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High precision interferometric studies of step bunching on KDP crystal surface growing from solution moving at rates up to 1 d s . It is shown that the bunch height is limited as the bunch propagates over the surface. An hypothesis is put forward describing why the bunch height decreases as the solution flow rate increases.
In this study, crystals of CdTe were grown from melts by the unseeded vertical gradient freeze method. The quality of grown crystal were studied by various characterization techniques including Synchrotron White Beam X-ray Topography (SWBXT), chemical analysis by glow discharge mass spectroscopy (GDMS), low temperature photoluminescence (PL), and Hall measurements. The SWBXT images from various angles show nearly strain-free grains, grains with inhomogeneous strains, as well as twinning nucleated in the shoulder region of the boule. The GDMS chemical analysis shows the contamination of Ga at a level of 3900 ppb, atomic. The low temperature PL measurement exhibits the characteristic emissions of a Ga-doped sample. The Hall measurements show a resistivity of 1 x l0(exp 7) ohm-cm at room temperature to 3 x 10(exp 9) ohm-cm at 78K with the respective hole and electron concentration of 1.7 x 10(exp 9) cm(exp -3) and 3.9 x 10(exp 7) cm(exp -3) at room temperature.
A pull rod for use in producing a single crystal from a molten alloy is provided that includes an elongated rod having a first end and a second end, a first cavity defined at the first end and a second cavity defined at the first end and in communication with the first cavity. The first cavity receives the molten alloy and the second cavity vents a gas from the molten alloy to thereby template a single crystal when the pull rod is dipped into and extracted from the molten alloy.
Various studies of the concentration of the solution around a growing crystal using interferometric techniques are reviewed. A holographic interferometric technique used in laboratory experiments shows that a simple description of the solution based on the assumption of a purely diffusive mechanism appears inadequate since the convection, effective even in reduced columns, always affects the growth.
The experimental setup for the in-situ high resolution optical monitoring of protein crystal growth/dissolution morphologies was substantially improved. By augmenting the observation system with a temperature-controlled enclosure, laser illumination for the interferometric microscope, and software for pixel by pixel light intensity recording, a height resolution of about two unit cells for lysozyme can now be obtained. The repartitioning of Na(+) and Cl(-) ions between lysozyme solutions and crystals was studied. Quite unexpectedly, it was found that the longer crystals were in contact with their solution, the lower was their ion content. The development of a model for diffusive-convective transport and resulting distribution of the growth rate on facets was completed. Results obtained for a realistic growth cell geometry show interesting differences between 'growth runs' at 1g and 0g. The kinematic viscosity of lysozyme solutions of various supersaturations and salt concentrations was monitored over time. In contrast to the preliminary finding of other authors, no changes in viscosity were found over four days. The experimental setup for light scattering investigations of aggregation and nucleation in protein solutions was completed, and a computer program for the evaluation of multi-angle light scattering data was acquired.
We are developing a novel technique with which we have grown diffraction quality protein crystals in very small volumes, utilizing chip-based, microfluidic ("LabChip") technology. With this technology volumes smaller than achievable with any laboratory pipette can be dispensed with high accuracy. We have performed a feasibility study in which we crystallized several proteins with the aid of a LabChip device. The protein crystals are of excellent quality as shown by X-ray diffraction. The advantages of this new technology include improved accuracy of dispensing for small volumes, complete mixing of solution constituents without bubble formation, highly repeatable recipe and growth condition replication, and easy automation of the method. We have designed a first LabChip device specifically for protein crystallization in batch mode and can reliably dispense and mix from a range of solution constituents. We are currently testing this design. Upon completion additional crystallization techniques, such as vapor diffusion and liquid-liquid diffusion will be accommodated. Macromolecular crystallization using microfluidic technology is envisioned as a fully automated system, which will use the 'tele-science' concept of remote operation and will be developed into a research facility aboard the International Space Station.
