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The use of energy stability theory to study problems in crystal growth is outlined and justified in terms of convection mechanisms. An application to the float zone process of crystal growth is given as an illustration.
Direct observation of solid-liquid interface is important for the directional solidification to determine the desired interface shape by controlling the growth parameters. To grow good quality single crystals of novel organic nonlinear optical materials, a simple inexpensive Bridgman-Stockbarger (BS) crystal growth system has been designed and fabricated. Two immiscible liquids have been utilized to create two zones for this crystal growth system. Bulk single crystals of benzil derivative and n-salicylidene-aniline have been successfully grown in this system. The optimum lowering rate has been found to be 0.1 mm/h for the flat interface. Results on the crystal growth and other parameters of the grown crystals are presented.
A silicon crystal growth experiment has been accomplished using the floating-zone technique under microgravity on a sounding rocket (TEXUS 36). Measurements of temperature fluctuations in the silicon melt zone due to time dependent thermocapillary convection (Marangoni convection) and an observation of the microscopic growth rate were simultaneously performed during the experiment. Temperature fluctuations of about 0.5 - 0.7 C with a frequency range < 0.5Hz were detectable. The microscopic growth rate fluctuates considerably around the average growth rate of 1 mm/min: Growth rates up to 3 to 4mm/min, close to zero mm/min, as well as negative values (backmelting) were observed. Dopant striations are clearly visible in the Sb-doped crystal. They were characterized by Spreading Resistance measurements and Differential Interference Contrast microscopy. The frequencies of temperature fluctuations, microscopic growth rates, and the dopant inhomogeneities correspond quite well, with main frequencies between 0.1 and 0.3 Hz. 3D numerical simulations were performed to predict the optimum position of the temperature sensor, and the characteristic temperature amplitudes and frequencies. At a position 3.4mm above the interface and 1.4mm inside the melt, equivalent to the sensor tip position in the experiment, temperature fluctuations up to 1.8 C and frequencies ? 0.25Hz were found in the simulations.
Several pg experiments on sounding rockets and the Space Shuttle have shown that time-dependent thermocapillary (Marangoni) convection is the major cause for the formation of dopant striations in floating-zone grown semiconductor crystals, at least in small-scale systems not employing RF heating. To quantify this correlation, a silicon floating-zone experiment was performed during the TEXUS36 flight (February 7, 1 998) in the monoellipsoid mirror furnace TEM02-ELLI. During the experiment, temperature fluctuations in the silicon melt zone and the microscopic growth rate were simultaneously measured. Temperature fluctuations of 0.5 C - 0.7 C with main frequencies between 0.1 Hz and 0.3Hz were detectable. The microscopic growth rate fluctuated considerably around the average growth rate of 1 mm/min: rates from 4mm/min to negative values (backmelting) were observed. Dopant striations are clearly visible in the Sb-doped crystal. They were characterized by Spreading Resistance measurements and Differential Interference Contrast microscopy. The frequencies associated with the dopant inhomogeneities correspond quite well with those of the temperature fluctuations and microscopic growth rates. 3D numerical simulations were performed to predict the optimum position of the temperature sensor, to evaluate characteristic temperature amplitudes and frequencies, and to give insight into the instability mechanisms of Marangoni convection in this configuration. The simulations were in good agreement with the experimental values, showing temperature fluctuations with frequencies? 0.25 Hz and amplitudes up to 1.8 C at a position equivalent to that of the sensor tip in the experiment.
Several earlier (micro)g experiments have shown that time-dependent thermocapillary (Marangoni) convection is the major cause for the formation of dopant striations in floating-zone grown semiconductor crystals, at least in small-scale systems not employing RF heating. To quantify this correlation, a silicon floating-zone experiment was performed on the TEXUS36 flight (February 7, 1 998) in the monoellipsoid mirror furnace TEM02-ELLI. During the experiment, temperature fluctuations in the silicon melt zone and the microscopic growth rate were simultaneously measured. Temperature fluctuations of 0.5 C - 0.7 C with main frequencies between 0.1 Hz and 0.3 Hz were detectable. The microscopic growth rate fluctuated considerably around the average growth rate of 1 mm/min: rates from 4mm/min to negative values (backmelting) were observed. Dopant striations are clearly visible in the Sb-doped crystal. The frequencies associated with the dopant inhomogeneities correspond quite well with those of the temperature fluctuations and microscopic growth rates. 3D numerical simulations were performed to predict the optimum position of the temperature sensor, to evaluate characteristic temperature amplitudes and frequencies, and to give insight into the instability mechanisms of Maran-goni convection in this configuration. The simulations were in good agreement with the experimental values, showing temperature fluctuations with frequencies f? 0.25 Hz and amplitudes up to 1.8 C at a position equivalent to that of the sensor tip in the experiment.
