Silicon dendritic web growth

NASA Technical Reports Server (NTRS)

Duncan, S.

1984-01-01

Technological goals for a silicon dendritic web growth program effort are presented. Principle objectives for this program include: (1) grow long web crystals front continuously replenished melt; (2) develop temperature distribution in web and melt; (3) improve reproductibility of growth; (4) develop configurations for increased growth rates (width and speed); (5) develop new growth system components as required for improved growth; and (6) evaluate quality of web growth.

Effect of compression rate on ice VI crystal growth using dDAC

NASA Astrophysics Data System (ADS)

Lee, Yun-Hee; Kim, Yong-Jae; Lee, Sooheyong; Cho, Yong Chan; Lee, Geun Woo; Frontier in Extreme Physics Team

It is well known that static and dynamic pressure give different results in many aspects. Understanding of crystal growth under such different pressure condition is one of the crucial issues for the formation of materials in the earth and planets. To figure out the crystal growth under the different pressure condition, we should control compression rate from static to dynamic pressurization. Here, we use a dynamic diamond anvil cell (dDAC) technique to study the effect of compression rate of ice VI crystal growth. Using dDAC with high speed camera, we monitored growth of a single crystal ice VI. A rounded ice crystal with rough surface was selected in the phase boundary of water and ice VI and then, its repetitive growth and melting has been carried out by dynamic operation of the pressure cell. The roughened crystal showed interesting growth transition with compression rate from three dimensional to two dimensional growth as well as faceting process. We will discuss possible mechanism of the growth change by compression rate with diffusion mechanism of water. This research was supported by the Converging Research Center Program through the Ministry of Science, ICT and Future Planning, Korea (NRF-2014M1A7A1A01030128).

Containerless protein crystal growth method

NASA Technical Reports Server (NTRS)

Rhim, Won-Kyu; Chung, Sang K.

1991-01-01

A method of growing protein crystals from levitated drops is introduced and unique features of containerless approach in 1-g and micro-G laboratories are discussed. Electrostatic multidrop levitation system which is capable of simultaneous four drop levitation is described. A method of controlling protein saturation level in a programmed way is introduced and discussed. Finally, some of the unique features of containerless approach of protein crystal growth in space are discussed and summarized.

Crystal growth of device quality GaAs in space

NASA Technical Reports Server (NTRS)

Gatos, H. C.; Lagowski, J.

1983-01-01

GaAs device technology has recently reached a new phase of rapid advancement, made possible by the improvement of the quality of GaAs bulk crystals. At the same time, the transition to the next generation of GaAs integrated circuits and optoelectronic systems for commercial and government applications hinges on new quantum steps in three interrelated areas: crystal growth, device processing and device-related properties and phenomena. Special emphasis is placed on the establishment of quantitative relationships among crystal growth parameters-material properties-electronic properties and device applications. The overall program combines studies of crystal growth on novel approaches to engineering of semiconductor material (i.e., GaAs and related compounds); investigation and correlation of materials properties and electronic characteristics on a macro- and microscale; and investigation of electronic properties and phenomena controlling device applications and device performance.

The use of moments of momentum to account for crystal habits

NASA Technical Reports Server (NTRS)

Barber, P. G.

1985-01-01

A three-step theory of crystal growth is proposed which involves first an association of molecules or ions in solution to form an impinging growth unit, then second the orientation of this unit prior to its impact on the surface of a crystal, and finally the attachment of this unit to the crystal face. From this theory the habit of a crystal is dependent upon the moments of momentum of the impinging growth unit. The results of sample calculations are presented or sodium chloride, succinic acid, sucrose, and chromium boride. The faces predicted by this proposed theory are compared with those predicted by other, energy-based calculations and with those experimentally observed. The proposed theory suggests alternative strategies for crystallization and habit modification which may be of technological importance. Listings of the two computer programs that were used are provided.

Ribbon Growth of Single Crystal GaAs for Solar Cell Application.

DTIC Science & Technology

1981-11-01

Entered) 20. Abstract (Cont.) 7growth techniques, dendrite seeds, and melt chemistry were optimized during the course of the program; however...Faceted Web. 10 Crystal Grown From a Melt Doped With 1.0 Atomic% Ge. 17 The Ge-Doped Crystals Grew at Low Undercooling and Contained Flatter Textured-Web...Ge Melt Doping. The 18 Textured-Web Sections Were the Widest Achieved at Small Undercooling, ɝ.0°C. 12 Radiation Exchange Between the Melt Surface

Thin EFG octagons

NASA Astrophysics Data System (ADS)

Kalejs, J. P.

1994-01-01

Mobil Solar Energy Corporation currently practices a unique crystal growth technology for producing crystalline silicon sheet, which is then cut with lasers into wafers. The wafers are processed into solar cells and incorporated into modules for photovoltaic applications. The silicon sheet is produced using a method known as Edge-defined Film-fed growth (EFG), in the form of hollow eight-sided polygons (octagons) with 10 cm faces. These are grown to lengths of 5 meters and thickness of 300 microns, with continuous melt replenishment, in compact furnaces designed to operate at a high sheet area production area of 135 sq cm/min. The present Photovoltaic Manufacturing Technology (PVMaT) three-year program seeks to advance the manufacturing line capabilities of the Mobil Solar crystal growth and cutting technologies. If successful, these advancements will provide significant reductions in already low silicon raw material usage, improve process productivity, laser cutting throughput and yield, and so lower both individual wafer cost and the cost of module production. This report summarizes the significant technical improvements in EFG technology achieved in Phase 1 of this program. Technical results are reported for each of the three main program areas: (1) thin octagon growth (crystal growth) -- to reduce the thickness of the octagon to an interim goal of 250 microns during Phase 1, with an ultimate goal of achieving 200 micron thicknesses; (2) laser cutting -- to improve the laser cutting process, so as to produce wafers with decreased laser cutting damage at increased wafer throughput rates; and (3) process control and product specification -- to implement advanced strategies in crystal growth process control and productivity designed to increase wafer yields.

Crystal Growth Control

NASA Technical Reports Server (NTRS)

Duval, Walter M. B.; Batur, Celal; Bennett, Robert J.

1997-01-01

We present an innovative design of a vertical transparent multizone furnace which can operate in the temperature range of 25 C to 750 C and deliver thermal gradients of 2 C/cm to 45 C/cm for the commercial applications to crystal growth. The operation of the eight zone furnace is based on a self-tuning temperature control system with a DC power supply for optimal thermal stability. We show that the desired thermal profile over the entire length of the furnace consists of a functional combination of the fundamental thermal profiles for each individual zone obtained by setting the set-point temperature for that zone. The self-tuning system accounts for the zone to zone thermal interactions. The control system operates such that the thermal profile is maintained under thermal load, thus boundary conditions on crystal growth ampoules can be predetermined prior to crystal growth. Temperature profiles for the growth of crystals via directional solidification, vapor transport techniques, and multiple gradient applications are shown to be easily implemented. The unique feature of its transparency and ease of programming thermal profiles make the furnace useful for scientific and commercial applications for the determination of process parameters to optimize crystal growth conditions.

The Design of a Transparent Vertical Multizone Furnace: Application to Thermal Field Tuning and Crystal Growth

NASA Technical Reports Server (NTRS)

Duvual, Walter M. B.; Batur, Celal; Bennett, Robert J.

1998-01-01

We present an innovative design of a vertical transparent multizone furnace which can operate in the temperature range of 25 C to 750 C and deliver thermal gradients of 2 C/cm to 45 C/cm for the commercial applications to crystal growth. The operation of the eight zone furnace is based on a self-tuning temperature control system with a DC power supply for optimal thermal stability. We show that the desired thermal profile over the entire length of the furnace consists of a functional combination of the fundamental thermal profiles for each individual zone obtained by setting the set-point temperature for that zone. The self-tuning system accounts for the zone to zone thermal interactions. The control system operates such that the thermal profile is maintained under thermal load, thus boundary conditions on crystal growth ampoules can be predetermined prior to crystal growth. Temperature profiles for the growth of crystals via directional solidification, vapor transport techniques, and multiple gradient applications are shown to be easily implemented. The unique feature of its transparency and ease of programming thermal profiles make the furnace useful in scientific and commercial applications for determining the optimized process parameters for crystal growth.

Growth of Solid Solution Crystals

NASA Technical Reports Server (NTRS)

Lehoczky, S. L.; Szofran, F. R.; Holland, L. R.

1985-01-01

The major objective of this program is to determine the conditions under which single crystals of solid solutions can be grown from the melt in a Bridgman configuration with a high degree of chemical homogeneity. The central aim is to assess the role of gravity in the growth process and to explore the possible advantages for growth in the absence of gravity. The alloy system being investigated is the solid solution semiconductor with x-values appropriate for infrared detector applications in Hg sub (1-x) Cd sub x Te the 8 to 14 micro m wavelength region. Both melt and Te-solvent growth are being considered. The study consists of an extensive ground-based experimental and theoretical research effort followed by flight experimentation where appropriate. Experimental facilities have been established for the purification, casting, and crystal growth of the alloy system. Facilities have been also established for the metallurgical, compositional, electric and optical characterization of the alloys. Crystals are being grown by the Bridgman-Stockbarger method and are analyzed by various experimental techniques to evaluate the effects of growth conditions on the longitudinal and radial compositional variations and defect densities in the crystals.

Fluid mechanics and mass transfer in melt crystal growth: Analysis of the floating zone and vertical Bridgman processes

NASA Technical Reports Server (NTRS)

Brown, R. A.

1986-01-01

This research program focuses on analysis of the transport mechanisms in solidification processes, especially one of interest to the Microgravity Sciences and Applications Program of NASA. Research during the last year has focused on analysis of the dynamics of the floating zone process for growth of small-scale crystals, on studies of the effect of applied magnetic fields on convection and solute segregation in directional solidification, and on the dynamics of microscopic cell formation in two-dimensional solidification of binary alloys. Significant findings are given.

Ground Based Program for the Physical Analysis of Macromolecular Crystal Growth

NASA Technical Reports Server (NTRS)

Malkin, Alexander J.

1999-01-01

In a reported period in situ atomic force microscopy was utilized in our laboratory to study mechanisms of growth and kinetics of crystallization of ten protein and virus crystals. These included canavalin, thaumatin, apoferritin, lipase, catalase, t-RNA, lysozyme, xylanase, turnip yellow mosaic virus (TYMV) and satellite tobacco mosaic virus (STMV). We have also designed and constructed in our laboratory both in situ conventional two-beam Michelson and phase shift Mach-Zenhder interferometers. Computer software for the processing of the interferometric images was developed as well. Interferometric techniques were applied for studies of growth kinetics and transport phenomena in crystallization of several macromolecular crystals. As a result of this work we have published 21 papers and have given many presentations at international and national meetings. A list of these publications and conference presentations is attached.

Silicon ribbon study program. [dendritic crystals for use in solar cells

NASA Technical Reports Server (NTRS)

Seidensticker, R. G.; Duncan, C. S.

1975-01-01

The feasibility is studied of growing wide, thin silicon dendritic web for solar cell fabrication and conceptual designs are developed for the apparatus required. An analysis of the mechanisms of dendritic web growth indicated that there were no apparent fundamental limitations to the process. The analysis yielded quantitative guidelines for the thermal conditions required for this mode of crystal growth. Crucible designs were then investigated: the usual quartz crucible configurations and configurations in which silicon itself is used for the crucible. The quartz crucible design is feasible and is incorporated into a conceptual design for a laboratory scale crystal growth facility capable of semi-automated quasi-continuous operation.

Results of the TTF-TCNQ and the calcium carbonate crystallization on the Long Duration Exposure Facility

NASA Technical Reports Server (NTRS)

Nielsen, Kjeld Flemming; Lind, M. David

1992-01-01

Experiment A0139A on the Long Duration Exposure Facility (LDEF) carried four large containers into orbit five years with crystal growth solutions for lead sulfide, calcium carbonate, and TTF-TCNQ. Although temperature data was lost, the experimental program had been working since the valves in all containers had been opened. All four experiments produced crystals of varying quality. The calcium carbonate crystals had the best appearance. The TTF-TCNQ crystals were packed together near the valve openings of the container. When taken apart, the single crystals showed some unusual morphological properties. X ray investigations as well as conductivity measurements on long duration space grown TTF-TCNQ crystals will be presented. Comparisons will be made with our previous space solution growth experiments. The TTF-TCNQ crystals are no longer of the highest interest, so this activity has been terminated in favor of calcium carbonate and calcium phosphate crystallizations.

Ground Based Program for the Physical Analysis of Macromolecular Crystal Growth

NASA Technical Reports Server (NTRS)

Malkin, Alexander J.

1998-01-01

During the past year we have focused on application of in situ Atomic Force Microscopy (AFM) for studies of the growth mechanisms and kinetics of crystallization for different macromolecular systems. Mechanisms of macrostep formation and their decay, which are important in understanding of defect formation, were studied on the surfaces of thaumatin, catalase, canavalin and lysozyme crystals. Experiments revealed that step bunching on crystalline surfaces occurred either due to two- or three-dimensional nucleation on the terraces of vicinal slopes or as a result of uneven step generation by complex dislocation sources. No step bunching arising from interaction of individual steps in the course of the experiment was observed. The molecular structure of the growth steps for thaumatin and lipase crystals were deduced. It was further shown that growth step advance occurs by incorporation of single protein molecules. In singular directions growth steps move by one-dimensional nucleation on step edges followed by lateral growth. One-dimensional nuclei have different sizes, less then a single unit cell, varying for different directions of step movement. There is no roughness due to thermal fluctuations, and each protein molecule which incorporated into the step remained. Growth kinetics for catalase crystals was investigated over wide supersaturation ranges. Strong directional kinetic anisotropy in the tangential step growth rates in different directions was seen. The influence of impurities on growth kinetics and cessation of macromolecular crystals was studied. Thus, for catalase, in addition to pronounced impurity effects on the kinetics of crystallization, we were also able to directly observe adsorption of some impurities. At low supersaturation we repeatedly observed filaments which formed from impurity molecules sedimenting on the surfaces. Similar filaments were observed on the surfaces of thaumatin, canavalin and STMV crystals as well, but the frequency was low compared with catalase crystallization. Cessation of growth of xylanase and lysozyme crystals was also observed and appeared to be a consequence of the formation of dense impurity adsorption layers. Attachment: "An in situ AFM investigation of catalase crystallization", "Atomic force microscopy studies of living cells: visualization of motility, division, aggregation, transformation, and apoptosis", AFM studies on mechanisms of nucleation and growth of macromolecular crystals", and "In situ atomic force microscopy studies of surface morphology, growth kinetics, defect structure and dissolution in macromolecular crystallization".

Tuning the Growth Pattern in 2D Confinement Regime of Sm2O3 and the Emerging Room Temperature Unusual Superparamagnetism

PubMed Central

Guria, Amit K.; Dey, Koushik; Sarkar, Suresh; Patra, Biplab K.; Giri, Saurav; Pradhan, Narayan

2014-01-01

Programming the reaction chemistry for superseding the formation of Sm2O3 in a competitive process of formation and dissolution, the crystal growth patterns are varied and two different nanostructures of Sm2O3 in 2D confinement regime are designed. Among these, the regular and self-assembled square platelets nanostructures exhibit paramagnetic behavior analogous to the bulk Sm2O3. But, the other one, 2D flower like shaped nanostructure, formed by irregular crystal growth, shows superparamagnetism at room temperature which is unusual for bulk paramagnet. It has been noted that the variation in the crystal growth pattern is due to the difference in the binding ability of two organic ligands, oleylamine and oleic acid, used for the synthesis and the magnetic behavior of the nanostructures is related to the defects incorporated during the crystal growth. Herein, we inspect the formation chemistry and plausible origin of contrasting magnetism of these nanostructures of Sm2O3. PMID:25269458

Development of advanced Czochralski Growth Process to produce low cost 150 KG silicon ingots from a single crucible for technology readiness

NASA Technical Reports Server (NTRS)

1981-01-01

The goals in this program for advanced czochralski growth process to produce low cost 150 kg silicon ingots from a single crucible for technology readiness are outlined. To provide a modified CG2000 crystal power capable of pulling a minimum of five crystals, each of approximately 30 kg in weight, 150 mm diameter from a single crucible with periodic melt replenishment. Crystals to have: resistivity of 1 to 3 ohm cm, p-type; dislocation density below 1- to the 6th power per cm; orientation (100); after growth yield of greater than 90%. Growth throughput of greater than 2.5 kg per hour of machine operation using a radiation shield. Prototype equipment suitable for use as a production facility. The overall cost goal is $.70 per peak watt by 1986. To accomplish these goals, the modified CG2000 grower and development program includes: (1) increased automation with a microprocessor based control system; (2) sensors development which will increase the capability of the automatic controls system, and provide technology transfer of the developed systems.

Shuttle Mission STS-50: Orbital Processing of High-Quality CdTe Compound Semiconductors Experiment: Final Flight Sample Characterization Report

NASA Technical Reports Server (NTRS)

Larson, David J.; Casagrande, Luis G.; DiMarzio, Don; Alexander, J. Iwan D.; Carlson, Fred; Lee, Taipo; Dudley, Michael; Raghathamachar, Balaji

1998-01-01

The Orbital Processing of High-Quality Doped and Alloyed CdTe Compound Semiconductors program was initiated to investigate, quantitatively, the influences of gravitationally dependent phenomena on the growth and quality of bulk compound semiconductors. The objective was to improve crystal quality (both structural and compositional) and to better understand and control the variables within the crystal growth production process. The empirical effort entailed the development of a terrestrial (one-g) experiment baseline for quantitative comparison with microgravity (mu-g) results. This effort was supported by the development of high-fidelity process models of heat transfer, fluid flow and solute redistribution, and thermo-mechanical stress occurring in the furnace, safety cartridge, ampoule, and crystal throughout the melting, seeding, crystal growth, and post-solidification processing. In addition, the sensitivity of the orbital experiments was analyzed with respect to the residual microgravity (mu-g) environment, both steady state and g-jitter. CdZnTe crystals were grown in one-g and in mu-g. Crystals processed terrestrially were grown at the NASA Ground Control Experiments Laboratory (GCEL) and at Grumman Aerospace Corporation (now Northrop Grumman Corporation). Two mu-g crystals were grown in the Crystal Growth Furnace (CGF) during the First United States Microgravity Laboratory Mission (USML-1), STS-50, June 24 - July 9, 1992.

STS-30 MS Cleave uses camcorder to record FEA-2 crystal growth

NASA Image and Video Library

1989-05-08

STS030-10-002 (8 May 1989) --- STS-30 Mission Specialist Mary L. Cleave operates 8mm video camcorder at Fluids Experiment Apparatus 2 (FEA-2) (SK73-000102) unit located in aft middeck locker onboard Atlantis, Orbiter Vehicle (OV) 103. Two 8mm video camcorders are positioned above FEA-2 unit to record experiment titled "Floating Zone Crystal Growth and Purification". Rockwell International (RI) through its Space Transportation Systems Division, Downey, California, is engaged in a joint endeavor agreement (JEA) with NASA's Office of Commercial Programs in the field for floating zone crystal growth research. Utah State University Aggies decal appears on aft bulkhead above FEA-2 unit.

Electronics materials research

NASA Technical Reports Server (NTRS)

1982-01-01

The electronic materials and is aimed at the establishment of quantitative relationships underlying crystal growth parameters, materials properties, electronic characteristics and device applications. The overall program evolves about the following main thrust areas: (1) crystal growth novel approaches to engineering of semiconductor materials; (2) investigation of materials properties and electronic characteristics on a macro and microscale; (3) surface properties and surface interactions with the bulk and ambients; (4) electronic properties controlling device applications and device performance.

Growth and characterization of crystals for room temperature I.R. detectors and second harmonic generation devices

NASA Technical Reports Server (NTRS)

Lal, R. B.

