value, etch pits density and absorption coefficient as compared with those of untreated and air-annealed slices, which indicates that the crystal quality became inferior after VTE treatment. (C) 2008 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The influence of low-temperature Ge seed layer on growth of high-quality Ge epilayer on Si(100) by ultrahigh vacuum chemical vapor deposition

High-quality Ge epilayer on Si(1 0 0) substrate with an inserted low-temperature Ge seed layer and a thin Si0.77Ge0.23 layer was grown by ultrahigh vacuum chemical vapor deposition. The epitaxial Ge layer with surface root-mean-square roughness of 0.7 nm and threading dislocation density of 5 x 10(5) cm(-2) was obtained. The influence of low temperature Ge seed layer on the quality of Ge epilayer was investigated. We demonstrated that the relatively higher temperature (350 degrees C) for the growth of Ge seed layer significantly improved the crystal quality and the Hall hole mobility of the Ge epilayer. (C) 2008 Elsevier B.V. All rights reserved.

Effects of crystalline quality on the ultraviolet emission and electrical properties of the ZnO films deposited by magnetron sputtering

The ZnO films were deposited on c-plane sapphire, Si (0 0 1) and MgAl2O4 (1 1 1) substrates in pure Ar ambient at different substrate temperatures ranging from 400 to 750 degrees C by radio frequency magnetron sputtering. X-ray diffraction, photoluminescence and Hall measurements were used to evaluate the growth temperature and the substrate effects on the properties of ZnO films. The results show that the crystalline quality of the ZnO films improves with increasing the temperature up to 600 degrees C, the crystallinity of the films is degraded as the growth temperature increasing further, and the ZnO film with the best crystalline quality is obtained on sapphire at 600 degrees C. The intensity of the photoluminescence and the electrical properties strongly depend on the crystalline quality of the ZnO films. The ZnO films with the better crystallinity have the stronger ultraviolet emission, the higher mobility and the lower residual carrier concentration. The effects of crystallinity on light emission and electrical properties, and the possible origin of the n-type conductivity of the undoped ZnO films are also discussed. (C) 2009 Elsevier B. V. All rights reserved.