High-resolution interferometry on facets of lysozyme crystals growing under steady external conditions revealed intrinsic kinetics instabilities that occur as fluctuations in the spacing of growth steps. The amplitude of these fluctuations is reduced by forced solution flow. This increased stability is interpreted in terms of the ratio of the characteristic rates of lattice incorporation and bulk transport. Apparently a steady state is approached as an asymptote of a continuous family of unsteady states.
The positive effects of microgravity on crystal quality and the fundamental properties of the vapor transport reaction were established by analyzing the results of three transport experiments on multicomponent systems performed during the Apollo-Soyuz Test Project mission. The systems employed were GeSe0.99Te0.01-GeI4(A), GeS0.98Se0.02-GeCl4(B), and GeS-GeCl4-Ar (C). The crystallographic analysis is based on a direct comparison of space and ground-based (prototype) crystals employing X-ray diffraction, microprobe, microscopic, and chemical etching techniques. The results demonstrate a considerable improvement of the space-grown crystals in terms of chemical and crystalline homogeneity, surface morphology, and bulk perfection relative to ground specimens.
The effects of asymmetry in furnace temperature profile and pulling velocity on the crystal interface shape are demonstrated while neglecting the latent heat of solidification. It is concluded that the furnace temperature profile may be varied in order to influence the interface shape of the crystal. An exact thermal analysis is performed on the Bridgman technique by including the latent heat of solidification as a source term. The exact temperature field is obtained for the case of a flat melt-crystal interface. The earlier observation regarding the influence of furnace temperature profile on the crystal interface shape is confirmed and a criterion for a flat crystal interface is obtained. Various furnace temperature profiles are selected and their corresponding results are presented.
The effects of asymmetry in furnace temperature profile and pulling velocity on the crystal interface shape are demonstrated while neglecting the latent heat of solidification. It is seen that the furnace temperature profile may be varied in order to influence the shape of the melt-crystal interface. An exact thermal analysis is then performed on the Bridgman technique by including the latent heat of solidification as a source term. The exact temperature field required for yielding a flat melt-crystal interface is obtained. The earlier observation regarding the influence of furnace temperature profile on the interface shape is confirmed and a criterion for achieving a flat interface is obtained. Various furnace temperature profiles are selected and their corresponding melt-crystal interface results are presented.
The surface morphology of freshly cleaved ZnSe single crystal grown by the physical vapor transport (PVT) method was investigated by Atomic Force Microscopy (AFM) and the results were correlated with Differential Scanning Calorimetry (DSC) data. Selenium precipitates have been revealed in undoped doped ZnSe crystals having a size of about 50 nm. A transition temperature around 221 C in the DSC measurements is interpreted as the eutectic temperature of Se-saturated ZnSe. The AFM images of doped ZnSe also show that possible Cr clusters are uniformly distributed and they have an estimated size of about 6 nm.
Rods of single crystal MgTaO 9 were produced free of macroscopic defects and their scintillation properties including afterglow were measured. The compound characteristics make it a candidate for high energy X-ray radiography applications.
This paper focuses on the research and development of high-purity germanium (HPGe) crystals for detector fabrication, specifically targeting applications in rare-event physics searches. The primary objective was to produce large-scale germanium crystals weighing >1 kg with a controlled diameter of ∼10 cm and an impurity range of approximately 1010/cm 3. Ensuring structural integrity and excellent crystalline quality requires a thorough assessment of dislocation density, a critical aspect of the crystal development process. Dislocation density measurements play a crucial role in maximizing the sensitivity of HPGe detectors, and our findings confirmed that the dislocation density fell within acceptable ranges for detector fabrication. Additionally, this paper examines the segregation coefficient of various contaminants during the crystal development process. Comprehensive analysis of impurity segregation is essential for reducing contaminant quantities in the crystal lattice and customizing purification processes. This, in turn, minimizes undesired background noise, enhancing signal-to-noise ratios for rare-event physics searches and overall detector performance. The investigation included the segregation coefficients of three major acceptors and one donor in crystals grown at the University of South Dakota, providing valuable insights for optimizing crystal purity and detector efficiency.