1995-01-01

One of the major objectives of this program was to modify the triglycine sulfate (TGS) crystals with suitable dopants and variants to achieve better pyroelectric properties and improved infrared detectivities (D(sup *)), and higher Curie transition temperature compared to undoped TGS crystals. Towards these objectives, many promising dopants, both inorganic and organic, were investigated in the last few years. These dopants gave significant improvement in the D(sup *) value of the infrared detectors fabricated from the grown crystals with no significant increase in the Curie temperature (49 C). The IR detectors were fabricated at EDO/Barnes Engineering Division, Shelton, CT. In the last one year many TGS crystals doped with urea were grown using the low temperature solution crystal growth facility. It is found that doping with urea, the normalized growth yield increased significantly compared to pure TGS crystals and there is an improvement in the pyroelectric and dielectric constant values of doped crystals. This gave a significant increase in the materials figure of merits. The Vicker's hardness of 10 wt percent urea doped crystals is found to be about three times higher in the (010) direction compared to undoped crystals. This report describes in detail the results of urea doped TGS crystals.

Crystal Growth of Device Quality Gaas in Space

NASA Technical Reports Server (NTRS)

Gatos, H. C.

1985-01-01

The GaAs research evolves about these key thrust areas. The overall program combines: (1) studies of crystal growth on novel approaches to engineering of semiconductor material (i.e., GaAs and related compounds); (2) investigation and correlation of materials properties and electronic characteristics on a macro- and microscale; and (3) investigation of electronic properties and phenomena controlling device applications and device performance. This effort is aimed at the essential ground-based program which would insure successful experimentation with and eventually processing of GaAs in near zero gravity environment. It is believed that this program addresses in a unique way materials engineering aspects which bear directly on the future exploitation of the potential of GaAs and related materials in device and systems applications.

Modeling of thin-film GaAs growth

NASA Technical Reports Server (NTRS)

Heinbockel, J. H.

1981-01-01

Efforts to produce a Monte Carlo computer program for the analysis of crystal growth are briefly discussed. A literature survey was conducted of articles relating to the subject. A list of references reviewed is presented.

Growth of single crystals of organic salts with large second-order optical nonlinearities by solution processes for devices

NASA Technical Reports Server (NTRS)

Leslie, Thomas M.

1995-01-01

Data obtained from the electric field induced second harmonic generation (EFISH) and Kurtz Powder Methods will be provided to MSFC for further refinement of their method. A theoretical model for predicting the second-order nonlinearities of organic salts is being worked on. Another task is the synthesis of a number of salts with various counterions. Several salts with promising SHG activities and new salts will be tested for the presence of two crystalline forms. The materials will be recrystallized from dry and wet solvents and compared for SHG efficiency. Salts that have a high SHG efficiency and no tendency to form hydrates will be documented. The synthesis of these materials are included in this report. A third task involves method to aid in the growth of large, high quality single crystals by solution processes. These crystals will be characterized for their applicability in the fabrication of devices that will be incorporated into optical computers in future programs. Single crystals of optimum quality may be obtained by crystal growth in low-gravity. The final task is the design of a temperature lowering single crystal growth apparatus for ground based work. At least one prototype will be built.

Computer simulation of rapid crystal growth under microgravity

NASA Astrophysics Data System (ADS)

Hisada, Yasuhiro; Saito, Osami; Mitachi, Koshi; Nishinaga, Tatau

We are planning to grow a Ge single crystal under microgravity by the TR-IA rocket in 1992. The furnace temperature should be controlled so as to finish the crystal growth in a quite short time interval (about 6 min). This study deals with the computer simulation of rapid crystal growth in space to find the proper conditions for the experiment. The crystal growth process is influenced by various physical phenomena such as heat conduction, natural and Marangoni convections, phase change, and radiation from the furnace. In this study, a 2D simulation with axial symmetry is carried out, taking into account the radiation field with a specific temperature distribution of the furnace wall. The simulation program consists of four modules. The first module is applied for the calculation of the parabolic partial differential equation by using the control volume method. The second one evaluates implicitly the phase change by the enthalpy method. The third one is for computing the heat flux from surface by radiation. The last one is for calculating with the Monte Carlo method the view factors which are necessary to obtain the heat flux.

Thin EFG octagons

NASA Astrophysics Data System (ADS)

Kalejs, J. P.

1994-03-01

This report describes work to advance the manufacturing line capabilities in crystal growth and laser cutting of Mobil Solar's unique edge-defined film-fed growth (EFG) octagon technology and to reduce the manufacturing costs of 10 cm x 10 cm polycrystalline silicon EFG wafers. The report summarizes the significant technical improvements in EFG technology achieved in the first 6 months of the PVMaT Phase 2 and the success in meeting program milestones. Technical results are reported for each of the three main pregrain areas: Task 5 -- Thin octagon growth (crystal growth) to reduce the thickness of the octagon to 200 microns; Task 6 -- Laser cutting-to improve the laser cutting process so as to produce wafers with decreased laser cutting damage at increased wafer throughput rates; and Task 7 -- Process control and product specification to implement advanced strategies in crystal growth process control and productivity designed to increase wafer yields.

Growth Defects in Biomacromolecular Crystals

NASA Technical Reports Server (NTRS)

2003-01-01

NASA's ground based program confirmed close similarity between protein and small molecules crystal growth, but also revealed essential differences. No understanding exists as to why and when crystals grown in space are, in approx. 20 percent of cases, of higher quality. More rationale is needed in flight experiments. Ferritin crystals grown in space are 2.5 times cleaner than their terrestrial counterparts. This may occur because of the existence of a zone depleted with respect to impurities around a crystal growing in stagnant solution. This zone should appear since the distribution coefficient for homologous impurities exceeds unity. This impurity depletion zone hypothesis requires verification and development. Thorough purification from homologous impurities brought about resolution improvement from 2.6 to 1.8 angstroms for ferritin and from 2.6 to 2.0 angstroms for canavalin.

Biotechnology Science Experiments on Mir

NASA Technical Reports Server (NTRS)

Kroes, Roger L.

1999-01-01

This paper describes the microgravity biotechnology experiments carried out on the Shuttle/Mir program. Four experiments investigated the growth of protein crystals, and three investigated cellular growth. Many hundreds of protein samples were processed using four different techniques. The objective of these experiments was to determine optimum conditions for the growth of very high quality single crystals to be used for structure determination. The Biotechnology System (BTS) was used to process the three cell growth investigations. The samples processed by these experiments were: bovine chondrocytes, human renal epithelial cells, and human breast cancer cells and endothelial cells. The objective was to determine the unique properties of cell aggregates produced in the microgravity environment.

Nucleation and growth control in protein crystallization

NASA Technical Reports Server (NTRS)

Rosenberger, Franz; Nyce, Thomas A.; Meehan, Edward J.; Sowers, Jennifer W.; Monaco, Lisa A.

1990-01-01

The five topics summarized in this final report are as follows: (1) a technique for the expedient, semi-automated determination of protein solubilities as a function of temperature and application of this technique to proteins other than lysozyme; (2) a small solution cell with adjustable temperature gradients for the growth of proteins at a predetermined location through temperature programming; (3) a microscopy system with image storage and processing capability for high resolution optical studies of temperature controlled protein growth and etching kinetics; (4) growth experiments with lysozyme in thermosyphon flow ; and (5) a mathematical model for the evolution of evaporation/diffusion induced concentration gradients in the hanging drop protein crystallization technique.

Project Explorer takes its second step: GAS-608 in engineering development

NASA Technical Reports Server (NTRS)

Kitchens, Philip H.

1988-01-01

An a continuation of its Project Explorer series, the Alabama Space and Rocket Center is sponsoring the development of two additional Get Away Special payloads. Details are given of GAS-608, including descriptions of its six experiments in organic crystal growth, roach eggs, yeast, radish seeds, bacterial morphology, and silicon crystals. A brief summary is also presented of GAS-105 and the Space Camp program for stimulating student first hand participation in space flight studies. GAS-608 will carry six student experiments, which will involve biology, crystal growth, and biochemistry in addition to a centralized package for electronics and power supply.

The First United States Microgravity Laboratory

NASA Technical Reports Server (NTRS)

Powers, C. Blake (Editor); Shea, Charlotte; Mcmahan, Tracy; Accardi, Denise; Mikatarian, Jeff

1991-01-01

The United States Microgravity Laboratory (USML-1) is one part of a science and technology program that will open NASA's next great era of discovery and establish the United States' leadership in space. A key component in the preparation for this new age of exploration, the USML-1 will fly in orbit for extended periods, providing greater opportunities for research in materials science, fluid dynamics, biotechnology, and combustion science. The major components of the USML-1 are the Crystal Growth Furnace, the Surface Tension Driven Convection Experiment (STDCE) Apparatus, and the Drop Physics Module. Other components of USML-1 include Astroculture, Generic Bioprocessing Apparatus, Extended Duration Orbiter Medical Project, Protein Crystal Growth, Space Acceleration Measurement System, Solid Surface Combustion Experiment, Zeolite Crystal Growth and Spacelab Glovebox provided by the European Space Agency.

Results of the TTF-TCNQ- and the calcium carbonate-crystallization on the Long Duration Exposure Facility

NASA Technical Reports Server (NTRS)

Nielsen, Kjeld Flemming; Lind, M. David

1991-01-01

Experiment AO139A on the Long Duration Exposure Facility (LDEF) carried four large containers into orbit for five years with crystal growth solutions for lead sulfide, calcium carbonate, and tetra thiafulvalene- tetra cyanoquino methane (TTF-TCNQ). The LDEF was in excellent condition after the long orbital stay, and although the temperature data was lost, the experiment program had been working since the valves in all containers were opened. All four experiments produced crystals; however, they were of varying quality. The calcium carbonate crystals had the best appearance. The TTF-TCNQ crystals were packed together near the valve openings of the container. When taken apart, the single crystals showed some unusual morphological properties. X-ray investigations as well as conductivity measurements on the long duration space grown TTF-TCNQ crystals are presented, and pictures of the calcium carbonate are shown. Comparisons are made with previous space solution growth experiments on the European Spacelab Mission and the Apollo-Soyuz Test Project.

Crystal Growth Furnace System Configuration and Planned Experiments on the Second United States Microgravity Laboratory Mission

NASA Technical Reports Server (NTRS)

Srinivas, R.; Hambright, G.; Ainsworth, M.; Fiske, M.; Schaefer, D.

1995-01-01

The Crystal Growth Furnace (CGF) is currently undergoing modifications and refurbishment and is currently undergoing modifications and refurbishment and is manifested to refly on the Second United States Microgravity Laboratory (USML-2) mission scheduled for launch in September 1995. The CGF was developed for the National Aeronautics and Space Administration (NASA) under the Microgravity Science and Applications Division (MSAD) programs at NASA Headquarters. The refurbishment and reflight program is being managed by the Marshall Space Flight Center (MSFC) in Huntsville, Alabama. Funding and program support for the CGF project is provided to MSFC by the office of Life and Microgravity Sciences and Applications at NASA Headquarters. This paper presents an overview of the CGF system configuration for the USML-2 mission, and provides a brief description of the planned on-orbit experiment operation.

An inverse modeling strategy and a computer program to model garnet growth and resorption

NASA Astrophysics Data System (ADS)

Lanari, Pierre; Giuntoli, Francesco

2017-04-01

GrtMod is a computer program that allows numerical simulation of the pressure-temperature (P-T) evolution of garnet porphyroblasts based on the composition of successive growth zones preserved in natural samples. For each garnet growth stage, a new reactive bulk composition is optimized, allowing for resorption and/or fractionation of the previously crystalized garnet. The successive minimizations are performed using a heuristic search method and an objective function that quantify the amount by which the predicted garnet composition deviates from the measured values. The automated strategy of GrtMod includes a two stages optimization and one refinement stage. In this contribution, we will present several application examples. The new strategy provides quantitative estimates of the optimal P-T conditions whereas it was generally derived in a qualitatively way by using garnet isopleth intersections in equilibrium phase diagrams. GrtMod can also be used to model the evolution of the reactive bulk composition along any P-T trajectories. The results for typical MORB and metapelite compositions demonstrate that fractional crystallization models are required to derive accurate P-T information from garnet compositional zoning. GrtMod can also be used to retrieve complex garnet histories involving several stages of resorption. For instance, it has been used to model the P-T condition of garnet growth in grains from the Sesia Zone (Western Alps). The compositional variability of successive growth zones is characterized using standardized X-ray maps and the program XMapTools. Permian garnet cores crystalized under granulite facies conditions (T > 800°C and P = 6 kbar), whereas Alpine garnet rims grew at eclogite facies conditions (650°C and 16 kbar) involving several successive episodes of resorption. The model predicts that up to 50 vol% of garnet was dissolved before a new episode of garnet growth.

Advanced dendritic web growth development and development of single-crystal silicon dendritic ribbon and high-efficiency solar cell program

NASA Technical Reports Server (NTRS)

Duncan, C. S.; Seidensticker, R. G.; Mchugh, J. P.; Hopkins, R. H.

1986-01-01

Efforts to demonstrate that the dendritic web technology is ready for commercial use by the end of 1986 continues. A commercial readiness goal involves improvements to crystal growth furnace throughput to demonstrate an area growth rate of greater than 15 sq cm/min while simultaneously growing 10 meters or more of ribbon under conditions of continuous melt replenishment. Continuous means that the silicon melt is being replenished at the same rate that it is being consumed by ribbon growth so that the melt level remains constant. Efforts continue on computer thermal modeling required to define high speed, low stress, continuous growth configurations; the study of convective effects in the molten silicon and growth furnace cover gas; on furnace component modifications; on web quality assessments; and on experimental growth activities.

Convective flow effects on protein crystal growth

NASA Technical Reports Server (NTRS)

Rosenberger, Franz; Monaco, Lisa A.

1993-01-01

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.

Ground Based Experiments in Support of Microgravity Research Results-Vapor Growth of Organic Nonlinear Optical Thin Film

NASA Technical Reports Server (NTRS)

Zugrav, M. Ittu; Carswell, William E.; Haulenbeek, Glen B.; Wessling, Francis C.

2001-01-01

This work is specifically focused on explaining previous results obtained for the crystal growth of an organic material in a reduced gravity environment. On STS-59, in April 1994, two experiments were conducted with N,N-dimethyl-p-(2,2-dicyanovinyl) aniline (DCVA), a promising nonlinear optical (NLO) material. The space experiments were set to reproduce laboratory experiments that yielded small, bulk crystals of DCVA. The results of the flight experiment, however, were surprising. Rather than producing a bulk single crystal, the result was the production of two high quality, single crystalline thin films. This result was even more intriguing when it is considered that thin films are more desirable for NLO applications than are bulk single crystals. Repeated attempts on the ground to reproduce these results were fruitless. A second set of flight experiments was conducted on STS-69 in September 1995. This time eight DCVA experiments were flown, with each of seven experiments containing a slight change from the first reference experiment. The reference experiment was programmed with growth conditions identical to those of the STS-59 mission. The slight variations in each of the other seven were an attempt to understand what particular parameter was responsible for the preference of thin film growth over bulk crystal growth in microgravity. Once again the results were surprising. In all eight cases thin films were grown again, albeit with varying quality. So now we were faced with a phenomenon that not only takes place in microgravity, but also is very robust, resisting all attempts to force the growth of bulk single crystals.

Fundamental Studies of Crystal Growth of Microporous Materials

NASA Technical Reports Server (NTRS)

Dutta, P.; George, M.; Ramachandran, N.; Schoeman, B.; Curreri, Peter A. (Technical Monitor)

2002-01-01

Microporous materials are framework structures with well-defined porosity, often of molecular dimensions. Zeolites contain aluminum and silicon atoms in their framework and are the most extensively studied amongst all microporous materials. Framework structures with P, Ga, Fe, Co, Zn, B, Ti and a host of other elements have also been made. Typical synthesis of microporous materials involve mixing the framework elements (or compounds, thereof) in a basic solution, followed by aging in some cases and then heating at elevated temperatures. This process is termed hydrothermal synthesis, and involves complex chemical and physical changes. Because of a limited understanding of this process, most synthesis advancements happen by a trial and error approach. There is considerable interest in understanding the synthesis process at a molecular level with the expectation that eventually new framework structures will be built by design. The basic issues in the microporous materials crystallization process include: (1) Nature of the molecular units responsible for the crystal nuclei formation; (2) Nature of the nuclei and nucleation process; (3) Growth process of the nuclei into crystal; (4) Morphological control and size of the resulting crystal; (5) Surface structure of the resulting crystals; (6) Transformation of frameworks into other frameworks or condensed structures. The NASA-funded research described in this report focuses to varying degrees on all of the above issues and has been described in several publications. Following is the presentation of the highlights of our current research program. The report is divided into five sections: (1) Fundamental aspects of the crystal growth process; (2) Morphological and Surface properties of crystals; (3) Crystal dissolution and transformations; (4) Modeling of Crystal Growth; (5) Relevant Microgravity Experiments.

Materials processing in space, 1980 science planning document. [crystal growth, containerless processing, solidification, bioprocessing, and ultrahigh vacuum processes

NASA Technical Reports Server (NTRS)

Naumann, R. J.

1980-01-01

The scientific aspects of the Materials Processing in Space program are described with emphasis on the major categories of interest: (1) crystal growth; (2) solidification of metals, alloys, and composites; (3) fluids and chemical processes; (4) containerless processing, glasses, and refractories; (5) ultrahigh vacuum processes; and (6) bioprocessing. An index is provided for each of these areas. The possible contributions that materials science experiments in space can make to the various disciplines are summarized, and the necessity for performing experiments in space is justified. What has been learned from previous experiments relating to space processing, current investigations, and remaining issues that require resolution are discussed. Recommendations for the future direction of the program are included.

Growth of mercuric iodide (HgI2) for nuclear radiation detectors

NASA Technical Reports Server (NTRS)

Vandenberg, L.; Schnepple, W. F.

1988-01-01

Mercuric iodide is a material used for the fabrication of the sensing element in solid state X-ray and gamma ray detecting instruments. The operation of the devices is determined to a large degree by the density of structural defects in the single crystalline material used in the sensing element. Since there were strong indications that the quality of the material was degraded by the effects of gravity during the growth process, a research and engineering program was initiated to grow one or more crystals of mercuric iodide in the reduced gravity environment of space. A special furnace assembly was designed which could be accommodated in a Spacelab rack, and at the same time made it possible to use the same growth procedures and controls used when growing a crystal on the ground. The space crystal, after the flight, was subjected to the same evaluation methods used for earth-grown crystals, so that comparisons could be made.

Program Solicitation Number 86.1, Small Business Innovation Research Program.

DTIC Science & Technology

1986-01-31

Temperature Heat Pipe Technology DESCRIPTION: Heat pipes have been shown to provide superior growth conditions for the growth of bulk semiconductor crystals... Heat pipes allow for the establishment of isothermal conditions over large areas. This thermal property controls the distribution of impurities, and...reliable high temperature heat pipes to operate at 1325 degrees C with inert overpressures of 60 atmospheres is required for the processing of III-V

Integration and use of Microgravity Research Facility: Lessons learned by the crystals by vapor transport experiment and Space Experiments Facility programs

NASA Technical Reports Server (NTRS)

Heizer, Barbara L.

1992-01-01

The Crystals by Vapor Transport Experiment (CVTE) and Space Experiments Facility (SEF) are materials processing facilities designed and built for use on the Space Shuttle mid deck. The CVTE was built as a commercial facility owned by the Boeing Company. The SEF was built under contract to the UAH Center for Commercial Development of Space (CCDS). Both facilities include up to three furnaces capable of reaching 850 C minimum, stand-alone electronics and software, and independent cooling control. In addition, the CVTE includes a dedicated stowage locker for cameras, a laptop computer, and other ancillary equipment. Both systems are designed to fly in a Middeck Accommodations Rack (MAR), though the SEF is currently being integrated into a Spacehab rack. The CVTE hardware includes two transparent furnaces capable of achieving temperatures in the 850 to 870 C range. The transparent feature allows scientists/astronauts to directly observe and affect crystal growth both on the ground and in space. Cameras mounted to the rack provide photodocumentation of the crystal growth. The basic design of the furnace allows for modification to accommodate techniques other than vapor crystal growth. Early in the CVTE program, the decision was made to assign a principal scientist to develop the experiment plan, affect the hardware/software design, run the ground and flight research effort, and interface with the scientific community. The principal scientist is responsible to the program manager and is a critical member of the engineering development team. As a result of this decision, the hardware/experiment requirements were established in such a way as to balance the engineering and science demands on the equipment. Program schedules for hardware development, experiment definition and material selection, flight operations development and crew training, both ground support and astronauts, were all planned and carried out with the understanding that the success of the program science was as important as the hardware functionality. How the CVTE payload was designed and what it is capable of, the philosophy of including the scientists in design and operations decisions, and the lessons learned during the integration process are descussed.

