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Total immersion crystal growth
Crystals of wide band gap materials are produced by positioning a holder receiving a seed crystal at the interface between a body of molten wide band gap material and an overlying layer of temperature-controlled, encapsulating liquid. The temperature of the layer decreases from the crystallization temperature of the crystal at the interface with the melt to a substantially lower temperature at which formation of crystal defects does not occur, suitably a temperature of 200 to 600 C. After initiation of crystal growth, the leading edge of the crystal is pulled through the layer until the leading edge of the crystal enters the ambient gas headspace which may also be temperature controlled. The length of the column of liquid encapsulant may exceed the length of the crystal such that the leading edge and trailing edge of the crystal are both simultaneously with the column of the crystal. The crystal can be pulled vertically by means of a pulling-rotation assembly or horizontally by means of a low-angle withdrawal mechanism.
Salt-induced aggregation of lysozyme: Implications for crystal growth
Crystallization of proteins is a prerequisite for structural analysis by x-ray crystallography. While improvements in protein crystals have been obtained in microgravity onboard the U.S. Space Shuttle, attempts to improve the crystal growth process both on the ground and in space have been limited by our lack of understanding of the mechanisms involved. Almost all proteins are crystallized with the aid of a precipitating agent. Many of the common precipitating agents are inorganic salts. An understanding of the role of salts on the aggregation of protein monomers is the key to the elucidation of the mechanisms involved in protein crystallization. In order for crystallization to occur individual molecules must self-associate into aggregates. Detection and characterization of aggregates in supersaturated protein solutions is the first step in understanding salt-induced crystallization.
High-purity silicon crystal growth
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.
Interaction between Convection and Heat Transfer in Crystal Growth
Crystals are integral components in some of our most sophisticated and rapidly developing industries. Single crystals are solids with the most uniform structures that can be obtained on an atomic scale. Because of their structural uniformity, crystals can transmit acoustic and electromagnetic waves and charged particles with essentially no scattering or interferences. This transparency, which can be selectively modified by controlled additions of impurities known as dopants, is the foundation of modern electronic industry. It has brought about widespread application of crystals in transistors, lasers, microwave devices, infrared detectors, magnetic memory devices, and many other magnets and electro-optic components. The performance of a crystal depends strongly on its compositional homogeneity. For instance, in modern microcircuitry, compositional variations of a few percent (down to a submicron length scale) can seriously jeopardize predicted yields. Since crystals are grown by carefully controlled phase transformations, the compositional adjustment in the solid is often made during growth from the nutrient. Hence, a detailed understanding of mass transfer in the nutrient is essential. Moreover, since mass transfer is often the slowest process during growth, it is usually the rate limiting mechanism. Crystal growth processes are usually classified according to the nature of the parent phase. Nevertheless, whether the growth occurs by solidification from a melt (melt growth), nucleation from a solution (solution growth), condensation from a vapor (physical vapor transport) or chemical reaction of gases (chemical vapor deposition), the parent phase is a fluid. As is with most non-equilibrium processes involving fluids, liquid or vapor, fluid motion plays an important role, affecting both the concentration and temperature gradients at the soli-liquid interface.
Unravelling crystal growth of nanoparticles
Crystal growth from nanoscale constituents is a ubiquitous phenomenon in biology, geology and materials science. Numerous studies have focused on understanding the onset of nucleation and on producing high-quality crystals by empirically sampling constituents with different attributes and varying the growth conditions. However, the kinetics of post-nucleation growth processes, an important determinant of crystal morphology and properties, have remained underexplored due to experimental challenges associated with real-space imaging at the nanoscale. Here we report the imaging of the crystal growth of nanoparticles of different shapes using liquid-phase transmission electron microscopy, resolving both lateral and perpendicular growth of crystal layers by tracking individual nanoparticles. We observe that these nanoscale systems exhibit layer-by-layer growth, typical of atomic crystallization, as well as rough growth prevalent in colloidal systems. Surprisingly, the lateral and perpendicular growth modes can be independently controlled, resulting in two mixed crystallization modes that, until now, have received only scant attention. Combining analytical considerations with molecular dynamics and kinetic Monte Carlo simulations, we develop a comprehensive framework for our observations, which are fundamentally determined by the size and shape of the building blocks. Furthermore, these insights unify the understanding of crystal growth across four orders of magnitude in particle size and suggest novel pathways to crystal engineering.