USA Several microgravity experiments on sounding rockets and the Space Shuttle have shown that time-dependent thermocapillary (Marangoni) convection is the major cause for the formation of dopant striations in floating-zone grown semiconductor crystals, at least in small-scale systems not employing RF heating. To quantify this correlation, a silicon floating-zone experiment was performed during the TEXUS36 flight (February 7, 1998) in the monoellipsoid mirror furnace TEM02-ELLI. During the experiment, temperature fluctuations in the silicon melt zone and the microscopic growth rate were simultaneously measured. Temperature fluctuations of 0.5 C - 0.7 C with main frequencies between 0.1 Hz and 0.3 Hz were detectable. The microscopic growth rate fluctuated considerably around the average growth rate of 1 mm/min: rates from 4 mm/min to negative values (backmelting) were observed. Dopant striations are clearly visible in the Sb-doped crystal. They were characterized by Spreading Resistance measurements and Differential Interference Contrast microscopy. The frequencies associated with the dopant inhomogeneities correspond quite well with those of the temperature fluctuations and microscopic growth rates. 3D numerical simulations were performed to predict the optimum position of the temperature sensor, to evaluate characteristic temperature amplitudes and frequencies, and to give insight into the instability mechanisms of Marangoni convection in this configuration. The simulations were in good agreement with the experimental values, showing temperature fluctuations with frequencies ? 0.25 Hz and amplitudes up to 1.8 C at a position equivalent to that of the sensor tip in the experiment.
The molecular structure of biological macromolecules is important in understanding how these molecules work and has direct application to rational drug design for new medicines and for the improvement and development of industrial enzymes. In order to obtain the molecular structure, large, well formed, single macromolecule crystals are required. The growth of macromolecule crystals is a difficult task and is often hampered on the ground by fluid flows that result from the interaction of gravity with the crystal growth process. One such effect is the bulk movement of the crystal through the fluid due to sedimentation. A second is buoyancy driven convection close to the crystal surface. On the ground the crystallization process itself induces both of these flows. Buoyancy driven convection results from density differences between the bulk solution and fluid close to the crystal surface which has been depleted of macromolecules due to crystal growth. Schlieren photograph of a growing lysozyme crystal illustrating a 'growth plume' resulting from buoyancy driven convection. Both sedimentation and buoyancy driven convection have a negative effect on crystal growth and microgravity is seen as a way to both greatly reduce sedimentation and provide greater stability for 'depletion zones' around growing crystals. Some current crystal growth hardware however such as those based on a vapor diffusion techniques, may also be introducing unwanted Marangoni convection which becomes more pronounced in microgravity. Negative effects of g-jitter on crystal growth have also been observed. To study the magnitude of fluid flows around growing crystals we have attached a number of different fluorescent probes to lysozyme molecules. At low concentrations, less than 40% of the total protein, the probes do not appear to effect the crystal growth process. By using these probes we expect to determine not only the effect of induced flows due to crystal growth hardware design but also hope to optimize crystallization hardware so that destructive flows are minimized both on the ground and in microgravity.
Crystal growth parameter effects on minority carrier lifetime and solar cell efficiencies were investigated using high purity techniques such as float zoning. Study objectives include the following: (1) optimize dopants and minority carrier lifetime in FZ material for high efficiency silicon solar cell applications; (2) improve the understanding of lifetime degradation mechanisms (point defects, impurities, thermal history, surface effects, etc.), and (3) crystallographic defect characterization of float zone and ribbon crystals via X-ray topography.
Additive processing is proven to be an effective method to improve the efficiency and stability of perovskite solar cells; however, its intrinsic role in directing the crystallization pathway and thus morphology formation remains unknown. In situ grazing-incidence wide-angle x-ray scattering (GIWAXS) is applied to study the function of a 1,8-diiodooctane (DIO) additive in manipulating the crystallization behavior of perovskite thin films. It is seen that the DIO additive could induce multi-stage intermediate crystallization phases and increases the activation energy for nucleation and growth, which postpones the perovskite phase transformation time and broadens the transition zone. The elongated crystallization process affords improved perovskite thin film crystallinity and reduces defect density, which enables a longer carrier diffusion length. As a result, improved device efficiency, moisture, and thermal stability can be achieved. The following study provides a new prospective in understanding the additive function in perovskite thin film morphology control from fundamental parameters, indicating the importance of minor processing conditions in global property management toward high device performance.
Transparent sphere of polymethylmethacrylate with major zones and poles of cubic crystals is used to make crystallographic visualizations and to interpret Laue X ray diffraction of single cubic crystals.
"Melt recharger" adds raw silicon to crucible in crystal-growing furnace without disturbing inert-gas atmosphere or significantly lowering temperature of melt. Crucible-refill hopper is lowered into hot zone of crystal-pulling chamber through an isolation valve. Cable that supports hopper is fastened to cone-shaped stopper in bottom of hopper. Stopper moves out of opening in hopper, allowing part of polysilicon charge to drop into crucible.
High purity molybdenum disilicide crystals are prepared by zone melting sintered compacts. This method yields single crystals or polycrystals free from macrocracks which allow better measurement and evaluation of mechanical properties.