Web-dendritic ribbon growth

NASA Technical Reports Server (NTRS)

Hilborn, R. B., Jr.; Faust, J. W., Jr.

1976-01-01

A web furnace was constructed for pulling dendritic-web samples. The effect of changes in the furnace thermal geometry on the growth of dendritic-web was studied. Several attempts were made to grow primitive dendrites for use as the dendritic seed crystals for web growth and to determine the optimum twin spacing in the dendritic seed crystal for web growth. Mathematical models and computer programs were used to determine the thermal geometries in the susceptor, crucible melt, meniscus, and web. Several geometries were determined for particular furnace geometries and growth conditions. The information obtained was used in conjunction with results from the experimental growth investigations in order to achieve proper conditions for sustained pulling of two dendrite web ribbons. In addition, the facilities for obtaining the following data were constructed: twin spacing, dislocation density, web geometry, resistivity, majority charge carrier type, and minority carrier lifetime.

System for the growth of bulk SiC crystals by modified CVD techniques

NASA Technical Reports Server (NTRS)

Steckl, Andrew J.

1994-01-01

The goal of this program was the development of a SiC CVD growth of films thick enough to be useful as pseudo-substrates. The cold-walled CVD system was designed, assembled, and tested. Extrapolating from preliminary evaluation of SiC films grown in the system at relatively low temperatures indicates that the growth rate at the final temperatures will be high enough to make our approach practical. Modifications of the system to allow high temperature growth and cleaner growth conditions are in progress. This program was jointly funded by Wright Laboratory, Materials Directorate and NASA LeRC and monitored by NASA.

Opportunity for academic research in a low-gravity environment - Crystal growth

NASA Technical Reports Server (NTRS)

Matthiesen, D. H.; Wargo, M. J.; Witt, A. F.

1986-01-01

The history of basic and applied research on crystal growth (CG), especially of semiconductor materials, is reviewed, stressing the dominance (at least in the U.S.) of industrial R&D projects over academic programs and the need for more extensive fundamental investigations. The NASA microgravity research program and the recommendations of the University Space Research Association are examined as they affect the availability of space facilities for academic CG research. Also included is a report on ground experiments on the effectiveness of magnetic fields in controlling vertical Bridgman CG and melt stability, using the apparatus employed in the Apollo-Soyuz experiments (Witt et al., 1978); the results are presented in graphs and briefly characterized. The role of NASA's microgravity CG program in stimulating academic work on CG, the importance of convection effects, CG work on materials other than semiconductors, and NSF support of CG research are discussed in a comment by R. F. Sekerka.

Convective flow effects on protein crystal growth

NASA Technical Reports Server (NTRS)

Rosenberger, Franz; Monaco, Lisa A.

1994-01-01

The long-term stability of the interferometric setup for the monitoring of protein morphologies has been improved. Growth or dissolution of a crystal on a 100 A scale can now be clearly distinguished from dimensional changes occurring within the optical path of the interferometer. This capability of simultaneously monitoring the local interfacial displacement at several widely-spaced positions on the crystal surface with high local depth resolution, has already yielded novel results. We found with lysozyme that (1) the normal growth rate is oscillatory, and (2) the mean growth step density is greater at the periphery of a facet than in its center. The repartitioning of Na(+) and Cl(-) ions between lysozyme solutions and crystals was studied for a wide range of crystallization conditions. A nucleation-growth-repartitioning model was developed to interpret the large body of data in a unified way. The results strongly suggests that (1) the ion to lysozyme ratio in the crystal depends mostly on kinetic rather than crystallographic parameters, and (2) lysozyme crystals possess a salt-rich core with a diameter on the order of 10 microns. The computational model for diffusive-convective transport in protein crystallization (see the First Report) has been applied to a realistic growth cell geometry, taking into account the findings of the above repartitioning studies. These results show that some elements of a moving boundary problem must be incorporated into the model in order to obtain a more realistic description. Our experimental setup for light scattering investigations of aggregation and nucleation in protein solutions has been extensively tested. Scattering intensity measurements with a true Rayleigh scatterer produced systematically increased forward scattering, indicating problems with glare. These have been resolved. Preliminary measurements with supersaturated lysozyme solutions revealed that the scatterers grow with time. Work has begun on a computer program for the unified evaluation of simultaneously obtained, multi-angle static and dynamic light scattering data.

Liquid phase electroepitaxial bulk growth of binary and ternary alloy semiconductors under external magnetic field

NASA Astrophysics Data System (ADS)

Sheibani, Hamdi

2002-01-01

Liquid Phase Electroepitaxy (LPEE) and is a relatively new, promising technique for producing high quality, thick compound semiconductors and their alloys. The main objectives are to reduce the adverse effect of natural convection and to determine the optimum growth conditions for reproducible desired crystals for the optoelectronic and electronic device industry. Among the available techniques for suppressing the adverse effect of natural convection, the application of an external magnetic field seems the most feasible one. The research work in this dissertation consists of two parts. The first part is focused on the design and development of a state of the art LPEE facility with a novel crucible design, that can produce bulk crystals of quality higher than those achieved by the existing LPEE system. A growth procedure was developed to take advantage of this novel crucible design. The research of the growth of InGaAs single crystals presented in this thesis will be a basis for the future LPEE growth of other important material and is an ideal vehicle for the development of a ternary crystal growth process. The second part of the research program is the experimental study of the LPEE growth process of high quality bulk single crystals of binary/ternary semiconductors under applied magnetic field. The compositional uniformity of grown crystals was measured by Electron Probe Micro-analysis (EPMA) and X-ray microanalysis. The state-of-the-art LPEE system developed at University of Victoria, because of its novel design features, has achieved a growth rate of about 4.5 mm/day (with the application of an external fixed magnetic field of 4.5 KGauss and 3 A/cm2 electric current density), and a growth rate of about 11 mm/day (with 4.5 KGauss magnetic field and 7 A/cm2 electric current density). This achievement is simply a breakthrough in LPEE, making this growth technique absolutely a bulk growth technique and putting it in competition with other bulk growth techniques. The growth rates achieved can even be higher for higher electric current and magnetic field intensities. (Abstract shortened by UMI.)

Ferroelectric materials for applications in sensor protection

NASA Astrophysics Data System (ADS)

Bhalla, Amar S.; Cross, L. Eric

1995-07-01

The focus of this program has been upon producing and characterizing new functional materials whose properties can be fine tuned to provide eye sensor protection against laser threats and to suit a range of optoelectronic device applications. Material systems that maximize orientational anisotropy (for use in scattering mode systems) and systems that minimize orientational anisotropy (for use in high field modulators and field induced photorefractive applications) were both approached. Relaxor ferroelectric tungsten bronze single crystals (Sr,Ba)Nb2O6 and (Pb,Ba)Nb2O6 solid solution families and relaxor ferroelectric perovskite (1-x)Pb(Mg(1/3)Nb(2/3))O(3-x)PbTiO3 (PMN-PT) families, were studied extensively. The unique capabilities of a laser heated pedestal growth (LHPG) system were utilized for growth of new materials in single crystal fiber form that produces crystals of long interaction length for optical wave in the crystal and high crystal perfection with maximized properties along chosen directions. Hot uniaxial pressing, hot forging, or appropriate solid state reaction processing methods were used to produce transparent polycrystalline ceramics to provide low scattering, high anisotropy ceramics or high scattering, high anisotropy ceramics. This final report summarizes significant results produced from this program through combination of experimental and crystal chemistry approaches in this field, delineates conclusions drawn from the research, and provides recommendations for future research.

The North Carolina A and T State University Student Space Shuttle Program

NASA Technical Reports Server (NTRS)

Hooker, F. D.; Ahrens, S. T.

1987-01-01

Inspired into being in 1979 by the late astronaut, Dr. Ronald McNair, the primary goal of this student centered program is to perform two experiments, Arthopod Development Study and Crystal Growth Study. Since 1979, 78 different students representing 12 majors have participated in every phase of development of the payload -- from coming up with the original ideas to final fabrication and testing. Students have also been involved in many extra activities such as presenting their results at annual meetings and hosting tours of our lab for local schools. The program has received extensive outside support in the form of funds, technical assistance and donated parts. The payload, made primarily out of aluminum, consists of a central column structure, a battery box, a crystal growth box, an arthropod development box, four control circuit boxes, and a thermograph box. The battery box contains 24, Eveready 6V, Alkaline batteries. The thermograph box contains 3 Ryan TempMentors. Fabrication of the payload is essentially complete and a complete testing program has been initiated.

Computational Simulation of Containment Influence on Defect Generation During Growth of GeSi

NASA Technical Reports Server (NTRS)

Motakef, Shariar; Yesilyurt, S.; Vujisic, L.

2001-01-01

This report contains results of theoretical work in conjunction with the NASA RDGS program. It is specifically focused on factors controlling the stability of detachment and the sensitivity of the detachment process to the processing and geometric parameters of the crystal growth process.

Zone leveling and solution growth of complex compound semiconductors in space

NASA Technical Reports Server (NTRS)

Bachmann, K. J.

1986-01-01

A research program on complex semiconducting compounds and alloys was completed that addressed the growth of single crystals of CdSe(y)Te(1-y), Zn(x)Cd(1-x)Te, Mn(x)Cd(1-x)Te, InP(y)As(1-y) and CuInSe2 and the measurement of fundamental physico-chemical properties characterizing the above materials. The purpose of this ground based research program was to lay the foundations for further research concerning the growth of complex ternary compound semiconductors in a microgravity environment.

Protein crystal growth; Proceedings of the First International Conference, Stanford University, CA, August 14-16, 1985

NASA Technical Reports Server (NTRS)

Feigelson, R. S. (Editor)

1986-01-01

Papers are presented on mechanisms of nucleation and growth of protein crystals, the role of purification in the crystallization of proteins and nucleic acids, and the effect of chemical impurities in polyethylene glycol on macromolecular crystallization. Also considered are growth kinetics of tetragonal lysozyme crystals, thermodynamic and kinetic considerations for crystal growth of complex molecules from solution, protein single-crystal growth under microgravity, and growth of organic crystals in a microgravity environment. Papers are also presented on preliminary investigations of protein crystal growth using the Space Shuttle, convective diffusion in protein crystal growth, and the growth and characterization of membrane protein crystals.

Control of fluid flow during Bridgman crystal growth using low-frequency vibrational stirring

NASA Astrophysics Data System (ADS)

Zawilski, Kevin Thomas

The goal of this research program was to develop an in depth understanding of a promising new method for stirring crystal growth melts called coupled vibrational stirring (CVS). CVS is a mixing technique that can be used in sealed systems and produces rapid mixing through vortex flows. Under normal operating conditions, CVS uses low-frequency vibrations to move the growth crucible along a circular path, producing a surface wave and convection in the melt. This research focused on the application of CVS to the vertical Bridgman technique. CVS generated flows were directly studied using a physical modeling system containing water/glycerin solutions. Sodium nitrate was chosen as a model growth system because the growth process could be directly observed using a transparent furnace. Lead magnesium niobate-lead titanate (PMNT) was chosen as the third system because of its potential application for high performance solid state transducers and actuators. In this study, the critical parameters for controlling CVS flows in cylindrical Bridgman systems were established. One of the most important results obtained was the dependence of an axial velocity gradient on the vibrational frequency. By changing the frequency, the intensity of fluid flow at a given depth can be easily manipulated. The intensity of CVS flows near the crystal-melt interface was found to be important. When flow intensity near the interface increased during growth, large growth rate fluctuations and significant changes in interface shape were observed. To eliminate such fluctuations, a constant flow rate near the crystal-melt interface was maintained by decreasing the vibrational frequency. A continuous frequency ramp was found to be essential to grow crystals of good quality under strong CVS flows. CVS generated flows were also useful in controlling the shape of the growth interface. In the sodium nitrate system without stirring, high growth rates produced a very concave interface. By adjusting the flow intensity near the interface, CVS flows were able to flatten the growth interface under these extreme growth conditions.

The Biophysics Microgravity Initiative

NASA Technical Reports Server (NTRS)

Gorti, S.

2016-01-01

Biophysical microgravity research on the International Space Station using biological materials has been ongoing for several decades. The well-documented substantive effects of long duration microgravity include the facilitation of the assembly of biological macromolecules into large structures, e.g., formation of large protein crystals under micro-gravity. NASA is invested not only in understanding the possible physical mechanisms of crystal growth, but also promoting two flight investigations to determine the influence of µ-gravity on protein crystal quality. In addition to crystal growth, flight investigations to determine the effects of shear on nucleation and subsequent formation of complex structures (e.g., crystals, fibrils, etc.) are also supported. It is now considered that long duration microgravity research aboard the ISS could also make possible the formation of large complex biological and biomimetic materials. Investigations of various materials undergoing complex structure formation in microgravity will not only strengthen NASA science programs, but may also provide invaluable insight towards the construction of large complex tissues, organs, or biomimetic materials on Earth.

Optimal design of solidification processes

NASA Technical Reports Server (NTRS)

Dantzig, Jonathan A.; Tortorelli, Daniel A.

1991-01-01

An optimal design algorithm is presented for the analysis of general solidification processes, and is demonstrated for the growth of GaAs crystals in a Bridgman furnace. The system is optimal in the sense that the prespecified temperature distribution in the solidifying materials is obtained to maximize product quality. The optimization uses traditional numerical programming techniques which require the evaluation of cost and constraint functions and their sensitivities. The finite element method is incorporated to analyze the crystal solidification problem, evaluate the cost and constraint functions, and compute the sensitivities. These techniques are demonstrated in the crystal growth application by determining an optimal furnace wall temperature distribution to obtain the desired temperature profile in the crystal, and hence to maximize the crystal's quality. Several numerical optimization algorithms are studied to determine the proper convergence criteria, effective 1-D search strategies, appropriate forms of the cost and constraint functions, etc. In particular, we incorporate the conjugate gradient and quasi-Newton methods for unconstrained problems. The efficiency and effectiveness of each algorithm is presented in the example problem.

Investigation of Vibrational Control of the Bridgman Crystal Growth Technique

NASA Technical Reports Server (NTRS)

Fedoseyev, Alexandre I.

1998-01-01

The objectives are: Conduct a parametric theoretical and numerical investigation of vibro-convective buoyancy-driven flow in differentially heated cylindrical containers. Investigate buoyant vibro-convective transport regimes in Bridgman-type systems with a focus on the use of vibration to suppress, or control, convection in order to achieve transport control during crystal growth. Assess the feasibility of vibro-convective control as a means of offsetting "g-jitter" effects under microgravity conditions, Exchange information with the experimental group at the General Physics Institute (GPI) of the Russian Academy of Science who are undertaking a complementary experimental program.

GROWTH AND CHARACTERIZATION OF SINGLE CRYSTALS OF RARE EARTH COMPOUNDS.

DTIC Science & Technology

SINGLE CRYSTALS, CRYSTAL GROWTH), (*CRYSTAL GROWTH, SINGLE CRYSTALS), (*RARE EARTH COMPOUNDS, SINGLE CRYSTALS), EPITAXIAL GROWTH, SODIUM COMPOUNDS, CHLORIDES, VAPOR PLATING, ELECTROSTATIC FIELDS, ENERGY, ATOMIC PROPERTIES , BONDING

On the origin of size-dependent and size-independent crystal growth: Influence of advection and diffusion

USGS Publications Warehouse

Kile, D.E.; Eberl, D.D.

2003-01-01

Crystal growth experiments were conducted using potassium alum and calcite crystals in aqueous solution under both non-stirred and stirred conditions to elucidate the mechanism for size-dependent (proportionate) and size-independent (constant) crystal growth. Growth by these two laws can be distinguished from each other because the relative size difference among crystals is maintained during proportionate growth, leading to a constant crystal size variance (??2) for a crystal size distribution (CSD) as the mean size increases. The absolute size difference among crystals is maintained during constant growth, resulting in a decrease in size variance. Results of these experiments show that for centimeter-sized alum crystals, proportionate growth occurs in stirred systems, whereas constant growth occurs in non-stirred systems. Accordingly, the mechanism for proportionate growth is hypothesized to be related to the supply of reactants to the crystal surface by advection, whereas constant growth is related to supply by diffusion. Paradoxically, micrometer-sized calcite crystals showed proportionate growth both in stirred and in non-stirred systems. Such growth presumably results from the effects of convection and Brownian motion, which promote an advective environment and hence proportionate growth for minute crystals in non-stirred systems, thereby indicating the importance of solution velocity relative to crystal size. Calcite crystals grown in gels, where fluid motion was minimized, showed evidence for constant, diffusion-controlled growth. Additional investigations of CSDs of naturally occurring crystals indicate that proportionate growth is by far the most common growth law, thereby suggesting that advection, rather than diffusion, is the dominant process for supplying reactants to crystal surfaces.

Ice crystal precipitation at Dome C site (East Antarctica)

NASA Astrophysics Data System (ADS)

Santachiara, G.; Belosi, F.; Prodi, F.

2016-01-01

For the first time, falling ice crystals were collected on glass slides covered with a thin layer of 2% formvar in chloroform at the Dome Concordia site (Dome C), Antarctica. Samplings were performed in the framework of the 27th Italian Antarctica expedition of the Italian National Program for Research in Antarctica in the period 21 February-6 August 2012. Events of clear-sky precipitations and precipitations from clouds were considered and the replicas obtained were examined under Scanning Electron Microscope (SEM). Several shapes of ice crystals were identified, including ;diamond dust; (plates, pyramids, hollow and solid columns), and crystal aggregates varying in complexity. Single events often contained both small (10 μm to 50 μm) and large (hundreds of microns) crystals, suggesting that crystals can form simultaneously near the ground (height of a few hundred metres) and at higher layers (height of thousands of metres). Images of sampled crystal replicas showed that single bullets are not produced separately, but by the disintegration of combinations of bullets. Rimed ice crystals were absent in the Dome C samples, i.e. the only mode of crystal growth was water vapour diffusion. On considering the aerosol in the sampled crystals, we reached the conclusion that inertial impaction, interception and Brownian motion were insufficient to explain the scavenged aerosol. We therefore presume that phoretic forces play a role in scavenging during the crystal growth process.

Interface demarcation in GaAs by current pulsing

NASA Technical Reports Server (NTRS)

Matthiesen, D. H.; Kafalas, J. A.; Duchene, G. A.; Bellows, A. H.

1990-01-01

GTE Laboratories is currently conducting a program to investigate the effect of convection in the melt on the properties of bulk grown gallium arsenide (GaAs). In addition to extensive ground based experimentation, a Get Away Special growth system has been developed to grow two GaAs crystals aboard the Space Shuttle, each with a one inch diameter. In order to perform a complete segregation analysis of the crystals grown in space, it is necessary to measure the interface shape and growth rate as well as the spatial distribution of the selenium dopant. The techniques for interface demarcation in selenium doped GaAs by current pulsing have been developed at GTE Laboratories and successful interface demarcation has been achieved for current pulses ranging from 20 to 90 amps, in both single crystal and polycrystalline regions.

Comment on "Evaluation of X-ray diffraction methods for determining the crystal growth mechanisms of clay minerals in mudstones, shales and slates," by L. N. Warr and D. R. Peacor

USGS Publications Warehouse

Eberl, D.D.; Srodon, J.; Drits, V.A.