Trends in rare earth thiophosphate syntheses: Rb 3 Ln(PS 4 ) 2 (Ln = La, Ce, Pr), Rb 3−x Na x Ln(PS 4 ) 2 (Ln = Ce, Pr; x = 0.50, 0.55), and RbEuPS 4 obtained by molten flux crystal growth
Crystal structures of new rubidium rare earth thiophosphates with the formulas Rb 3 Ln(PS 4 ) 2 (Ln = La, Ce, Pr), Rb 3−x Na x Ln(PS 4 ) 2 (Ln = Ce, Pr; x = 0.50, 0.55), and RbEuPS 4 crystallized out of a molten RbCl flux.
Flux crystal growth: a versatile technique to reveal the crystal chemistry of complex uranium oxides
Molten flux crystal growth is a thriving field for the discovery of uranium oxides.
Crystal Growth for Beginners. Fundamentals of Nucleation, Crystal Growth and Epitaxy , 3rd edition . Edited by Ivan V Markov. World Scientific, 2017. Pp. 632. Hardback. Price GBP 123.00. ISBN 978-981-3143-42-5
Crystal growth is a classical discipline lying at the interfaces of Physics, Chemistry, Materials Science and Medicine. The research field has enjoyed an increasing number of young investigators over the past couple of decades, largely due to the burgeoning fields of nanoscience and nanotechnology which aim to fabricate nano-devices and/or to deliver nano-medicines in a process that mimics the exquisite wisdom of biologically controlled crystals. The interdisciplinary nature of these fields has posed a request for introductory monographs on the fundamental concepts of crystallization that are suitable for the diverse scientific backgrounds of researchers new to the field. Among many of the introductory crystal growth books, the Crystal Growth for Beginners (3rd edition) by Ivan Markov is an excellent one that can serve the purpose and is worth reading.
Optical diagnostics of solution crystal growth
Solution crystal growth monitoring of LAP/TGS crystals by various optical diagnostics systems, such as conventional and Mach-Zehnder (M-Z) interferometers, optical heterodyne technique, and ellipsometry, is under development. The study of the dynamics of the crystal growth process requires a detailed knowledge of crystal growth rate and the concentration gradient near growing crystals in aqueous solution. Crystal growth rate can be measured using conventional interferometry. Laser beam reflections from the crystal front as well as the back surface interfere with each other, and the fringe shift due to the growing crystal yields information about the growth rate. Our preliminary results indicate a growth rate of 6 A/sec for LAP crystals grown from solution. Single wavelength M-Z interferometry is in use to calculate the concentration gradient near the crystal. Preliminary investigation is in progress using an M-Z interferometer with 2 cm beam diameter to cover the front region of the growing crystal. In the optical heterodyne technique, phase difference between two rf signals (250 KHZ) is measured of which one is a reference signal, and the other growth signal, whose phase changes due to a change in path length as the material grows. From the phase difference the growth rate can also be calculated. Our preliminary results indicate a growth rate of 1.5 A/sec. the seed and solution temperatures were 26.46 C and 27.92 C respectively, and the solution was saturated at 29.0 C. an ellipsometer to measure the growth rate and interface layer is on order from JOBIN YVON, France. All these systems are arranged in such a manner that measurements can be made either sequentially or simultaneously. These techniques will be adapted for flight experiment.
Crystal Growth, Single Crystal Structure, and Biological Activity of Thiazolo-Pyridine Dicarboxylic Acid Derivatives
Four novel TPDCA derivatives were prepared via a supersaturation method combining TPDCA with water, N-methyl-2-pyrrolidone (NMP), Na(PO 2 H 2 ), and ammonia solution: 2(C 9 H 7 NO 5 S)H 2 O (1), (C 9 H 7 NO 5 S)C 5 H 9 NO (2), (C 9 H 7 NO 5 S)Na(PO 2 H 2 ) (3), and (C 9 H 5 NO 5 S)(NH 4 )2(H 2 O) (4). Their crystal structures were determined by single-crystal X-ray diffraction. Compounds (1) and (2) crystallize in the monoclinic space groups P2 1 and P2 1 /c, respectively, whereas compounds (3) and (4) crystallize in the triclinic space group P1 - . Weak and moderate hydrogen bonds were detected in the four compounds. In the biological tests, (1) and (3) exhibited significant antibacterial activity against Escherichia coli and Staphylococcus aureus; in addition, (1) was cytotoxic against leukemia HL-60 cells with the IC 50 value of 158.5 ± 12.5 μM.