Copper indium disulfide (CuInS2) is a semiconductor with a direct energy band gap of 1.53 eV, an optimal value for highly efficient thin-film solar cells. But it has reached only ~ 11 % power conversion efficiency, far less than the theoretically achievable value of ~ 30 %. The cause of this low performance is not understood. A single crystal grown from 1 mol% Cu-deficient melt was studied, using atomic resolution high-angle annular dark-field (HAADF) scanning transmission electron microscopy (STEM) and electron dispersive spectroscopy (EDS). While the bulk crystal is exactly stoichiometric CuInS2, it contains nanometer-thick, structurally coherent, Cu-deficient interphases that form along rotational twin boundaries in the {112} plane. Transition zones from bulk crystal to interphase are observed, where In is seen to move from its normal site InIn in the chalcopyrite structure to a tetrahedral interstitial site Ini, while Cu remains in its normal CuCu position. Two InIn rows of the bulk crystal merge into one row of Ini, causing excess Ini in the interphase. The concentrations of CuCu and Ini reflect a ratio of Cu vacancies, VCu, to excess Ini of ~ 2. Their relative lattice positions, and the high electrical resistivity of the crystal, suggests that VCu and excess Ini ‘precipitate’ as self-compensating, electrically neutral, [VCu1- Ini2+ VCu1-] defect triplets. This is the first atomic-level observation of the ordered defect that has been invoked as the basic structural modifier in chalcopyrite compound homologs. The interphases introduce an optical gap of 1.47 eV. Electron trapping in band tail states, evident from a photoconductivity exponent of 0.54, is the likely cause of an unusually low electron mobility of 0.1 cm2V-1s-1. The overall result is that making CuInS2 slightly copper-poor inserts nanometer-thick layers of the interphase into the bulk crystal. This study shows that apparently conflicting results of the effect of Cu deficiency on CuInS2 thin-film solar cells may be resolved by analyzing structure and composition at nanometer spatial resolution.
This work under the rubrique of Antiferromagnetism and Superconductivity covers significant aspects of the most important and highest quality of superconductors in the class of quantum materials and the influence of magnetism on the superconducting state. These compounds include high temperature superconductors, pnictide iron-based superconductors, and topological superconductors. Special note is given that crystal growth of uranium based superconductors was performed with equipment created at Northwestern University for this purpose using novel ultra-high vacuum, electron-beam, float zone refining and crystal growth, producing the best quality of bulk single crystals of UPt3 in the literature with RRR=1546.
Many of Type B Allende inclusions are found to have reverse zoning over restricted portions of each crystal, in contrast to those in Type A's, which are reversely zoned throughout. Results of dynamic crystallization experiments on compositions similar to an average Type B inclusion are reported in which reversely zoned melilite rims were grown on normally zoned cores. The fact that these zoning patterns have been duplicated is interpreted as evidence that natural melilites having such zoning were formed by crystallization from a melt. Since reverse zoning could only be produced over a restricted range of experimental conditions, the presence in natural inclusions of the kinds of zoning patterns described here may place constraints on the conditions under which the inclusions formed.
A process for the purification of molten materials during crystal growth by electromigration of impurities to localized dirty zones. In the Czochralski crystal growing process, the impurities are electromigrated away from the crystallization interface by applying a direct electrical current to the molten silicon for electromigrating the charged impurities away from the crystal growth interface. The edge-defined film-fed crystal growth process, a direct electrical current is applied between the two faces which are used in forming the molten silicon into a ribbon. The impurities, migrated to one side only of the crystal ribbon, may be removed or left in place. If left in place, they will not adversely affect the ribbon when used in solar collectors. The migration of the impurity to one side only of the silicon ribbon is especially suitable for use with asymmetric dies which preferentially crystallize uncharged impurities along one side or face of the ribbon.
Fassaite rims around spinel grains that are enclosed entirely by normally zoned cores of melilite crystals are interpreted as relict grains which predate the melting of Allende type B1 refractory inclusions. Nonrelict subliquidus fassaite did not begin crystallizing from melts of these compositions until the onset of precipitation of the reversely zoned melilite mantles around the same melilite crystal cores. Relict fassaite is fractionated and highly enriched in REE and other refractory lithophiles compared to subliquidus fassaite in the same inclusion. Mass balance suggests that the relict fassaite represents only 3 percent of the original premelt amount of fassaite, and that melilite and at least one other phase were additional condensate precursors of these inclusions.
Research is aimed at the fundamental understanding of the interactions of heat and mass transport and fluid mechanics in crystal growth from the melt, especially in how it pertains to experiments supported by the Microgravity Science and Applications program. Emphasis has been on studies of the vertical Bridgman system, on small-scale floating zone systems proposed for space flight, and on quantitative prediction of nonlinear transitions in melt/solid interface morphologies leading to the formation of dendrites in directional solidification. The analysis of vertical Bridgman growth has lead to the complete numerical analysis of transport phenomena in directional solidification and to a detailed comparison of calculations to the GaGe growth experiments of Wang and Witt. Calculations show the central role of the ampoule material in determining the radial temperature gradients in the melt and thus, the intensity of convection. Results indicate that diffusion-controlled growth can not be achieved on Earth with conventional growth systems, but are feasible in microgravity