2003-01-01

A recent paper by Warr and Peacor (2002) suggested that our use of the Bertaut-Warren-Averbach technique (MudMaster computer program) for studying changes in crystallite thickness distributions (CTDs) of clay minerals during diagenesis and very low-grade metamorphism is not reliable because it is dependent on many variables which can not be fully controlled. Furthermore, the authors implied that the measured shapes of CTDs cannot be used with confidence to deduce crystal growth mechanisms and histories for clays, based on our CTD simulation approach (using the Galoper computer program). We disagree with both points, and show that the techniques are powerful, reliable and useful for studying clay mineral alteration in rocks. ?? 2003 Schweiz. Mineral. Petrogr. Ges.

Decades of Data: Extracting Trends from Microgravity Crystallization History

NASA Technical Reports Server (NTRS)

Judge, R. A.; Snell, E. H.; Kephart, R.; vanderWoerd, M.

2004-01-01

The reduced acceleration environment of an orbiting spacecraft has been proposed as an ideal environment for biological crystal growth as the first sounding rocket flight in 1981 many crystallization experiments have flown with some showing improvement and others not. To further explore macromolecule crystal improvement in microgravity we have accumulated data from published reports and reports submitted by 63 missions including the Space Shuttle program, unmanned satellites, the Russian Space Station MIR and sounding rocket experiments. While it is not at this point in time a comprehensive record of all flight crystallization experimental results, there is however sufficient information for emerging trends to be identified. In this study the effects of the acceleration environment, the techniques of crystallization, sample molecular weight and the response of individual macromolecules to microgravity crystallization will be investigated.

Crystallization of sodium chloride from a concentrated calcium chloride-potassium chloride-sodium chloride solution in a CMSMPR crystallizer: Observation of crystal size distribution and model validation

NASA Astrophysics Data System (ADS)

Choi, Byung Sang

Compared to overwhelming technical data available in other advanced technologies, knowledge about particle technology, especially in particle synthesis from a solution, is still poor due to the lack of available equipment to study crystallization phenomena in a crystallizer. Recent technical advances in particle size measurement such as Coulter counter and laser light scattering have made in/ex situ study of some of particle synthesis, i.e., growth, attrition, and aggregation, possible with simple systems. Even with these advancements in measurement technology, to grasp fully the crystallization phenomena requires further theoretical and technical advances in understanding such particle synthesis mechanisms. Therefore, it is the motive of this work to establish the general processing parameters and to produce rigorous experimental data with reliable performance and characterization that rigorously account for the crystallization phenomena of nucleation, growth, aggregation, and breakage including their variations with time and space in a controlled continuous mixed-suspension mixed-product removal (CMSMPR) crystallizer. This dissertation reports the results and achievements in the following areas: (1) experimental programs to support the development and validation of the phenomenological models and generation of laboratory data for the purpose of testing, refining, and validating the crystallization process, (2) development of laboratory well-mixed crystallizer system and experimental protocols to generate crystal size distribution (CSD) data, (3) the effects of feed solution concentration, crystallization temperature, feed flow rate, and mixing speed, as well as different types of mixers resulting in the evolution of CSDs with time from a concentrated brine solution, (4) with statistically designed experiments the effects of processing variables on the resultant particle structure and CSD at steady state were quantified and related to each of those operating conditions by studying the detailed crystallization processes, such as nucleation, growth, and breakage, as well as agglomeration. The purification of CaCl2 solution involving the crystallization of NaCl from the solution mixture of CaCl2, KCl, and NaCl as shipped from Dow Chemical, Ludington, in a CMSMPR crystallizer was studied as our model system because of its nucleation and crystal growth tendencies with less agglomeration. This project also generated a significant body of experimental data that are available at URL that is http://www.che.utah.edu/˜ring/CrystallizationWeb.

Development of advanced Czochralski growth process to produce low cost 150 kg silicon ingots from a single crucible for technology readiness

NASA Technical Reports Server (NTRS)

1981-01-01

The process development continued, with a total of nine crystal growth runs. One of these was a 150 kg run of 5 crystals of approximately 30 kg each. Several machine and process problems were corrected and the 150 kg run was as successful as previous long runs on CG2000 RC's. The accelerated recharge and growth will be attempted when the development program resumes at full capacity in FY '82. The automation controls (Automatic Grower Light Computer System) were integrated to the seed dip temperature, shoulder, and diameter sensors on the CG2000 RC development grower. Test growths included four crystals, which were grown by the computer/sensor system from seed dip through tail off. This system will be integrated on the Mod CG2000 grower during the next quarter. The analytical task included the completion and preliminary testing of the gas chromatograph portion of the Furnace Atmosphere Analysis System. The system can detect CO concentrations and will be expanded to oxygen and water analysis in FY '82.

New Directions in Biotechnology

NASA Technical Reports Server (NTRS)

2003-01-01

The macromolecule crystallization program within NASA is undergoing considerable pressure, particularly budgetary pressure. While it has shown some successes, they have not lived up to the expectations of others, and technological advances may rapidly overtake the natural advantages offered by crystallization in microgravity. Concomitant with the microgravity effort has been a research program to study the macromolecule crystallization process. It was believed that a better understanding of the process would lead to growth of improved crystals for X-ray diffraction studies. The results of the various research efforts have been impressive in improving our understanding of macromolecule crystallization, but have not led to any improved structures. Macromolecule crystallization for structure determination is "one of", the job being unique for every protein and finished once a structure is obtained. However, the knowledge gained is not lost, but instead lays the foundation for developments in new areas of biotechnology and nanotechnology. In this it is highly analogous to studies into small molecule crystallization, the results of which have led to our present day microelectronics-based society. We are conducting preliminary experiments into areas such as designed macromolecule crystals, macromolecule-inorganic hybrid structures, and macromolecule-based nanotechnology. In addition, our protein crystallization studies are now being directed more towards industrial and new approaches to membrane protein crystallization.

Materials processing threshold report. 1: Semiconductor crystals for infrared detectors

NASA Technical Reports Server (NTRS)

Sager, E. V.; Thompson, T. R.; Nagler, R. G.

1980-01-01

An extensive search was performed of the open literature pertaining to infrared detectors to determine what constitutes a good detector and in what way performance is limited by specific material properties. Interviews were conducted with a number of experts in the field to assess their perceptions of the state of the art and of the utility of zero-gravity processing. Based on this information base and on a review of NASA programs in crystal growth and infrared sensors, NASA program goals were reassessed and suggestions are presented as to possible joint and divergent efforts between NASA and DOD.

Control of interface shape during high melting sesquioxide crystal growth by HEM technique

NASA Astrophysics Data System (ADS)

Hu, Kaiwei; Zheng, Lili; Zhang, Hui

2018-02-01

During crystal growth in heat exchanger method (HEM) system, the shape of the growth interface changes with the proceeding of the growth process, which limits the crystal size and reduces the quality of the crystal. In this paper, a modified HEM system is proposed to control the interface shape for growth of sesquioxide crystals. Numerical simulation is performed to predict heat transfer, melt flow and interface shape during growth of high melting sesquioxide crystals by the heat exchanger method. The results show that a flat or slightly convex interface shape is beneficial to reduce the solute pileup in front of the melt/crystal interface and decrease the radial temperature gradient inside the crystal during growth of sesquioxide crystals. The interface shape can be controlled by adjusting the gap size d and lower resistance heater power during growth. The growth rate and the melt/crystal interface position can be obtained by two measured temperatures.

New Programs Utilizing Light Scattering and Flow Imaging Techniques for Macromolecular Crystal Growth and Fluid Dynamics Studies

NASA Technical Reports Server (NTRS)

2003-01-01

Dr. Phil Segre, a physicist by training, is a recent addition to the Biotech group, SD46, having joined NASA in August of 2000. Over the past two years he has been developing a laboratory for the study of macromolecular and protein crystal growth. The main apparatus for this work is a Dynamic Light Scattering apparatus, DLS, which is capable of making highly precise measurements of size distributions of both protein solutions and protein crystals. With Drs. Chernov and Thomas (USRA), he has begun a collaboration studying the affects of protein impurities on protein crystal growth and subsequent crystal quality. One of the hypotheses behind the differences between Earth and space grown protein crystals is that the absorption of harmful impurities is reduced in space due to the absence of convective flows. Using DLS measurements we are examining crystal growth with varying amounts of impurities and testing whether there is a strong physical basis behind this hypothesis. With Dr. Joe Ng of UAH he has been collaborating on a project to examine the folding/unfolding dynamics of large RNA complexes. A detailed understanding of this process is necessary for the handling of RNA in biotech applications, and the DLS instrument gives details and results beyond that of other instruments. With Prof. Jim McClymer of the University of Maine (summer faculty visitor to NASA in 2001, 2002), we have been studying the crystallization process in model colloidal suspensions whose behavior in some cases can mimic that of much smaller protein solutions. An understanding of the self-assembly of colloids is the first step in the process of engineering novel materials for photonic and light switching applications. Finally, he has begun an investigation into the physics of particle sedimentation. In addition to the DLS instrument he also has an instrument (called PIV) that can measure flow fields of fluids. The applications are to the dynamics of protein crystal motions both on earth and in low-gravity.

STS-34: Mission Overview Briefing

NASA Technical Reports Server (NTRS)

1989-01-01

Live footage shows Milt Heflin, the Lead Flight Director participating in the STS-34 Mission Briefing. He addresses the primary objective, and answered questions from the audience and other NASA Centers. Heflin also mentions the Shuttle Solar Backscatter Ultraviolet secondary payload, and several experiments. These experiments include Growth Hormone Crystal Distribution (Plants), Polymer Morphology, Sensor Technology Experiment, Mesoscale Lightning Experiment, Shuttle Student Involvement Program "Ice Crystals", and the Air Force Maui Optical Site.

Surrogate Seeds For Growth Of Crystals

NASA Technical Reports Server (NTRS)

Shlichta, Paul J.

1989-01-01

Larger crystals of higher quality grown. Alternative method for starting growth of crystal involves use of seed crystal of different material instead of same material as solution. Intended for growing single-crystal proteins for experiments but applicable in general to growth of crystals from solutions and to growth of semiconductor or other crystals from melts.

Features in simulation of crystal growth using the hyperbolic PFC equation and the dependence of the numerical solution on the parameters of the computational grid

DOE Office of Scientific and Technical Information (OSTI.GOV)

Starodumov, Ilya; Kropotin, Nikolai

2016-08-10

We investigate the three-dimensional mathematical model of crystal growth called PFC (Phase Field Crystal) in a hyperbolic modification. This model is also called the modified model PFC (originally PFC model is formulated in parabolic form) and allows to describe both slow and rapid crystallization processes on atomic length scales and on diffusive time scales. Modified PFC model is described by the differential equation in partial derivatives of the sixth order in space and second order in time. The solution of this equation is possible only by numerical methods. Previously, authors created the software package for the solution of the Phasemore » Field Crystal problem, based on the method of isogeometric analysis (IGA) and PetIGA program library. During further investigation it was found that the quality of the solution can strongly depends on the discretization parameters of a numerical method. In this report, we show the features that should be taken into account during constructing the computational grid for the numerical simulation.« less

Thermal analysis of Bridgman-Stockbarger growth. [mercury cadmium telluride single crystals

NASA Technical Reports Server (NTRS)

Knopf, F. W.

1979-01-01

A thermal analysis of a cylindrical HgCdTe sample in a Bridgman-Stockbarger crystal growth configuration was conducted with emphasis on the thermal profile, interface shape and position, and the thermal gradients at the liquid-solid interface. Alloys of HgTe and CdTe with compositions approximating 20 percent CdTe, 80 percent HgTe were used. This composition results in a bandgap suited for the detection of 10.6 micron CO2 radiation. The sensitivity of the sample thermal characteristics to important growth parameters, such as thermal diffusivities, thermal conductivities, furnace temperature profile, ampoule dimensions, and growth velocity was assessed. Numerical techniques and associated computational models necessary to analyze the heat transfer process within the sample and the Bridgman-Stockbarger boundary conditions were developed. This thermal analysis mode was programmed in FORTRAN V, and is currently operational on the MSFC Univac 1100 system.

Study of FES/CAST/HGS

NASA Technical Reports Server (NTRS)

Workman, Gary L.; Cummings, Rick; Jones, Brian

1992-01-01

The microgravity materials processing program has been instrumental in providing the crystal growth community with an experimental environment to better understand the phenomena associated with the growing of crystals. In many applications one may pursue the growth of large single crystals which cannot be grown on earth due to convective driven flows. A microgravity environment is characterized by neither convection of buoyancy. Consequently superior crystals are able to be grown in space. On the other hand, since neither convection nor buoyancy dominates the fluid flow in a microgravity environment, then lesser dominating phenomena can affect crystal growth, such as surface driven flows or diffusion limited solidification. In the case of experiments that are to be flown in space using the Fluid Experiments System (FES), diffusion limited growth should be the dominating phenomenon. The use of holographic and Schlieren optical techniques for studying the concentration gradients in solidification processes has been used by several investigators over the years. The Holographic Ground System (HGS) facility at MSFC has been a primary resource in researching this capability. Consequently scientific personnel have been able to utilize these techniques in both ground based research and in space experiments. An important event in the scientific utilization of the HGS facilities was the TGS (triglycine sulfate) Crystal Growth and the Casting and Solidification Technology (CAST) experiments that were flown on the International Microgravity Lab (IML) mission in March of this year. The preparation and processing of these space observations are the primary experiments reported in this work. This project provides some ground-based studies to optimize on the holographic techniques used to acquire information about the crystal growth processes flown on IML. Since the ground-based studies will be compared with the space-based experimental results, it is necessary to conduct sufficient ground based studies to best determine how the experiment in space worked. The current capabilities in computer based systems for image processing and numerical computation have certainly assisted in those efforts. As anticipated, this study has certainly shown that these advanced computing capabilities are helpful in the data analysis of such experiments.

Immiscible fluid: Heat of fusion heat storage system

NASA Technical Reports Server (NTRS)

Edie, D. D.; Melsheimer, S. S.; Mullins, J. C.

1980-01-01

Both heat and mass transfer in direct contact aqueous crystallizing systems were studied as part of a program desig- ned to evaluate the feasibility of direct contact heat transfer in phase change storage using aqueous salt system. Major research areas, discussed include (1) crystal growth velocity study on selected salts; (2) selection of salt solutions; (3) selection of immiscible fluids; (4) studies of heat transfer and system geometry; and (5) system demonstration.

Shape Evolution of Detached Bridgman Crystals Grown in Microgravity

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.

2015-01-01

Detached (or dewetted) Bridgman crystal growth defines that process in which a gap exists between a growing crystal and the crucible wall. In microgravity, the parameters that influence the existence of a stable gap are the growth angle of the solidifying crystal, the contact angle between the melt and the crucible wall, and the pressure difference across the meniscus. During actual crystal growth, the initial crystal radius will not have the precise value required for stable detached growth. Beginning with a crystal diameter that differs from stable conditions, numerical calculations are used to analyze the transient crystal growth process. Depending on the initial conditions and growth parameters, the crystal shape will either evolve towards attachment at the crucible wall, towards a stable gap width, or inwards towards eventual collapse of the meniscus. Dynamic growth stability is observed only when the sum of the growth and contact angles exceeds 180 degrees.

Thermophysical Property Measurements of Molten Semiconductors in 1-g and Reduced-g Condition

NASA Technical Reports Server (NTRS)

Rhim, Won-Kyu

1999-01-01

Understanding and controlling the formation kinetics of varieties of crystal imperfections such as point defects, non uniform distribution of doping atoms, and impurity atoms in growing crystals are very important. Theoretical (numerical) modeling of the crystal growth process is an essential step to achieving these objectives. In order to obtain reliable modeling results, input parameters, i.e. various thermophysical parameters, must be accurate. The importance of accurate thermophysical properties of semiconductors in crystal growth cannot be overly emphasized. The total hemispherical emissivity, for instance, has a dramatic impact on the thermal environment. It determines the radiative emission from the surface of the melt which determines to a large extent the profile of the solidified crystal. In order to understand the convection and the turbulence in a melt, viscosity becomes an important parameter. The liquid surface tension determines the shape of the liquid-atmosphere interface near the solid-liquid-atmosphere triple point. Currently used values for these parameters are rather inaccurate, and this program intends to provide more reliable measurements of these thermophysical properties. Thus, the objective of this program is in the accurate measurements of various thermophysical properties which can be reliably used in the modeling of various crystal growth processes. In this program, thermophysical properties of molten semiconductors, such as Si, Ge, Si-Ge, and InSb will be measured as a function of temperature using the High Temperature Electrostatic Levitator at JPL. Each material will be doped by different kinds of impurities at various doping levels. Thermophysical properties which will be measured include: density, thermal expansion coefficient, surface tension, viscosity, specific heat, hemispherical total emissivity, and perhaps electrical and thermal conductivities. Many molten semiconductors are chemically reactive with crucibles. As a result, these dispersed impurities in the melts tend to substantially modify the properties of pure semiconductors. Sample levitation done in a vacuum clearly helps maintain the sample purity. However, in the 1-g environment, all gravity caused effects such as convection, sedimentation and buoyancy are still present in the sample. In addition, large forces needed to levitate a sample in the presence of the gravity can cause additional flows in the melt. The use of the High Temperature Electrostatic Levitator (HTESL) for the present research is a recent development and little is known about the flows induced by the electrostatic forces. In this ground base program, we will define the limits of HTESL technology as various thermophysical properties of molten semiconductors are measured.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yuan, Chunqing; Smith, R. Scott; Kay, Bruce D.

The crystallization kinetics of nanoscale amorphous solid water (ASW) films are investigated using temperature-programmed desorption (TPD) and reflection absorption infrared spectroscopy (RAIRS). TPD measurements are used to probe surface crystallization and RAIRS measurements are used to probe bulk crystallization. Isothermal TPD results show that surface crystallization is independent of the film thickness (from 100 to 1000 ML). Conversely, the RAIRS measurements show that the bulk crystallization time increases linearly with increasing film thickness. These results suggest that nucleation and crystallization begin at the ASW/vacuum interface and then the crystallization growth front propagates linearly into the bulk. This mechanism was confirmedmore » by selective placement of an isotopic layer (5% D2O in H2O) at various positions in an ASW (H2O) film. In this case, the closer the isotopic layer was to the vacuum interface, the earlier the isotopic layer crystallized. These experiments provide direct evidence to confirm that ASW crystallization in vacuum proceeds by a “top-down” crystallization mechanism.« less

Unsteady-state transfer of impurities during crystal growth of sucrose in sugarcane solutions

NASA Astrophysics Data System (ADS)

Martins, P. M.; Ferreira, A.; Polanco, S.; Rocha, F.; Damas, A. M.; Rein, P.

2009-07-01

In this work, we present growth rate data of sucrose crystals in the presence of impurities that can be used by both sugar technologists and crystal growth scientists. Growth rate curves measured in a pilot-scale evaporative crystallizer suggest a period of slow growth that follows the seeding of crystals into supersaturated technical solutions. The observed trend was enhanced by adding typical sugarcane impurities such as starch, fructose or dextran to the industrial syrups. Maximum growth rates of sucrose resulted at intermediate rather than high supersaturation levels in the presence of the additives. The effects of the additives on the sucrose solubility and sucrose mass transfer in solution were taken into account to explain the observed crystal growth kinetics. A novel mechanism was identified of unsteady-state adsorption of impurities at the crystal surface and their gradual replacement by the crystallizing solute towards the equilibrium occupation of the active sites for growth. Specifically designed crystallization experiments at controlled supersaturation confirmed this mechanism by showing increasing crystal growth rates with time until reaching a steady-state value for a given supersaturation level and impurity content.