Size and Morphology Controlled Synthesis of Boehmite Nanoplates and Crystal Growth Mechanisms
The aluminum oxyhydroxide boehmite is an important crystalline phase in nature and industry. We report development of a flexible additive-free hydrothermal synthesis method to prepare high quality boehmite nanoplates with sizes ranging from under 20 nm to 5 um via using hydrated alumina gels and amorphous powders as precursors. The size and morphology of the boehmite nanoplates was systematically varied between hexagonal and rhombic by adjusting precursor concentrations, pH, and the synthesis temperature, due to face-specific effects. The transformation mechanism is consistent with dissolution and reprecipitation, and involves transitory initial appearance of metastable gibbsite that is later consumed upon nucleation of boehmite. Detailed X-ray pair distribution characterization of the solids over time showed similarities in short-range order that suggest linkages in local chemistry and bonding topology between the precursors and product boehmite, yet also that precursor-specific differences in long-range order appear to manifest subtle changes in resulting boehmite characteristics, suggesting that the rate and extent of water release or differences in the resulting solubilized aluminate speciation leads to slightly different polymerization and condensation pathways. The findings suggest that during dissolution of the precursor that precursor-specific dehydration or solution speciation could be important aspects of the transformation impacting the molecular level details of boehmite nucleation and growth.
In-Situ Crystallization of a Lithium Disilicate Glass--Effect of Pressure on Crystal Growth Rate
Crystallization of a Li2O.2SiO2 (LS2) glass subjected to a uniform hydrostatic pressure of 4.5 GPa and 6 GPa was investigated up to a temperature of 750 C. The density of the compressed glass is about 2% greater at 4.5 GPa than at 1 atm and, depending upon the processing temperature, up to 10% greater at 6 GPa. Crystal growth rates investigated as a function of temperature and pressure show that lithium disilicate crystal growth is an order of magnitude slower at 4.5 GPa than 1 atm resulting in a shift of +45 C (plus or minus 10 C) in the growth rate curve at high pressure compared to 1 atm condition. At 6 GPa lithium disilicate crystallization is suppressed entirely, while a new high pressure lithium metasilicate crystallizes at temperatures 95 C (plus or minus 10 C) higher than those reported for lithium disilicate crystallization at 1 atm. The decrease in crystal growth rate with increasing pressure for lithium disilicate glass up to 750 C is related to an increase in viscosity with pressure associated with fundamental changes in glass structure accommodating densification.
Kinetic Roughening and Energetics of Tetragonal Lysozyme Crystal Growth
Lysozyme crystal growth rates over 5 orders of magnitude in range can be described using a layer-by-layer model where growth occurs by 2D nucleation on the crystal surface. Based upon the 2D nucleation model of layer growth, the effective barrier for growth was determined to be gamma = 1.3 plus or minus 0.3 x 10(exp -13) erg/molecule, corresponding to a barrier of 3.2 plus or minus 0.7 k(sub B)T, at 22 C. For solution supersaturation, In c/c(sub eq) greater than or equal to 1.9 plus or minus 0.2, the nucleation model would not predict or consistently estimate the highest observable crystal growth rates. As such, a kinetic roughening hypothesis where crystal growth occurs by a continuous mode was implemented for all growth rate data obtained above In c(sub r)/c(sub eq) greater than or equal to 2. That is, independent of the solution conditions that vary with either buffer pH, temperature or precipitant concentration, crystal growth occurs by the continuous addition of molecules anywhere on the crystal surface, above a roughening solution supersaturation. The energy barrier, E(sub c), for the continuous growth process is determined as 6.1 plus or minus 0.4 x 10(exp -13) erg/molecule or 15 plus or minus 1 k(sub B)T at 22 C.
Growth of spherical crystals of indium with respect to crystal growth in space
Spherical indium crystal manufacture in space, suspending and positioning weightless containerless melt in air and vacuum by adhesion and cohesion for crystal growth
The impact of space research on semiconductor crystal growth technology
Crystal growth experiments in reduced gravity environment and related ground-based research have contributed significantly to the establishment of a scientific basis for semiconductor growth from the melt. NASA-sponsored research has been instrumental in the introduction of heat pipes for heat and mass transfer control in crystal growth and in the development of magnetic field induced melt stabilization, approaches primarily responsible for recent advances in crystal growth technology.
High pO(2) Floating Zone Crystal Growth of the Perovskite Nickelate PrNiO3
Single crystals of PrNiO3 were grown under an oxygen pressure of 295 bar using a unique high-pressure optical-image floating zone furnace. The crystals, with volume in excess of 1 mm(3), were characterized structurally using single crystal and powder X-ray di ff raction. Resistivity, specific heat, and magnetic susceptibility were measured, all of which evidenced an abrupt, first order metal-insulator transition (MIT) at similar to 130 K, in agreement with previous literature reports on polycrystalline specimens. Temperature-dependent single crystal di ff raction was performed to investigate changes through the MIT. Our study demonstrates the opportunity space for high fugacity, reactive environments for single crystal growth specifically of perovskite nickelates but more generally to correlated electron oxides.