The positive effects of microgravity on crystal quality and fundamental properties of the vapor transport reaction were established by analyzing the results of three transport experiments on multi-component systems performed during the Apollo Soyuz Test Project (ASTP) mission. The systems employed were GeSe(0.99)Te(0.01) - GeI4 (A), GeS(0.98)Se(0.02) - GeCl4 (B), and GeS - GeCl4-Ar (C). The crystallographic analysis is based on a direct comparison of space and ground-based (prototype) crystals, employing X-ray diffraction, microprobe, microscopic, and chemical etching techniques. The results demonstrate a considerable improvement of the space-grown crystals in terms of chemical and crystalline homogeneity, surface morphology, and bulk perfection relative to ground specimens. The confirmation of greater mass transport rates than predicted for micro-gravity by present vapor transport models is of basic scientific and practical importance for the improvement of transport models and techniques on earth and for the development of a transport model for space conditions. The internal consistency and agreement between ASTP and Skylab results obtained for different compounds, transport agents, and temperature gradients strongly support the validity of these observations. The combined findings of improved crystal quality and high mass transport rates are of technological significance for space-processing applications.
Research Focus Area: Power Electronics, Temperature Tolerant Devices. Demonstrate initial feasibility of totally new "Large Tapered Crystal" (LTC) process for growing vastly improved large-diameter wide-band gap wafers. Addresses Targets: The goal of this research is to experimentally investigate and demonstrate feasibility of the key unproven LTC growth processes in SiC. Laser-assisted growth of long SiC fiber seeds. Radial epitaxial growth enlargement of seeds into large SiC boules. Uniqueness and Impacts open a new technology path to large-diameter SiC and GaN wafers with 1000-fold defect density improvement at 2-4 fold lower cost. Leapfrog improvement in wide band gap power device capability and cost.
Most of optical and semiconductor single crystalline materials produced in the electronic industry is grown with the Czochralski technique. This is the only technique capable of producing large high quality single crystals in a reasonable amount of time. The technique originated, and took its name, from pioneering work by Polish engineer J. Czochralski in 1917, who pulled single crystal wires (fibers) of low melting point metals from the melt in order to determine the maximum speeds at which they could be crystallized. The technique has been modified and its application has been extended first to the growth of silicon and later to a very wide range of compound semiconductors, metals, oxides and halides. It is now the dominant technique for the wide range of materials in the electronic industries. Czochralski growth is initiated by dipping a seed crystal of a chosen crystallographic orientation onto the surface of a melt contained in the heated crucible. The seed is then slowly withdrawn, solidifying the adherent column of the melt in steady state at an average rate given by the sum of the pulling rate and the rate of lowering the solid-liquid interface due to the depletion of the melt in the crucible. The control of the desired crystal diameter is achieved by closely controlling the heat balance at the solid-liquid interface.
The objective of the project is to determine the relative contributions of gravity-driven fluid flows to the compositional distribution, incorporation of impurities and defects, and deviation from stoichiometry observed in the crystals grown by vapor transport as results of buoyance-driven convection and growth interface fluctuations caused by irregular fluid-flows. ZnSe and related ternary compounds, such as ZnSeS and ZnSeTe, were grown by vapor transport technique with real time in-situ non-invasive monitoring techniques. The grown crystals were characterized extensively to correlate the grown crystal properties with the growth conditions.
A method and apparatus are disclosed for growing in a gravitational field a microscopic crystal from a solution. The solution is held in a vertical chamber which is relatively thin, the thin being generally perpendicular to the vertical. There is a substrate crystal disposed at either the upper or lower end of the chamber and the crystal grows from this substrate crystal in one direction. The temperature conditions of the solution are controlled so that, as the crystal forms, the effects of buoyant convection within the solution are minimized. This is accomplished in two different ways depending upon whether the crystal is grown from the upper or lower end of the chamber. When grown from the upper end of the chamber, the temperature of the solution is controlled so that it remains essentially isothermal so that there is essentially no heat loss from the solution. When the crystal is grown from the lower end of the chamber, the temperature of the solution is controlled so that there is a differential in temperature throughout the solution which provides a positive thermal gradient within the chamber.