Growth of single crystals of BaFe12O19 by solid state crystal growth

NASA Astrophysics Data System (ADS)

Fisher, John G.; Sun, Hengyang; Kook, Young-Geun; Kim, Joon-Seong; Le, Phan Gia

2016-10-01

Single crystals of BaFe12O19 are grown for the first time by solid state crystal growth. Seed crystals of BaFe12O19 are buried in BaFe12O19+1 wt% BaCO3 powder, which are then pressed into pellets containing the seed crystals. During sintering, single crystals of BaFe12O19 up to ∼130 μm thick in the c-axis direction grow on the seed crystals by consuming grains from the surrounding polycrystalline matrix. Scanning electron microscopy-energy dispersive spectroscopy analysis shows that the single crystal and the surrounding polycrystalline matrix have the same chemical composition. Micro-Raman scattering shows the single crystal to have the BaFe12O19 structure. The optimum growth temperature is found to be 1200 °C. The single crystal growth behavior is explained using the mixed control theory of grain growth.

An Apparatus for Growth of Small Crystals From Solutions.

ERIC Educational Resources Information Center

Mitrovic, Mico M.

1995-01-01

Describes an apparatus for crystal growth that was designed to study growth kinetics of small crystals from solutions and to obtain crystals of various substances. Describes the use of the apparatus in laboratory practical experiments in the field of crystal growth physics within the course "Solid State Physics". (JRH)

Design, fabrication and test of prototype furnace for continuous growth of wide silicon ribbon

NASA Technical Reports Server (NTRS)

Duncan, C. S.; Seidensticker, R. G.

1976-01-01

A program having the overall objective of growing wide, thin silicon dendritic web crystals quasi-continuously from a semi-automated facility is discussed. The design considerations and fabrication of the facility as well as the test and operation phase are covered; detailed engineering drawings are included as an appendix. During the test and operation phase of the program, more than eighty growth runs and numerous thermal test runs were performed. At the conclusion of the program, 2.4 cm wide web was being grown at thicknesses of 100 to 300 micrometers. As expected, the thickness and growth rate are closely related. Solar cells made from this material were tested at NASA-Lewis and found to have conversion efficiencies comparable to devices fabricated from Czochralski material.

Mobil Solar Energy Corporation thin EFG octagons. Semiannual subcontract report, 1 April 1992--30 September 1992

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kalejs, J.P.

1993-09-01

This report describes work carried out for the PVMaT program at Mobil Solar for the period covering April 1, 1992, to September 30, 1992. Mobil Solar is developing advanced technology for growing and cutting 200-{mu}m-thick edge-defined film-fed growth (EFG) octagon tubes that will reduce the manufacturing costs of 10-cm {times} 10-cm polycrystalline EFG silicon wafers. Mobil Solar has made progress in identifying factors that impact on thickness nonuniformity and means to reduce the deleterious impact of ambient-related effects that have caused reduction in crystal growth productivity and wafer yield. The current main obstacle to meeting material yield targets arises duemore » to the buckling produced by thermal stress. Studies of laser cutting of EFG silicon using ND:YAG and dye lasers are underway to develop reduced damage cutting methods. Mobil Solar has carried out design reviews for crystal growth and laser cutting equipment. A task has been initiated to evaluate new online sensors for crystal growth process control and to study implementation of advanced control concepts for productivity and yield improvements.« less

Solution Growth and Characterization of Single Crystals on Earth and in Microgravity

NASA Technical Reports Server (NTRS)

Aggarwal, M. D.; Currie, J. R.; Penn, B. G.; Batra, A. K.; Lal, R. B.

2007-01-01

Crystal growth has been of interest to physicists and engineers for a long time because of their unique properties. Single crystals are utilized in such diverse applications as pharmaceuticals, computers, infrared detectors, frequency measurements, piezoelectric devices, a variety of high-technology devices, and sensors. Solution crystal growth is one of the important techniques to grow a variety of crystals when the material decomposes at the melting point and a suitable solvent is available to make a saturated solution at a desired temperature. In this Technical Memorandum (TM) an attempt is made to give the fundamentals of growing crystals from solution including improved designs of various crystallizers. Since the same solution crystal growth technique could not be used in microgravity, the authors proposed a new cooled-sting technique to grow crystals in space. The authors experience from conducting two Space Shuttle solution crystal growth experiments are also detailed in this TM and the complexity of solution growth experiments to grow crystals in space are also discussed. These happen to be some of the early experiments performed in space, and various lessons learned are described. A brief discussion of protein crystal growth that shares basic principles of the solution growth technique is given, along with some flight hardware information for growth in microgravity.

Growth and Characteristics of Bulk Single Crystals Grown from Solution on Earth and in Microgravity

NASA Technical Reports Server (NTRS)

Aggarwal, M. D.; Batra, A. K.; Lal, R. B.; Penn, Benjamin G.; Frazier, Donald O.

2011-01-01

The growth of crystals has been of interest to physicists and engineers for a long time because of their unique properties. Single crystals are utilized in such diverse applications as pharmaceuticals, computers, infrared detectors, frequency measurements, piezoelectric devices, a variety of high technology devices and sensors. Solution crystal growth is one of the important techniques to grow a variety of crystals when the material decomposes at the melting point and a suitable solvent is available to make a saturated solution at a desired temperature. In this chapter an attempt is made to give some fundamentals of growing crystals from solution including improved designs of various crystallizers. Since the same solution crystal growth technique could not be used in microgravity, authors had proposed a new cooled sting technique to grow crystals in space. Authors? experiences of conducting two space shuttle experiments relating to solution crystal growth are also detailed in this work. The complexity of these solution growth experiments to grow crystals in space are discussed. These happen to be some of the early experiments performed in space, and various lessons learned are described. A brief discussion of protein crystal growth that also shares basic principles of solution growth technique is given along with some flight hardware information for its growth in microgravity.

Overview of materials processing in space activity at Marshall Space Flight Center

NASA Technical Reports Server (NTRS)

Williams, J. R.; Chassay, R. P.; Moore, W. W.; Ruff, R. C.; Yates, I. C.

1984-01-01

An overview of activities involving the Space Transportation System (STS), now in the operational phase, and results of some of the current space experiments, as well as future research opportunities in microgravity environment, are presented. The experiments of the Materials Processing in Space Program flown on the STS, such as bioseparation processes, isoelectric focusing, solidification and crystal growth processes, containerless processes, and the Materials Experiment Assembly experiments are discussed. Special consideration is given to the experiments to be flown aboard the Spacelab 3 module, the Fluids Experiments System, and the Vapor Crystal Growth System. Ground-based test facilities and planned space research facilities, as well as the nature of the commercialization activities, are briefly explained.

Modeling Czochralski growth of oxide crystals for piezoelectric and optical applications

NASA Astrophysics Data System (ADS)

Stelian, C.; Duffar, T.

2018-05-01

Numerical modeling is applied to investigate the impact of crystal and crucible rotation on the flow pattern and crystal-melt interface shape in Czochralski growth of oxide semi-transparent crystals used for piezoelectric and optical applications. Two cases are simulated in the present work: the growth of piezoelectric langatate (LGT) crystals of 3 cm in diameter in an inductive furnace, and the growth of sapphire crystals of 10 cm in diameter in a resistive configuration. The numerical results indicate that the interface shape depends essentially on the internal radiative heat exchanges in the semi-transparent crystals. Computations performed by applying crystal/crucible rotation show that the interface can be flattened during LGT growth, while flat-interface growth of large diameter sapphire crystals may not be possible.

Application of enthalpy model for floating zone silicon crystal growth

NASA Astrophysics Data System (ADS)

Krauze, A.; Bergfelds, K.; Virbulis, J.

2017-09-01

A 2D simplified crystal growth model based on the enthalpy method and coupled with a low-frequency harmonic electromagnetic model is developed to simulate the silicon crystal growth near the external triple point (ETP) and crystal melting on the open melting front of a polycrystalline feed rod in FZ crystal growth systems. Simulations of the crystal growth near the ETP show significant influence of the inhomogeneities of the EM power distribution on the crystal growth rate for a 4 in floating zone (FZ) system. The generated growth rate fluctuations are shown to be larger in the system with higher crystal pull rate. Simulations of crystal melting on the open melting front of the polycrystalline rod show the development of melt-filled grooves at the open melting front surface. The distance between the grooves is shown to grow with the increase of the skin-layer depth in the solid material.

Protein crystal growth in microgravity

NASA Technical Reports Server (NTRS)

Rosenblum, William M.; Delucas, Lawrence J.; Wilson, William W.

1989-01-01

Major advances have been made in several of the experimental aspects of protein crystallography, leaving protein crystallization as one of the few remaining bottlenecks. As a result, it has become important that the science of protein crystal growth is better understood and that improved methods for protein crystallization are developed. Preliminary experiments with both small molecules and proteins indicate that microgravity may beneficially affect crystal growth. For this reason, a series of protein crystal growth experiments using the Space Shuttle was initiated. The preliminary space experiments were used to evolve prototype hardware that will form the basis for a more advanced system that can be used to evaluate effects of gravity on protein crystal growth. Various optical techniques are being utilized to monitor the crystal growth process from the incipient or nucleation stage and throughout the growth phase. The eventual goal of these studies is to develop a system which utilizes optical monitoring for dynamic control of the crystallization process.

Protein crystal growth in a microgravity environment

NASA Technical Reports Server (NTRS)

Bugg, Charles E.

1988-01-01

Protein crystal growth is a major experimental problem and is the bottleneck in widespread applications of protein crystallography. Research efforts now being pursued and sponsored by NASA are making fundamental contributions to the understanding of the science of protein crystal growth. Microgravity environments offer the possibility of performing new types of experiments that may produce a better understanding of protein crystal growth processes and may permit growth environments that are more favorable for obtaining high quality protein crystals. A series of protein crystal growth experiments using the space shuttle was initiated. The first phase of these experiments was focused on the development of micro-methods for protein crystal growth by vapor diffusion techniques, using a space version of the hanging drop method. The preliminary space experiments were used to evolve prototype hardware that will form the basis for a more advanced system that can be used to evaluate effects of gravity on protein crystal growth.

Crystal growth, structure and morphology of hydrocortisone methanol solvate

NASA Astrophysics Data System (ADS)

Chen, Jianxin; Wang, Jiangkang; Zhang, Ying; Wu, Hong; Chen, Wei; Guo, Zhichao

2004-04-01

Hydrocortisone (HC), an important grucocorticoid, was crystallized from methanol solvent in the form of its methanol solvate. Its crystal structure belongs to orthorhombic, space group P2 12 12 1, with the unit cell parameters a=7.712(3) Å, b=14.392(5) Å, c=18.408(6) Å, Z=4. The methanol takes part in intermolecular hydrogen bonding, so if we change the solvent, the crystal habit of HC maybe different. The long parallelepiped morphology was also predicted by Cerius 2TM simulation program. The influence of intermolecular interaction was taken into account in the attachment energy model. The morphology calculation performed on the potential energy minimized model using a generic DREIDING 2.21 force field and developed minimization protocol with derived partial charges fits the experimental crystal shape well.

Kinetic Roughening Transition and Energetics of Tetragonal Lysozyme Crystal Growth

NASA Technical Reports Server (NTRS)

Gorti, Sridhar; Forsythe, Elizabeth L.; Pusey, Marc L.

2004-01-01

Interpretation of lysozyme crystal growth rates using well-established physical theories enabled the discovery of a phenomenon possibly indicative of kinetic roughening. For example, lysozyme crystals grown above a critical supersaturation sigma, (where supersaturation sigma = ln c/c(sub eq), c = the protein concentration and c(sub eq) = the solubility concentration) exhibit microscopically rough surfaces due to the continuous addition of growth units anywhere on the surface of a crystal. The rate of crystal growth, V(sub c), for the continuous growth process is determined by the continuous flux of macromolecules onto a unit area of the crystal surface, a, from a distance, xi, per unit time due to diffusion, and a probability of attachment onto the crystal surface, expressed. Based upon models applied, the energetics of lysozyme crystal growth was determined. The magnitudes of the energy barriers of crystal growth for both the (110) and (101) faces of tetragonal lysozyme crystals are compared. Finally, evidence supportive of the kinetic roughening hypothesis is presented.

Crystal growth in fused solvent systems

NASA Technical Reports Server (NTRS)

Ulrich, D. R.; Noone, M. J.; Spear, K. E.; White, W. B.; Henry, E. C.

1973-01-01

Research is reported on the growth of electronic ceramic single crystals from solution for the future growth of crystals in a microgravity environment. Work included growth from fused or glass solvents and aqueous solutions. Topics discussed include: crystal identification and selection; aqueous solution growth of triglycine sulphate (TGS); and characterization of TGS.

Phenytoin crystal growth rates in the presence of phosphate and chloride ions

NASA Astrophysics Data System (ADS)

Zipp, G. L.; Rodríguez-Hornedo, N.

1992-09-01

Phenytoin crystal growth kinetics have been measured as a function of supersaturation in pH 2.2 phosphoric acid and pH 2.2 hydrochloric acid solutions. Two different methods were used for the kinetic analysis. The first involved a zone-sensing device which provided an analysis of the distribution of crystals in a batch crystallizer. Crystal growth rates were calculated from the increase in the size of the distribution with time. In the second method, growth rates were evaluated from the change in size with time of individual crystals observed under an inverted microscope. The results from each method compare favorably. The use of both techniques provides an excellent opportunity to exploit the strengths of each: an average growth rate from a population of crystals from batch crystallization and insight into the effect of growth on the morphology of the crystals from the individual crystal measurements.

Inclusion free cadmium zinc tellurium and cadmium tellurium crystals and associated growth method

DOEpatents

Bolotnikov, Aleskey E [South Setauket, NY; James, Ralph B [Ridge, NY

2010-07-20

The present disclosure provides systems and methods for crystal growth of cadmium zinc tellurium (CZT) and cadmium tellurium (CdTe) crystals with an inverted growth reactor chamber. The inverted growth reactor chamber enables growth of single, large, high purity CZT and CdTe crystals that can be used, for example, in X-ray and gamma detection, substrates for infrared detectors, or the like. The inverted growth reactor chamber enables reductions in the presence of Te inclusions, which are recognized as an important limiting factor in using CZT or CdTe as radiation detectors. The inverted growth reactor chamber can be utilized with existing crystal growth techniques such as the Bridgman crystal growth mechanism and the like. In an exemplary embodiment, the inverted growth reactor chamber is a U-shaped ampoule.

Surface and bulk crystallization of amorphous solid water films: Confirmation of “top-down” crystallization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yuan, Chunqing; Smith, R. Scott; Kay, Bruce D.

2016-01-11

Here, the crystallization kinetics of nanoscale amorphous solid water (ASW) films are investigated using temperature-programmed desorption (TPD) and reflection absorption infrared spectroscopy (RAIRS). TPD measurements are used to probe surface crystallization and RAIRS measurements are used to probe bulk crystallization. Isothermal TPD results show that surface crystallization is independent of the film thickness (from 100 to 1000 ML). Conversely, the RAIRS measurements show that the bulk crystallization time increases linearly with increasing film thickness. These results suggest that nucleation and crystallization begin at the ASW/vacuum interface and then the crystallization growth front propagates linearly into the bulk. This mechanism wasmore » confirmed by selective placement of an isotopic layer (5% D 2O in H 2O) at various positions in an ASW (H 2O) film. In this case, the closer the isotopic layer was to the vacuum interface, the earlier the isotopic layer crystallized. These experiments provide direct evidence to confirm that ASW crystallization in vacuum proceeds by a “top-down” crystallization mechanism.« less

Fluid Physics and Macromolecular Crystal Growth in Microgravity

NASA Technical Reports Server (NTRS)

Pusey, M.; Snell, E.; Judge, R.; Chayen, N.; Boggon, T.

2000-01-01

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.

Measurable characteristics of lysozyme crystal growth

NASA Technical Reports Server (NTRS)

Gorti, Sridhar; Forsythe, Elizabeth L.; Pusey, Marc L.

2005-01-01

The behavior of protein crystal growth is estimated from measurements performed at both the microscopic and molecular levels. In the absence of solutal flow, it was determined that a model that balances the macromolecular flux toward the crystal surface with the flux of the crystal surface well characterizes crystal growth observed using microscopic methods. Namely, it was determined that the model provides accurate estimates for the crystal-growth velocities upon evaluation of crystal-growth measurements obtained in time. Growth velocities thus determined as a function of solution supersaturation were further interpreted using established deterministic models. From analyses of crystal-growth velocities, it was found that the mode of crystal growth varies with respect to increasing solution supersaturation, possibly owing to kinetic roughening. To verify further the hypothesis of kinetic roughening, crystal growth at the molecular level was examined using atomic force microscopy (AFM). From the AFM measurements, it was found that the magnitude of surface-height fluctuations, h(x), increases with increasing solution supersaturation. In contrast, the estimated characteristic length, xi, decreases rapidly upon increasing solution supersaturation. It was conjectured that the magnitude of both h(x) and xi could possibly determine the mode of crystal growth. Although the data precede any exact theory, the non-critical divergence of h(x) and xi with respect to increasing solution supersaturation was nevertheless preliminarily established. Moreover, approximate models to account for behavior of both h(x) and xi are also presented.

Crystal Growth Rate Dispersion: A Predictor of Crystal Quality in Microgravity?

NASA Technical Reports Server (NTRS)

Kephart, Richard D.; Judge, Russell A.; Snell, Edward H.; vanderWoerd, Mark J.

2003-01-01

In theory macromolecular crystals grow through a process involving at least two transport phenomena of solute to the crystal surface: diffusion and convection. In absence of standard gravitational forces, the ratio of these two phenomena can change and explain why crystal growth in microgravity is different from that on Earth. Experimental evidence clearly shows, however, that crystal growth of various systems is not equally sensitive to reduction in gravitational forces, leading to quality improvement in microgravity for some crystals but not for others. We hypothesize that the differences in final crystal quality are related to crystal growth rate dispersion. If growth rate dispersion exists on Earth, decreases in microgravity, and coincides with crystal quality improvements then this dispersion is a predictor for crystal quality improvement. In order to test this hypothesis, we will measure growth rate dispersion both in microgravity and on Earth and will correlate the data with previously established data on crystal quality differences for the two environments. We present here the first crystal growth rate measurement data for three proteins (lysozyme, xylose isomerase and human recombinant insulin), collected on Earth, using hardware identical to the hardware to be used in microgravity and show how these data correlate with crystal quality improvements established in microgravity.

On geological interpretations of crystal size distributions: Constant vs. proportionate growth

USGS Publications Warehouse

Eberl, D.D.; Kile, D.E.; Drits, V.A.

2002-01-01

Geological interpretations of crystal size distributions (CSDs) depend on understanding the crystal growth laws that generated the distributions. Most descriptions of crystal growth, including a population-balance modeling equation that is widely used in petrology, assume that crystal growth rates at any particular time are identical for all crystals, and, therefore, independent of crystal size. This type of growth under constant conditions can be modeled by adding a constant length to the diameter of each crystal for each time step. This growth equation is unlikely to be correct for most mineral systems because it neither generates nor maintains the shapes of lognormal CSDs, which are among the most common types of CSDs observed in rocks. In an alternative approach, size-dependent (proportionate) growth is modeled approximately by multiplying the size of each crystal by a factor, an operation that maintains CSD shape and variance, and which is in accord with calcite growth experiments. The latter growth law can be obtained during supply controlled growth using a modified version of the Law of Proportionate Effect (LPE), an equation that simulates the reaction path followed by a CSD shape as mean size increases.

Connection between the growth rate distribution and the size dependent crystal growth

NASA Astrophysics Data System (ADS)

Mitrović, M. M.; Žekić, A. A.; IIić, Z. Z.

2002-07-01

The results of investigations of the connection between the growth rate dispersions and the size dependent crystal growth of potassium dihydrogen phosphate (KDP), Rochelle salt (RS) and sodium chlorate (SC) are presented. A possible way out of the existing confusion in the size dependent crystal growth investigations is suggested. It is shown that the size independent growth exists if the crystals belonging to one growth rate distribution maximum are considered separately. The investigations suggest possible reason for the observed distribution maxima widths, and the high data scattering on the growth rate versus the crystal size dependence.

Effect of Low-Concentration Polymers on Crystal Growth in Molecular Glasses: A Controlling Role for Polymer Segmental Mobility Relative to Host Dynamics.

PubMed

Huang, Chengbin; Powell, C Travis; Sun, Ye; Cai, Ting; Yu, Lian

2017-03-02

Low-concentration polymers can strongly influence crystal growth in small-molecule glasses, a phenomenon important for improving physical stability against crystallization. We measured the velocity of crystal growth in two molecular glasses, nifedipine (NIF) and o-terphenyl (OTP), each doped with four or five different polymers. For each polymer, the concentration was fixed at 1 wt % and a wide range of molecular weights was tested. We find that a polymer additive can strongly alter the rate of crystal growth, from a 10-fold reduction to a 10-fold increase. For a given polymer, increasing molecular weight slows down crystal growth and the effect saturates around DP = 100, where DP is the degree of polymerization. For all the systems studied, the polymer effect on crystal growth rate forms a master curve in the variable (T g,polymer - T g,host )/T cryst , where T g is the glass transition temperature and T cryst is the crystallization temperature. These results support the view that a polymer's effect on crystal growth is controlled by its segmental mobility relative to the host-molecule dynamics. In the proposed model, crystal growth rejects impurities and creates local polymer-rich regions, which must be traversed by host molecules to sustain crystal growth at rates determined by polymer segmental mobility. Our results do not support the view that host-polymer hydrogen bonding plays a controlling role in crystal growth inhibition.

Protein crystal growth in low gravity

NASA Technical Reports Server (NTRS)

Feigelson, Robert S.

1990-01-01

The effect of low gravity on the growth of protein crystals and those parameters which will affect growth and crystal quality was studied. The proper design of the flight hardware and experimental protocols are highly dependent on understanding the factors which influence the nucleation and growth of crystals of biological macromolecules. Thus, those factors are investigated and the body of knowledge which has been built up for small molecule crystallization. These data also provide a basis of comparison for the results obtained from low-g experiments. The flows around growing crystals are detailed. The preliminary study of the growth of isocitrate lyase, the crystal morphologies found and the preliminary x ray results are discussed. The design of two apparatus for protein crystal growth by temperature control are presented along with preliminary results.

Microgravity

NASA Image and Video Library

1998-01-01

Dr. Daniel Carter, president of New Century Pharmaceuticals in Huntsville, Al, is one of three principal investigators in NASA's microgravity protein crystal growth program. Dr. Carter's experties is in albumins. Albumins are proteins in the bloodstream that transport materials, drugs, nutrients, and wastes. Photo credit: NASA/Marshall Space Flight Center

KSC-03pd1445

NASA Image and Video Library

2003-05-06

KENNEDY SPACE CENTER, FLA. - Dennis Morrison, senior biotech program scientist, talks to a reporter about an experiment recovered during the search for Columbia debris. He is the principle investigator on microencapsulation and urokinase crystal growth included in the Commercial ITA Biomedical Experiments payload on mission STS-107.

KSC-03pd1443

NASA Image and Video Library

2003-05-06

KENNEDY SPACE CENTER, FLA. - Dennis Morrison, senior biotech program scientist, talks to the media about an experiment recovered during the search for Columbia debris. He is the principle investigator on microencapsulation and urokinase crystal growth included in the Commercial ITA Biomedical Experiments payload on mission STS-107.

KSC-03pd1444

NASA Image and Video Library

2003-05-06

KENNEDY SPACE CENTER, FLA. - Dennis Morrison, senior biotech program scientist, talks to a reporter about an experiment recovered during the search for Columbia debris. He is the principle investigator on microencapsulation and urokinase crystal growth included in the Commercial ITA Biomedical Experiments payload on mission STS-107.

The study of single crystals for space processing and the effect of zero gravity

NASA Technical Reports Server (NTRS)

Lal, R. B.

1975-01-01

A study was undertaken to analyze different growth techniques affected by a space environment. Literature on crystal growth from melt, vapor phase and float zone was reviewed and the physical phenomena important for crystal growth in zero-gravity environment was analyzed. Recommendations for potential areas of crystal growth feasible for space missions are presented and a bibliography of articles in the area of crystal growth in general is listed.

Face-selective crystal growth behavior of L-aspartic acid in the presence of L-asparagine

NASA Astrophysics Data System (ADS)

Sato, Hiroyasu; Doki, Norihito; Yoshida, Saki; Yokota, Masaaki; Shimizu, Kenji

2016-02-01

The kinetic mechanism of L-asparagine (L-Asn) action on L-aspartic acid (L-Asp) crystal growth, namely the face-selective effect of L-Asn on the L-Asp crystal growth rate in each direction, was examined. In the a-axis direction, the effect of L-Asn on the L-Asp crystal growth rate was small. Enhancement and inhibition of L-Asp crystal growth, and interestingly the dissolution of the L-Asp crystal face, were observed in the b-axis direction, depending on the amount of L-Asn added. In the c-axis direction, the L-Asp crystal growth rate decreased with the increase in the amount of L-Asn added, and the experimental results were well fitted with a Langmuir adsorption isotherm. The study showed that there were crystal growth conditions where enhancement and inhibition, as well as inhibition and dissolution, coexisted in the presence of an additive with a structure similar to the growing crystal.

Delta L: An Apparatus for Measuring Macromolecular Crystal Growth Rates in Microgravity

NASA Technical Reports Server (NTRS)

Judge, Russell A.; Whitaker, Ann F. (Technical Monitor)

2001-01-01

In order to determine how macromolecule crystal quality improvement in microgravity is related to crystal growth characteristics, is was necessary to develop new hardware that could measure the crystal growth rates of a population of crystals growing under the same solution conditions. As crystal growth rate is defined as the change or delta in a defined dimension or length (L) of a crystal over time, the hardware was named Delta L. Delta L consists of fluids, optics, and data acquisition, sub-assemblies. Temperature control is provided for the crystal growth chamber. Delta L will be used in connection with the Glovebox Integrated Microgravity Isolation Technology (g-LIMIT) inside the Microgravity Science Glovebox (MSG), onboard the International Space Station (ISS). Delta L prototype hardware has been assembled. This paper will describe an overview of the design of Delta L and present preliminary crystal growth rate data.

Potential productivity benefits of float-zone versus Czochralski crystal growth

NASA Technical Reports Server (NTRS)

Abe, T.

1985-01-01

Efficient mass production of single-crystal silicon is necessary for the efficient silicon solar arrays needed in the coming decade. However, it is anticipated that there will be difficulty growing such volumes of crystals using conventional Czochralski (Cz) methods. While the productivity of single crystals might increase with a crystal diameter increase, there are two obstacles to the mass production of large diameter Czochralski crystals, the long production cycle due to slow growth rate and the high heat requirements of the furnaces. Also counterproductive would be the large resistivity gradient along the growth direction of the crystals due to impurity concentration. Comparison between Float zone (FZ) and Cz crystal growth on the basis of a crystal 150 mm in diameter is on an order of two to four times in favor of the FZ method. This advantage results from high growth rates and steady-state growth while maintaining a dislocation-free condition and impurity segregation.

Decades of Data: Extracting Trends from Microgravity Crystallization History

NASA Technical Reports Server (NTRS)

Judge, Russell A.; Snell, Edward H.; Kephart, Richard; vanderWoerd, Mark; Curreri, Peter A. (Technical Monitor)

2002-01-01

The reduced acceleration environment of an orbiting spacecraft has been posited as an ideal environment for biological crystal growth since buoyancy driven convection and sedimentation are greatly reduced. Since the first sounding rocket flight in 1981 many crystallization experiments have flown with some showing improvement and others not. To further explore macromolecule crystal improvement in microgravity we have accumulated data from published reports and reports submitted by individual investigators to NASA, forming a database called BIOSEArCH (Biological Space Experiment Archive of Crystallization History). To date it contains information from 63 missions including, the Space Shuttle program, unmanned satellites, the Russian Space Station MIR and sounding rocket experiments, containing reports for more than 736 macromolecule experiments. While it is not at this point in time a comprehensive record of all flight crystallization experimental results, there is however sufficient information for emerging trends to be identified. These trends will be highlighted.

1. Innovative Relaxor-Based PiezoCrystals: Phase Diagrams, Crystal Growth, Domain Structures and Electric Properties. 2. Piezo- and Ferroelectric Materials Based on Morphotropic Phase Boundary Synthesis, Characterization and Structure - Property Relations

DTIC Science & Technology

2006-03-31

crystals by the flux method and modified Bridgman technique, the growth results were hardly reproducible, and the quality of the crystals was still a serious... growth . 2.2.1.2.2) Solution Bridgman Growth A modified Bridgman method using excess of PbO as solvent was developed for the growth of PZNT91/9 crystals ...of growth , the grown crystal can be rotated via the A120 3 rod which was driven by a motor at a speed of 0 to 30 rmp. Figure 15(b) gives the

Study to Determine the Feasibility of Utilizing Skull-Melting Techniques for the Growth of Single Crystals of Yttrium Vanadate

DTIC Science & Technology

1986-04-01

these conditions and the sublimation product (IrO 2 ) contaminates the melt and resultant crystal. The goal of this program is to explore the...element; if the skull-melting operation is carried out under oxidizing conditions, the combustion products of high-purity graphite (CO 2 and CO) do not...polycrstalline ingots. Subsequent annealing of 16 S’ .1i" these 0 2 -defficient ingots in air at 1200 degrees C resulted in powdering and disintergration

Crystal Growth Furnace - An overview of the system configuration and planned experiments on the First United States Microgravity Laboratory mission

NASA Technical Reports Server (NTRS)

Srinivas, R.; Schaefer, D. A.

1992-01-01

The Crystal Growth Furnace (CGF) system configuration for the First United States Microgravity Laboratory (USML-1) mission is reviewed, and the planned on-orbit experiments are briefly described. The CGF is configured to accommodate four scientific experiments involving crystal growth which are based on the classical Bridgman method and CVT method, including vapor transport crystal growth of mercury cadmium telluride; crystal growth of mercury zinc telluride by directional solidification; seeded Bridgman growth of zinc-doped cadmium telluride; and Bridgman growth of selenium-doped gallium arsenide.

Optical Diagnostics of Solution Crystal Growth

NASA Technical Reports Server (NTRS)

Kim, Yongkee; Reddy, B. R.; George, T. G.; Lal, R. B.

1996-01-01

Non-contact optical techniques such as, optical heterodyne, ellipsometry and interferometry, for real time in-situ monitoring of solution crystal growth are demonstrated. Optical heterodyne technique has the capability of measuring the growth rate as small as 1A/sec. In a typical Michelson interferometer set up, the crystal is illuminated by a Zeeman laser with frequency omega(sub 1) and the reference beam with frequency omega(sub 2). As the crystal grows, the phase of the rf signal changes with respect to the reference beam and this phase change is related to the crystal growth rate. This technique is demonstrated with two examples: (1) by measuring the copper tip expansion/shrinkage rate and (2) by measuring the crystal growth rate of L-Arginine Phosphate (LAP). The first test shows that the expansion/shrinkage rate of copper tip was fast in the beginning, and gets slower as the expansion begins to stabilize with time. In crystal growth, the phase change due the crystal growth is measured using a phase meter and a strip chart recorder. Our experimental results indicate a varied growth rate from 69.4 to 92.6A per sec. The ellipsometer is used to study the crystal growth interface. From these measurements and a theoretical modeling of the interface, the various optical parameters can be deduced. Interferometry can also be used to measure the growth rate and concentration gradient in the vicinity of the crystal.

Programmable and coherent crystallization of semiconductors

PubMed Central

Yu, Liyang; Niazi, Muhammad R.; Ngongang Ndjawa, Guy O.; Li, Ruipeng; Kirmani, Ahmad R.; Munir, Rahim; Balawi, Ahmed H.; Laquai, Frédéric; Amassian, Aram

2017-01-01

The functional properties and technological utility of polycrystalline materials are largely determined by the structure, geometry, and spatial distribution of their multitude of crystals. However, crystallization is seeded through stochastic and incoherent nucleation events, limiting the ability to control or pattern the microstructure, texture, and functional properties of polycrystalline materials. We present a universal approach that can program the microstructure of materials through the coherent seeding of otherwise stochastic homogeneous nucleation events. The method relies on creating topographic variations to seed nucleation and growth at designated locations while delaying nucleation elsewhere. Each seed can thus produce a coherent growth front of crystallization with a geometry designated by the shape and arrangement of seeds. Periodic and aperiodic crystalline arrays of functional materials, such as semiconductors, can thus be created on demand and with unprecedented sophistication and ease by patterning the location and shape of the seeds. This approach is used to demonstrate printed arrays of organic thin-film transistors with remarkable performance and reproducibility owing to their demonstrated spatial control over the microstructure of organic and inorganic polycrystalline semiconductors. PMID:28275737

Hopper Growth of Salt Crystals.

PubMed

Desarnaud, Julie; Derluyn, Hannelore; Carmeliet, Jan; Bonn, Daniel; Shahidzadeh, Noushine

2018-06-07

The growth of hopper crystals is observed for many substances, but the mechanism of their formation remains ill understood. Here we investigate their growth by performing evaporation experiments on small volumes of salt solutions. We show that sodium chloride crystals that grow very fast from a highly supersaturated solution form a peculiar form of hopper crystal consisting of a series of connected miniature versions of the original cubic crystal. The transition between cubic and such hopper growth happens at a well-defined supersaturation where the growth rate of the cubic crystal reaches a maximum (∼6.5 ± 1.8 μm/s). Above this threshold, the growth rate varies as the third power of supersaturation, showing that a new mechanism, controlled by the maximum speed of surface integration of new molecules, induces the hopper growth of cubic crystals in cascade.

A study of crystal growth by solution technique. [triglycine sulfate single crystals

NASA Technical Reports Server (NTRS)

Lal, R. B.

1979-01-01

The advantages and mechanisms of crystal growth from solution are discussed as well as the effects of impurity adsorption on the kinetics of crystal growth. Uncertainities regarding crystal growth in a low gravity environment are examined. Single crystals of triglycine sulfate were grown using a low temperature solution technique. Small components were assembled and fabricated for future space flights. A space processing experiment proposal accepted by NASA for the Spacelab-3 mission is included.

Dr. Daniel Carter

NASA Technical Reports Server (NTRS)

1998-01-01

Dr. Daniel Carter, president of New Century Pharmaceuticals in Huntsville, Al, is one of three principal investigators in NASA's microgravity protein crystal growth program. Dr. Carter's experties is in albumins. Albumins are proteins in the bloodstream that transport materials, drugs, nutrients, and wastes. Photo credit: NASA/Marshall Space Flight Center

Effect of precipitation inhibitors on indomethacin supersaturation maintenance: mechanisms and modeling.

PubMed

Patel, Dhaval D; Anderson, Bradley D

2014-05-05

This study quantitatively explores the mechanisms underpinning the effects of model pharmaceutical polymeric precipitation inhibitors (PPIs) on the crystal growth and, in turn, maintenance of supersaturation of indomethacin, a model poorly water-soluble drug. A recently developed second-derivative UV spectroscopy method and a first-order empirical crystal growth model were used to determine indomethacin crystal growth rates in the presence of model PPIs. All three model PPIs including HP-β-CD, PVP, and HPMC inhibited indomethacin crystal growth at both high and low degrees of supersaturation (S). The bulk viscosity changes in the presence of model PPIs could not explain their crystal growth inhibitory effects. At 0.05% w/w, PVP (133-fold) and HPMC (28-fold) were better crystal growth inhibitors than HP-β-CD at high S. The inhibitory effect of HP-β-CD on the bulk diffusion-controlled indomethacin crystal growth at high S was successfully modeled using reactive diffusion layer theory, which assumes reversible complexation in the diffusion layer. Although HP-β-CD only modestly inhibited indomethacin crystal growth at either high S (∼15%) or low S (∼2-fold), the crystal growth inhibitory effects of PVP and HPMC were more dramatic, particularly at high S (0.05% w/w). The superior crystal growth inhibitory effects of PVP and HPMC as compared with HP-β-CD at high S were attributed to a change in the indomethacin crystal growth rate-limiting step from bulk diffusion to surface integration. Indomethacin crystal growth inhibitory effects of all three model PPIs at low S were attributed to retardation of the rate of surface integration of indomethacin, a phenomenon that may reflect the adsorption of PPIs onto the growing crystal surface. The quantitative approaches outlined in this study should be useful in future studies to develop tools to predict supersaturation maintenance effects of PPIs.

Segregation control in vertical Bridgman crystal growth

NASA Astrophysics Data System (ADS)

Tao, Y.; Kou, S.

1996-11-01

To help the crystal grow at a constant dopant concentration in vertical Bridgman crystal growth, the dopant concentration of the growth melt, i.e. the melt from which the crystal grows, was kept constant. To achieve this, three different methods were used to replenish the growth melt at a controlled rate and suppress dopant diffusion between the growth melt and the replenishing melt. In method one, a replenishing crucible having a long melt passageway was immersed in the growth melt. In method two, a replenishing crucible having an independent feed-rate control mechanism was held above the growth melt. In method three, a submerged diffusion baffle was used to form a long melt passageway between the growth melt and the replenishing melt. NaNO 3 was used as a model material for crystal growth. Single crystals were grown by these three methods with effective segregation control. Method two was applied to InSb and single crystals were also grown with effective segregation control.

Control of heat transfer in continuous-feeding Czochralski-silicon crystal growth with a water-cooled jacket

NASA Astrophysics Data System (ADS)

Zhao, Wenhan; Liu, Lijun

2017-01-01

The continuous-feeding Czochralski method is an effective method to reduce the cost of single crystal silicon. By promoting the crystal growth rate, the cost can be reduced further. However, more latent heat will be released at the melt-crystal interface under a high crystal growth rate. In this study, a water-cooled jacket was applied to enhance the heat transfer at the melt-crystal interface. Quasi-steady-state numerical calculation was employed to investigate the impact of the water-cooled jacket on the heat transfer at the melt-crystal interface. Latent heat released during the crystal growth process at the melt-crystal interface and absorbed during feedstock melting at the feeding zone was modeled in the simulations. The results show that, by using the water-cooled jacket, heat transfer in the growing crystal is enhanced significantly. Melt-crystal interface deflection and thermal stress increase simultaneously due to the increase of radial temperature at the melt-crystal interface. With a modified heat shield design, heat transfer at the melt-crystal interface is well controlled. The crystal growth rate can be increased by 20%.

Bridgman growth of large-aperture yttrium calcium oxyborate crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wu, Anhua, E-mail: wuanhua@mail.sic.ac.cn; Jiang, Linwen; Qian, Guoxing

2012-09-15

Highlights: ► YCOB is a novel non-linear optical crystal possessing good thermal, mechanical and nonlinear optical properties. ► Large size crystal growth is key technology question for YCOB crystal. ► YCOB crystals 3 in. in diameter were grown with modified vertical Bridgman method. ► It is a more effective growth method to obtain large size and high quality YCOB crystal. -- Abstract: Large-aperture yttrium calcium oxyborate YCa{sub 4}O(BO{sub 3}){sub 3} (YCOB) crystals with 3 in. in diameter were grown with modified vertical Bridgman method, and the large crystal plate (63 mm × 68 mm × 20 mm) was harvested formore » high-average power frequency conversion system. The crack, facet growth and spiral growth can be effectively controlled in the as-grown crystal, and Bridgman method displays more effective in obtain large size and high quality YCOB crystal plate than Czochralski technique.« less

High purity low dislocation GaAs single crystals

NASA Technical Reports Server (NTRS)

Chen, R. T.; Holmes, D. E.; Kirkpatrick, C. G.

1982-01-01

Recent advances in GaAs bulk crystal growth using the LEC (liquid encapsulated Czochralski) technique are described. The dependence of the background impurity concentration and the dislocation density distribution on the materials synthesis and growth conditions were investigated. Background impurity concentrations as low as 4 x 10 to the 15th power were observed in undoped LEC GaAs. The dislocation density in selected regions of individual ingots was very low, below the 3000 cm .3000/sq cm threshold. The average dislocation density over a large annular ring on the wafers fell below the 10000/sq cm level for 3 inch diameter ingots. The diameter control during the program advanced to a diameter variation along a 3 inch ingot less than 2 mm.

Crystal growth and annealing for minimized residual stress

DOEpatents

Gianoulakis, Steven E.

2002-01-01

A method and apparatus for producing crystals that minimizes birefringence even at large crystal sizes, and is suitable for production of CaF.sub.2 crystals. The method of the present invention comprises annealing a crystal by maintaining a minimal temperature gradient in the crystal while slowly reducing the bulk temperature of the crystal. An apparatus according to the present invention includes a thermal control system added to a crystal growth and annealing apparatus, wherein the thermal control system allows a temperature gradient during crystal growth but minimizes the temperature gradient during crystal annealing.

An assessment of calcite crystal growth mechanisms based on crystal size distributions

USGS Publications Warehouse

Kile, D.E.; Eberl, D.D.; Hoch, A.R.; Reddy, M.M.

2000-01-01

Calcite crystal growth experiments were undertaken to test a recently proposed model that relates crystal growth mechanisms to the shapes of crystal size distributions (CSDs). According to this approach, CSDs for minerals have three basic shapes: (1) asymptotic, which is related to a crystal growth mechanism having constant-rate nucleation accompanied by surface-controlled growth; (2) lognormal, which results from decaying-rate nucleation accompanied by surface-controlled growth; and (3) a theoretical, universal, steady-state curve attributed to Ostwald ripening. In addition, there is a fourth crystal growth mechanism that does not have a specific CSD shape, but which preserves the relative shapes of previously formed CSDs. This mechanism is attributed to supply-controlled growth. All three shapes were produced experimentally in the calcite growth experiments by modifying nucleation conditions and solution concentrations. The asymptotic CSD formed when additional reactants were added stepwise to the surface of solutions that were supersaturated with respect to calcite (initial Ω = 20, where Ω = 1 represents saturation), thereby leading to the continuous nucleation and growth of calcite crystals. Lognormal CSDs resulted when reactants were added continuously below the solution surface, via a submerged tube, to similarly supersaturated solutions (initial Ω = 22 to 41), thereby leading to a single nucleation event followed by surface-controlled growth. The Ostwald CSD resulted when concentrated reactants were rapidly mixed, leading initially to high levels of supersaturation (Ω >100), and to the formation and subsequent dissolution of very small nuclei, thereby yielding CSDs having small crystal size variances. The three CSD shapes likely were produced early in the crystallization process, in the nanometer crystal size range, and preserved during subsequent growth. Preservation of the relative shapes of the CSDs indicates that a supply-controlled growth mechanism was established and maintained during the constant-composition experiments. CSDs having shapes intermediate between lognormal and Ostwald also were generated by varying the initial levels of supersaturation (initial Ω = 28.2 to 69.2) in rapidly mixed solutions. Lognormal CSDs were observed for natural calcite crystals that are found in septarian concretions occurring in southeastern Colorado. Based on the model described above, these CSDs indicate initial growth by surface control, followed by supply-controlled growth. Thus, CSDs may be used to deduce crystal growth mechanisms from which geologic conditions early in the growth history of a mineral can be inferred. Conversely, CSD shape can be predicted during industrial crystallization by applying the appropriate conditions for a particular growth mechanism.

A Simple Inexpensive Bridgman-Stockbarger Crystal Growth System for Organic Materials

NASA Technical Reports Server (NTRS)

Choi, J.; Aggarwal, M. D.; Wang, W. S.; Metzl, R.; Bhat, K.; Penn, Benjamin G.; Frazier, Donald O.

1996-01-01

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.

In situ study of the growth and degradation processes in tetragonal lysozyme crystals on a silicon substrate by high-resolution X-ray diffractometry

NASA Astrophysics Data System (ADS)

Kovalchuk, M. V.; Prosekov, P. A.; Marchenkova, M. A.; Blagov, A. E.; D'yakova, Yu. A.; Tereshchenko, E. Yu.; Pisarevskii, Yu. V.; Kondratev, O. A.

2014-09-01

The results of an in situ study of the growth of tetragonal lysozyme crystals by high-resolution X-ray diffractometry are considered. The crystals are grown by the sitting-drop method on crystalline silicon substrates of different types: both on smooth substrates and substrates with artificial surface-relief structures using graphoepitaxy. The crystals are grown in a special hermetically closed crystallization cell, which enables one to obtain images with an optical microscope and perform in situ X-ray diffraction studies in the course of crystal growth. Measurements for lysozyme crystals were carried out in different stages of the crystallization process, including crystal nucleation and growth, developed crystals, the degradation of the crystal structure, and complete destruction.

Three dimensional modeling of cirrus during the 1991 FIRE IFO 2: Detailed process study

NASA Technical Reports Server (NTRS)

Jensen, Eric J.; Toon, Owen B.; Westphal, Douglas L.

1993-01-01

A three-dimensional model of cirrus cloud formation and evolution, including microphysical, dynamical, and radiative processes, was used to simulate cirrus observed in the FIRE Phase 2 Cirrus field program (13 Nov. - 7 Dec. 1991). Sulfate aerosols, solution drops, ice crystals, and water vapor are all treated as interactive elements in the model. Ice crystal size distributions are fully resolved based on calculations of homogeneous freezing of solution drops, growth by water vapor deposition, evaporation, aggregation, and vertical transport. Visible and infrared radiative fluxes, and radiative heating rates are calculated using the two-stream algorithm described by Toon et al. Wind velocities, diffusion coefficients, and temperatures were taken from the MAPS analyses and the MM4 mesoscale model simulations. Within the model, moisture is transported and converted to liquid or vapor by the microphysical processes. The simulated cloud bulk and microphysical properties are shown in detail for the Nov. 26 and Dec. 5 case studies. Comparisons with lidar, radar, and in situ data are used to determine how well the simulations reproduced the observed cirrus. The roles played by various processes in the model are described in detail. The potential modes of nucleation are evaluated, and the importance of small-scale variations in temperature and humidity are discussed. The importance of competing ice crystal growth mechanisms (water vapor deposition and aggregation) are evaluated based on model simulations. Finally, the importance of ice crystal shape for crystal growth and vertical transport of ice are discussed.

The control of ice crystal growth and effect on porous structure of konjac glucomannan-based aerogels.

PubMed

Ni, Xuewen; Ke, Fan; Xiao, Man; Wu, Kao; Kuang, Ying; Corke, Harold; Jiang, Fatang

2016-11-01

Konjac glucomannan (KGM)-based aerogels were prepared using a combination of sol-gel and freeze-drying methods. Preparation conditions were chosen to control ice crystal growth and aerogel structure formation. The ice crystals formed during pre-freezing were observed by low temperature polarizing microscopy, and images of aerogel pores were obtained by scanning electron microscopy. The size of ice crystals were calculated and size distribution maps were drawn, and similarly for aerogel pores. Results showed that ice crystal growth and aerogel pore sizes may be controlled by varying pre-freezing temperatures, KGM concentration and glyceryl monostearate concentration. The impact of pre-freezing temperatures on ice crystal growth was explained as combining ice crystal growth rate with nucleation rate, while the impacts of KGM and glyceryl monostearate concentration on ice crystal growth were interpreted based on their influences on sol network structure. Copyright © 2016 Elsevier B.V. All rights reserved.

Development and melt growth of novel scintillating halide crystals

NASA Astrophysics Data System (ADS)

Yoshikawa, Akira; Yokota, Yuui; Shoji, Yasuhiro; Kral, Robert; Kamada, Kei; Kurosawa, Shunsuke; Ohashi, Yuji; Arakawa, Mototaka; Chani, Valery I.; Kochurikhin, Vladimir V.; Yamaji, Akihiro; Andrey, Medvedev; Nikl, Martin

2017-12-01

Melt growth of scintillating halide crystals is reviewed. The vertical Bridgman growth technique is still considered as very popular method that enables production of relatively large and commercially attractive crystals. On the other hand, the micro-pulling-down method is preferable when fabrication of small samples, sufficient for preliminary characterization of their optical and/or scintillation performance, is required. Moreover, bulk crystal growth is also available using the micro-pulling-down furnace. The examples of growths of various halide crystals by industrially friendly melt growth techniques including Czochralski and edge-defined film-fed growth methods are also discussed. Finally, traveling molten zone growth that in some degree corresponds to horizontal zone melting is briefly overviewed.

Growth of benzil crystals by vertical dynamic gradient freeze technique in a transparent furnace

NASA Astrophysics Data System (ADS)

Lan, C. W.; Song, C. R.

1997-09-01

The vertical dynamic gradient freeze technique using a transparent furnace was applied to the growth of benzil single crystals. A flat-bottom ampoule with a <0001> seed was used for growth. During crystal growth, dynamic heating profiles were controlled through a computer, and the growth interface was recorded by a CCD camera. Computer simulation was also conducted, and the calculated convex interface and dynamic growth rate were consistent with the observed ones for various growth conditions. Conditions for growing single crystals were also determined, and they were mainly limited by constitutional supercooling. As the grown crystals were clear in appearance, their optical absorption spectra were insensitive to growth conditions and post-annealing.

Protein crystal growth tray assembly

NASA Technical Reports Server (NTRS)

Carter, Daniel C. (Inventor); Miller, Teresa Y. (Inventor)

1992-01-01

A protein crystal growth tray assembly includes a tray that has a plurality of individual crystal growth chambers. Each chamber has a movable pedestal which carries a protein crystal growth compartment at an upper end. The several pedestals for each tray assembly are ganged together for concurrent movement so that the solutions in the various pedestal growth compartments can be separated from the solutions in the tray's growth chambers until the experiment is to be activated.

Rate limits in silicon sheet growth - The connections between vertical and horizontal methods

NASA Technical Reports Server (NTRS)

Thomas, Paul D.; Brown, Robert A.

1987-01-01

Meniscus-defined techniques for the growth of thin silicon sheets fall into two categories: vertical and horizontal growth. The interactions of the temperature field and the crystal shape are analyzed for both methods using two-dimensional finite-element models which include heat transfer and capillarity. Heat transfer in vertical growth systems is dominated by conduction in the melt and the crystal, with almost flat melt/crystal interfaces that are perpendicular to the direction of growth. The high axial temperature gradients characteristic of vertical growth lead to high thermal stresses. The maximum growth rate is also limited by capillarity which can restrict the conduction of heat from the melt into the crystal. In horizontal growth the melt/crystal interface stretches across the surface of the melt pool many times the crystal thickness, and low growth rates are achievable with careful temperature control. With a moderate axial temperature gradient in the sheet a substantial portion of the latent heat conducts along the sheet and the surface of the melt pool becomes supercooled, leading to dendritic growth. The thermal supercooling is surpressed by lowering the axial gradient in the crystal; this configuration is the most desirable for the growth of high quality crystals. An expression derived from scaling analysis relating the growth rate and the crucible temperature is shown to be reliable for horizontal growth.

Growth Kinetics and Morphology of Barite Crystals Derived from Face-Specific Growth Rates

DOE PAGES

Godinho, Jose R. A.; Stack, Andrew G.

2015-03-30

Here we investigate the growth kinetics and morphology of barite (BaSO 4) crystals by measuring the growth rates of the (001), (210), (010), and (100) surfaces using vertical scanning interferometry. Solutions with saturation indices 1.1, 2.1, and 3.0 without additional electrolyte, in 0.7 M NaCl, or in 1.3 mM SrCl2 are investigated. Face-specific growth rates are inhibited in the SrCl 2 solution relative to a solution without electrolyte, except for (100). Contrarily, growth of all faces is promoted in the NaCl solution. The variation of face-specific rates is solution-specific, which leads to a. change of the crystal morphology and overallmore » growth rate of crystals. The measured face-specific growth rates are used to model the growth of single crystals. Modeled crystals have a morphology and size similar to those grown from solution. Based on the model the time dependence of surface area and growth rates is analyzed. Growth rates change with time due to surface area normalization for small crystals and large growth intervals. By extrapolating rates to crystals with large surfaces areas, time-independent growth rates are 0.783, 2.96, and 0.513 mmol∙m -2∙h -1, for saturation index 2.1 solutions without additional electrolyte, NaCl, and SrCl 2, respectively.« less

Growth Kinetics and Morphology of Barite Crystals Derived from Face-Specific Growth Rates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Godinho, Jose R. A.; Stack, Andrew G.

Here we investigate the growth kinetics and morphology of barite (BaSO 4) crystals by measuring the growth rates of the (001), (210), (010), and (100) surfaces using vertical scanning interferometry. Solutions with saturation indices 1.1, 2.1, and 3.0 without additional electrolyte, in 0.7 M NaCl, or in 1.3 mM SrCl2 are investigated. Face-specific growth rates are inhibited in the SrCl 2 solution relative to a solution without electrolyte, except for (100). Contrarily, growth of all faces is promoted in the NaCl solution. The variation of face-specific rates is solution-specific, which leads to a. change of the crystal morphology and overallmore » growth rate of crystals. The measured face-specific growth rates are used to model the growth of single crystals. Modeled crystals have a morphology and size similar to those grown from solution. Based on the model the time dependence of surface area and growth rates is analyzed. Growth rates change with time due to surface area normalization for small crystals and large growth intervals. By extrapolating rates to crystals with large surfaces areas, time-independent growth rates are 0.783, 2.96, and 0.513 mmol∙m -2∙h -1, for saturation index 2.1 solutions without additional electrolyte, NaCl, and SrCl 2, respectively.« less

Unidirectional growth of benzil crystal from solution by Sankaranarayanan-Ramasamy method and its characterization

NASA Astrophysics Data System (ADS)

Rajalakshmi, M.; Shyju, T. S.; Indirajith, R.; Gopalakrishnan, R.

2012-02-01

Good quality <1 0 0> benzil single crystal with a diameter 18 mm and length 75 mm was successfully grown from solution by the unidirectional growth method of Sankaranarayanan-Ramasamy (SR) for the first time in the literature. The seed crystals have been harvested from conventional solution growth technique and subsequently used for unidirectional growth. The grown crystal was subjected to various characterization studies. The results of UV-vis spectral analysis, photoluminescence, etching and microhardness studies were compared with conventional solution grown crystal to that of SR method grown crystal. The quality of SR method grown benzil crystal is better than conventional solution grown crystal.

Fast growth of n-type 4H-SiC bulk crystal by gas-source method

NASA Astrophysics Data System (ADS)

Hoshino, Norihiro; Kamata, Isaho; Tokuda, Yuichiro; Makino, Emi; Kanda, Takahiro; Sugiyama, Naohiro; Kuno, Hironari; Kojima, Jun; Tsuchida, Hidekazu

2017-11-01

Fast growth of n-type 4H-SiC crystals was attempted using a high-temperature gas-source method. High growth rates exceeding 9 mm/h were archived at a seed temperature of 2550 °C, although the formation of macro-step bunching caused doping fluctuation and voids in the grown crystal. We investigated a trade-off between growth-rate enhancement and macro-step formation and how to improve the trade-off. By controlling the growth conditions, the growth of highly nitrogen-doped 4H-SiC crystals without the doping fluctuation and void formation were accomplished under a high growth rate exceeding 3 mm/h, maintaining the density of threading screw dislocations in the same level with the seed crystal. The influence of growth parameters on nitrogen incorporations into grown crystals was also surveyed.

Maintenance of supersaturation I: indomethacin crystal growth kinetic modeling using an online second-derivative ultraviolet spectroscopic method.

PubMed

Patel, Dhaval D; Joguparthi, Vijay; Wang, Zeren; Anderson, Bradley D

2011-07-01

Formulations that produce supersaturated solutions after their oral administration have received increased attention as a means to improve bioavailability of poorly water-soluble drugs. Although it is widely recognized that excipients can prolong supersaturation, the mechanisms by which these beneficial effects are realized are generally unknown. Difficulties in separately measuring the kinetics of nucleation and crystal growth have limited progress in understanding the mechanisms by which excipients contribute to the supersaturation maintenance. This paper describes the crystal growth kinetic modeling of indomethacin, a poorly water-soluble drug, from supersaturated aqueous suspensions using a newly developed, online second-derivative ultraviolet spectroscopic method. The apparent indomethacin equilibrium solubility after crystal growth at a high degree of supersaturation (S=6) was approximately 55% higher than the indomethacin equilibrium solubility determined prior to growth, which was attributed to the deposition of a higher energy indomethacin form on the seed crystals. The indomethacin crystal growth kinetics (S=6) was of first order. By comparing the mass transfer coefficients from indomethacin dissolution and crystal growth, it was shown that the indomethacin crystal growth kinetics at S=6 was bulk diffusion controlled. The change in indomethacin seed crystal size distribution before and after crystal growth was determined and modeled using a mass-balance relationship. Copyright © 2011 Wiley-Liss, Inc. and the American Pharmacists Association

Crystal growth mechanisms in miarolitic cavities in the Lake George ring complex and vicinity, Colorado

USGS Publications Warehouse

Kile, D.E.; Eberl, D.D.

1999-01-01

The Crystal Peak area of the Pikes Peak batholith, near Lake George in central Colorado, is world-renowned for its crystals of amazonite (the blue-green variety of microcline) and smoky quartz. Such crystals, collected from individual miarolitic pegmatites, have a remakably small variation in crystal size within each pegmatite, and the shapes of plots of their crystal size distributions (CSDs) are invariably lognormal or close to lognormal in all cases. These observations are explained by a crystal growth mechanism that was governed initially by surface-controlled kinetics, during which crystals tended to grow larger in proportion to their size, thereby establishing lognormal CSDs. Surface-controlled growth was followed by longer periods of supply controlled growth, during which growth rate was predominantly size-independent, consequently preserving the lognormal shapes of the CSDs and the small size variation. The change from surface- to supply controlled growth kinetics may have resulted from an increasing demand for nutrients that exceeded diffusion limitations of the system. The proposed model for crystal growth in this locality appears to be common in the geologic record, and can be used with other information, such as isotopic data, to deduce physico-chemical conditions during crystal formation.

Calculation Of Clinopyroxene And Olivine Growth Rates Using Plagioclase Residence Time

NASA Astrophysics Data System (ADS)

Kilinc, A. I.; Borell, A.; Leu, A.

2012-12-01

According to the Crystal Size Distribution theory (CSD) in a plot of logarithm of number of crystals of a given size range per unit volume [ln(n)], against crystal size [L] shows a straight line. Slope of that line is given by where is the crystal residence time and G is the crystal growth rate. Therefore if is known then G can be calculated. We used thin sections of the Kilauea basalt from Hawaii where olivine, clinopyroxene and plagioclase crystallized within a small temperature range, and the crystal growth rate of plagioclase is known. Assuming that crystal residence times of these three minerals are the same, we plotted ln(n) against L and using the slope and the known crystal growth rate of plagioclase we calculated the crystal growth rates of clinopyroxene and olivine. For the clinopyroxene growth rate we report 10-10.9cm/sec, which is in good agreement with Congdon's data of 10-10 cm/sec. We also calculated the growth rate of olivine is a basaltic melt as 10-8.5 cm/sec which is comparable to < 10-10 to 10-7 cm/sec given by Donaldson and Jambon.

Protein Crystal Growth With the Aid of Microfluidics

NASA Technical Reports Server (NTRS)

vanderWoerd, Mark

2003-01-01

Protein crystallography is one of three well-known methods to obtain the structure of proteins. A major rate limiting step in protein crystallography is protein crystal nucleation and growth, which is still largely a process conducted by trial-and-error methods. Many attempts have been made to improve protein crystal growth by performing growth in microgravity. Although the use of microgravity appears to improve crystal quality in some attempts, this method has been inefficient because several reasons: we lack a fundamental understanding of macromolecular crystal growth in general and of the influence of microgravity in particular, we have to start with crystal growth conditions in microgravity based on conditions on the ground and finally the hardware does not allow for experimental iteration without reloading samples on the ground. To partially accommodate the disadvantages of the current hardware, we have used microfluidic technology (Lab-on-a-Chip devices) to design the concept of a more efficient crystallization device, suitable for use on the International Space Station and in high-throughput applications on the ground. The concept and properties of microfluidics, the application design process, and the advances in protein crystal growth hardware will be discussed in this presentation. Some examples of proteins crystallized in the new hardware will be discussed, including the differences between conventional crystallization versus crystallization in microfluidics.

Liquid encapsulated crystal growth

NASA Technical Reports Server (NTRS)

Morrison, Andrew D. (Inventor)

1989-01-01

Low-defect crystals are grown in a closed ampoule under a layer of encapsulant. After crystal growth, the crystal is separated from the melt and moved into the layer of encapsulant and cooled to a first temperature at which crystal growth stops. The crystal is then moved into the inert gas ambient in the ampoule and further cooled. The crystal can be separated from the melt by decanting the melt into an adjacent reservoir or by rotating the ampoule to rotate the crystal into the encapsulant layer.

Liquid encapsulated crystal growth

NASA Technical Reports Server (NTRS)

Morrison, Andrew D. (Inventor)

1987-01-01

Low-defect crystals are grown in a closed ampoule under a layer of encapsulant. After crystal growth, the crystal is separated from the melt and moved into the layer of encapsulant and cooled to a first temperature at which crystal growth stops. The crystal is then moved into the inert gas ambient in the ampoule and further cooled. The crystal can be separated from the melt by decanting the melt into and adjacent reservoir or by rotating the ampoule to rotate the crystal into the encapsulant layer.

Using Strong Magnetic Fields to Control Solutal Convection

NASA Technical Reports Server (NTRS)

Ramachandran, N.; Leslie, F. W.

2003-01-01

An important component in biotechnology, particularly in the area of protein engineering and rational drug design is the knowledge of the precise three-dimensional molecular structure of proteins. The quality of structural information obtained from X-ray diffraction methods is directly dependent on the degree of perfection of the protein crystals. As a consequence, the growth of high quality macromolecular crystals for diffraction analyses has been the central focus for biochemists, biologists, and bioengineers. Macromolecular crystals are obtained from solutions that contain the crystallizing species in equilibrium with higher aggregates, ions, precipitants, other possible phases of the protein, foreign particles, the walls of the container, and a likely host of other impurities. By changing transport modes in general, i.e., reduction of convection and sedimentation, as is achieved in microgravity , we have been able to dramatically affect the movement and distribution of macromolecules in the fluid, and thus their transport, formation of crystal nuclei, and adsorption to the crystal surface. While a limited number of high quality crystals from space flights have been obtained, as the recent National Research Council (NRC) review of the NASA microgravity crystallization program pointed out, the scientific approach and research in crystallization of proteins has been mainly empirical yielding inconclusive results. We postulate that we can reduce convection in ground-based experiments and we can understand the different aspects of convection control through the use of strong magnetic fields and field gradients. We postulate that limited convection in a magnetic field will provide the environment for the growth of high quality crystals. The approach exploits the variation of fluid magnetic susceptibility with concentration for this purpose and the convective damping is realized by appropriately positioning the crystal growth cell so that the magnetic susceptibility force counteracts terrestrial gravity. The general objective is to test the hypothesis of convective control using a strong magnetic field and magnetic field gradient and to understand the nature of the various forces that come into play. Specifically we aim to delineate causative factors and to quantify them through experiments, analysis and numerical modeling. The paper will report on the experimental results using paramagnetic salts and solutions in magnetic fields and compare them to analytical predictions.

Countering Solutal Buoyant Convection with High Magnetic Fields

NASA Technical Reports Server (NTRS)

Ramachandran, N.; Leslie, F. W.

2002-01-01

An important component in biotechnology, particularly in the area of protein engineering and rational drug design is the knowledge of the precise three-dimensional molecular structure of proteins. The quality of structural information obtained from X-ray diffraction methods is directly dependent on the degree of perfection of the protein crystals. As a consequence, the growth of high quality macromolecular crystals for diffraction analyses has been the central focus for biochemist, biologists, and bioengineers. Macromolecular crystals are obtained from solutions that contain the crystallizing species in equilibrium with higher aggregates, ions, precipitant, other possible phases of the protein, foreign particles, the walls of the container, and a likely host of other impurities. By changing transport modes in general, i.e., reduction of convection and sedimentation, as is achieved in microgravity, we have been able to dramatically effect the movement and distribution of macromolecules in the fluid, and thus their transport, formation of crystal nuclei, and adsorption to the crystal surface. While a limited number of high quality crystals from space flights have been obtained, as the recent National Research Council (NRC) review of the NASA microgravity crystallization program pointed out, the scientific approach and research in crystallization of proteins has been mainly empirical yielding inconclusive results. We postulate that we can reduce convection in ground-based experiments and we can understand the different aspects of convection control through the use of strong magnetic fields and field gradients. We postulate that limited convection in a magnetic field will provide the environment for the growth of high quality crystals. The approach exploits the variation of fluid magnetic susceptibility with concentration for this purpose and the convective damping is realized by appropriately positioning the crystal growth cell so that the magnetic susceptibility force counteracts terrestrial gravity. The general objective is to test the hypothesis of convective control using a strong magnetic field and magnetic field gradient and to understand the nature of the various forces that come into play. Specifically we aim to delineate causative factors and to quantify them through experiments, analysis and numerical modeling. The paper will report on the current status of the investigation and discuss results from the experimental and modeling efforts.

Cross-Linking Studies of Lysozyme Nucleation

NASA Technical Reports Server (NTRS)

Forsythe, Elizabeth; Pusey, Marc

2000-01-01

Tetragonal chicken egg white crystals consist of 4(sub 3) helices running in alternating directions, the helix rows having a two fold symmetry with each other. The unit cell consists of one complete tetrameric turn from each of two adjacent helices (an octamer). PBC analysis indicates that the helix intermolecular bonds are the strongest in the crystal, therefore likely formed first. AFM analysis of the (110) surface shows only complete helices, no half steps or bisected helices being found, while AFM line scans to measure the growth step increments show that they are multiples of the 4(sub 3) helix tetramer dimensions. This supports our thesis that the growth units are in fact multiples of the four molecule 4(sub 3) helix unit, the "average" growth unit size for the (110) face being an octamer (two turns about the helix) and the (101) growth unit averaging about the size of a hexamer. In an effort to better understand the species involved in the crystal nucleation and growth process, we have initiated an experimental program to study the species formed in solution compared to what is found in the crystal through covalent cross-linking studies. These experiments use the heterobifunctional cross-linking agent aminoethyl-4-azidonitroanaline (AEANA). An aliphatic amine at one end is covalently attached to the protein by a carbodiimide-mediated reaction, and a photo reactive group at the other can be used to initiate crosslinking. Modifications to the parent structure can be used to alter the distance between the two reactive groups and thus the cross-linking agents "reach". In practice, the cross-linking agent is first coupled to the asp101 side chain through the amine group. Asp101 lies within the active site cleft, and previous work with fluorescent probes had shown that derivatives at this site still crystallize in the tetragonal space group. This was also found to be the case with the AEANA derivative, which gave red tetragonal crystals. The protein now has a reactive group that can be photoactivated at a specific point in the nucleation or crystal growth process to "capture" protein molecules bound within reach of the crosslinking agent. If those bound protein molecules have a defined geometric relationship with the capturing molecule, such as would be found in a crystal, then the photoreacted cross-linking site should be consistent. Random protein interactions, typical of an amorphous precipitate or interaction, would show a random cross-linking reaction. The results of these and other experiments will be presented.

A preliminary review of organic materials single crystal growth by the Czochralski technique

NASA Astrophysics Data System (ADS)

Penn, B. G.; Shields, A. W.; Frazier, D. O.

1988-09-01

The growth of single crystals of organic compounds by the Czochralski method is reviewed. From the literature it is found that single crystals of benzil, a nonlinear optical material with a d sub 11 value of 11.2 + or - 1.5 x d sub 11 value of alpha quartz, has fewer dislocations than generally contained in Bridgman crystals. More perfect crystals were grown by repeated Czochralski growth. This consists of etching away the defect-containing portion of a Czochralski grown crystal and using it as a seed for further growth. Other compounds used to grow single crystals are benzophenone, 12-tricosanone (laurone), and salol. The physical properties, growth apparatus, and processing conditions presented in the literature are discussed. Moreover, some of the possible advantages of growing single crystals of organic compounds in microgravity to obtain more perfect crystals than on Earth are reviewed.

A preliminary review of organic materials single crystal growth by the Czochralski technique

NASA Technical Reports Server (NTRS)

Penn, B. G.; Shields, A. W.; Frazier, D. O.

1988-01-01

The growth of single crystals of organic compounds by the Czochralski method is reviewed. From the literature it is found that single crystals of benzil, a nonlinear optical material with a d sub 11 value of 11.2 + or - 1.5 x d sub 11 value of alpha quartz, has fewer dislocations than generally contained in Bridgman crystals. More perfect crystals were grown by repeated Czochralski growth. This consists of etching away the defect-containing portion of a Czochralski grown crystal and using it as a seed for further growth. Other compounds used to grow single crystals are benzophenone, 12-tricosanone (laurone), and salol. The physical properties, growth apparatus, and processing conditions presented in the literature are discussed. Moreover, some of the possible advantages of growing single crystals of organic compounds in microgravity to obtain more perfect crystals than on Earth are reviewed.

Crystal Growth of ZnSe and Related Ternary Compound Semiconductors by Vapor Transport

NASA Technical Reports Server (NTRS)

Su, Ching-Hua; Brebrick, Robert F.; Volz, Martin P.; Burger, Arnold; Dudley, Michael; Matyi, Richard J.; Ramachandran, Narayanan; Sha, Yi-Gao; Volz, Martin P.; Shih, Hung-Dah

2001-01-01

Crystal growth by vapor transport has several distinct advantages over melt growth techniques. Among various potential benefits from material processing in reduced gravity the followings two are considered to be related to crystal growth by vapor transport: (1) elimination of the crystal weight and its influence on the defect formation and (2) reduction of natural buoyancy-driven convective flows arising from thermally and/ or solutally induced density gradient in fluids. The previous results on vapor crystal growth of semiconductors showed the improvements in surface morphology, crystalline quality, electrical properties and dopant distribution of the crystals grown in reduced gravity as compared to the crystals grown on Earth. But the mechanisms, which are responsible for the improvements and cause the gravitational effects on the complicated and coupled processes of vapor mass transport and growth kinetics, are not well understood.

Single crystalline growth of a soluble organic semiconductor in a parallel aligned liquid crystal solvent using rubbing-treated polyimide films

NASA Astrophysics Data System (ADS)

Matsuzaki, Tomoya; Shibata, Yosei; Takeda, Risa; Ishinabe, Takahiro; Fujikake, Hideo

2017-01-01

For directional control of organic single crystals, we propose a crystal growth method using liquid crystal as the solvent. In this study, we examined the formation of 2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene (C8-BTBT) single crystals using a parallel aligned liquid crystal (LC) cell and rubbing-treated polyimide films in order to clarify the effects of LC alignment on anisotropic C8-BTBT crystal growth. Based on the results, we found that the crystal growth direction of C8-BTBT single crystals was related to the direction of the aligned LC molecules because of rubbing treatment. Moreover, by optical evaluation, we found that the C8-BTBT single crystals have a aligned molecular structure.

Protein crystals and their growth

NASA Technical Reports Server (NTRS)

Chernov, Alexander A.

2003-01-01

Recent results on the associations between protein molecules in crystal lattices, crystal-solution surface energy, elastic properties, strength, and spontaneous crystal cracking are reviewed and discussed. In addition, some basic approaches to understanding the solubility of proteins are followed by an overview of crystal nucleation and growth. It is argued that variability of mixing in batch crystallization may be a source of the variation in the number of crystals ultimately appearing in the sample. The frequency at which new molecules join a crystal lattice is measured by the kinetic coefficient and is related to the observed crystal growth rate. Numerical criteria used to discriminate diffusion- and kinetic-limited growth are discussed on this basis. Finally, the creation of defects is discussed with an emphasis on the role of impurities and convection on macromolecular crystal perfection.

Materials processing in space program tasks-supplement

NASA Technical Reports Server (NTRS)

Pentecost, E. (Compiler)

1983-01-01

An overview of the program scope for managers and scientists in industry, university, and government communities is provided. An introductory description of the program, its history, strategy, and overall goals; identification of the organizational structures and people involved; and a description of each research task, together with a list of recent publications are included. The tasks are grouped into six categories: crystal growth; solidification of metals, alloys, and composites; fluids, transports, and chemical processes; and ultrahigh vacuum and containerless processing technologies; combustion experiments; and experimental technology.

Method for the growth of large low-defect single crystals

NASA Technical Reports Server (NTRS)

Powell, J. Anthony (Inventor); Neudeck, Philip G. (Inventor); Trunek, Andrew J. (Inventor); Spry, David J. (Inventor)

2008-01-01

A method and the benefits resulting from the product thereof are disclosed for the growth of large, low-defect single-crystals of tetrahedrally-bonded crystal materials. The process utilizes a uniquely designed crystal shape whereby the direction of rapid growth is parallel to a preferred crystal direction. By establishing several regions of growth, a large single crystal that is largely defect-free can be grown at high growth rates. This process is particularly suitable for producing products for wide-bandgap semiconductors, such as SiC, GaN, AlN, and diamond. Large low-defect single crystals of these semiconductors enable greatly enhanced performance and reliability for applications involving high power, high voltage, and/or high temperature operating conditions.

The Effects of Impurities on Protein Crystal Growth and Nucleation: A Preliminary Study

NASA Technical Reports Server (NTRS)

Schall, Constance A.

1998-01-01

Kubota and Mullin (1995) devised a simple model to account for the effects of impurities on crystal growth of small inorganic and organic molecules in aqueous solutions. Experimentally, the relative step velocity and crystal growth of these molecules asymptotically approach zero or non-zero values with increasing concentrations of impurities. Alternatively, the step velocity and crystal growth can linearly approach zero as the impurity concentration increases. The Kubota-Mullin model assumes that the impurity exhibits Langmuirian adsorption onto the crystal surface. Decreases in step velocities and subsequent growth rates are related to the fractional coverage (theta) of the crystal surface by adsorbed impurities; theta = Kx / (I +Kx), x = mole fraction of impurity in solution. In the presence of impurities, the relative step velocity, V/Vo, and the relative growth rate of a crystal face, G/Go, are proposed to conform to the following equations: V/Vo approx. = G/Go = 1 - (alpha)(theta). The adsorption of impurity is assumed to be rapid and in quasi-equilibrium with the crystal surface sites available. When the value of alpha, an effectiveness factor, is one the growth will asymptotically approach zero with increasing concentrations of impurity. At values less than one, growth approaches a non-zero value asymptotically. When alpha is much greater than one, there will be a linear relationship between impurity concentration and growth rates. Kubota and Mullin expect alpha to decrease with increasing supersaturation and shrinking size of a two dimensional nucleus. It is expected that impurity effects on protein crystal growth will exhibit behavior similar to that of impurities in small molecule growth. A number of proteins were added to purified chicken egg white lysozyme, the effect on crystal nucleation and growth assessed.

Crystal growth and annealing method and apparatus

DOEpatents

Gianoulakis, Steven E.; Sparrow, Robert

2001-01-01

A method and apparatus for producing crystals that minimizes birefringence even at large crystal sizes, and is suitable for production of CaF.sub.2 crystals. The method of the present invention comprises annealing a crystal by maintaining a minimal temperature gradient in the crystal while slowly reducing the bulk temperature of the crystal. An apparatus according to the present invention includes a thermal control system added to a crystal growth and annealing apparatus, wherein the thermal control system allows a temperature gradient during crystal growth but minimizes the temperature gradient during crystal annealing. An embodiment of the present invention comprises a secondary heater incorporated into a conventional crystal growth and annealing apparatus. The secondary heater supplies heat to minimize the temperature gradients in the crystal during the annealing process. The secondary heater can mount near the bottom of the crucible to effectively maintain appropriate temperature gradients.

Protein crystal growth in space

NASA Technical Reports Server (NTRS)

Bugg, C. E.; Clifford, D. W.

1987-01-01

The advantages of protein crystallization in space, and the applications of protein crystallography to drug design, protein engineering, and the design of synthetic vaccines are examined. The steps involved in using protein crystallography to determine the three-dimensional structure of a protein are discussed. The growth chamber design and the hand-held apparatus developed for protein crystal growth by vapor diffusion techniques (hanging-drop method) are described; the experimental data from the four Shuttle missions are utilized to develop hardware for protein crystal growth in space and to evaluate the effects of gravity on protein crystal growth.

Phase-field crystal simulation facet and branch crystal growth

NASA Astrophysics Data System (ADS)

Chen, Zhi; Wang, Zhaoyang; Gu, Xinrui; Chen, Yufei; Hao, Limei; de Wit, Jos; Jin, Kexin

2018-05-01

Phase-field crystal model with one mode is introduced to describe morphological transition. The relationship between growth morphology and smooth density distribution was investigated. The results indicate that the pattern selection of dendrite growth is caused by the competition between interface energy anisotropy and interface kinetic anisotropy based on the 2D phase diagram. When the calculation time increases, the crystal grows to secondary dendrite at the dimensionless undercooling equal to - 0.4. Moreover, when noise is introduced in the growth progress, the symmetry is broken in the growth mode, and there becomes irregular fractal-like growth morphology. Furthermore, the single crystal shape develops into polycrystalline when the noise amplitude is large enough. When the dimensionless undercooling is less than - 0.3, the noise has a significant effect on the growth shape. In addition, the growth velocity of crystal near to liquid phase line is slow, while the shape far away from the liquid adapts to fast growth. Based on the simulation results, the method was proved to be effective, and it can easily obtain different crystal shapes by choosing the different points in 2D phase diagram.

Unidirectional growth of benzil crystal from solution by Sankaranarayanan-Ramasamy method and its characterization.

PubMed

Rajalakshmi, M; Shyju, T S; Indirajith, R; Gopalakrishnan, R

2012-02-01

Good quality <100> benzil single crystal with a diameter 18 mm and length 75 mm was successfully grown from solution by the unidirectional growth method of Sankaranarayanan-Ramasamy (SR) for the first time in the literature. The seed crystals have been harvested from conventional solution growth technique and subsequently used for unidirectional growth. The grown crystal was subjected to various characterization studies. The results of UV-vis spectral analysis, photoluminescence, etching and microhardness studies were compared with conventional solution grown crystal to that of SR method grown crystal. The quality of SR method grown benzil crystal is better than conventional solution grown crystal. Copyright © 2011 Elsevier B.V. All rights reserved.

Site-discrimination by molecular imposters at dissymmetric molecular crystal surfaces

NASA Astrophysics Data System (ADS)

Poloni, Laura N.

The organization of atoms and molecules into crystalline forms is ubiquitous in nature and has been critical to the development of many technologies on which modern society relies. Classical crystal growth theory can describe atomic crystal growth, however, a description of molecular crystal growth is lacking. Molecular crystals are often characterized by anisotropic intermolecular interactions and dissymmetric crystal surfaces with anisotropic growth rates along different crystallographic directions. This thesis describes combination of experimental and computational techniques to relate crystal structure to surface structure and observed growth rates. Molecular imposters, also known as tailor-made impurities, can be used to control crystal growth for practical applications such as inhibition of pathological crystals, but can also be used to understand site specificity at crystal growth surfaces. The first part of this thesis builds on previous real-time in situ atomic force microscopy (AFM) observations of dislocation-actuated growth on the morphologically significant face of hexagonal L-cystine crystals, which aggregate in vivo to form kidney stones in patients suffering from cystinuria. The inhibitory effect of various L-cystine structural mimics (a.k.a. molecular imposters) was investigated through experimental and computational methods to identify the key structural factors responsible for molecular recognition between molecular imposters and L-cystine crystal surface sites. The investigation of L-cystine crystal growth in the presence of molecular imposters through a combination of kinetic analysis using in situ AFM, morphology analysis and birefringence measurements of bulk crystals, and molecular modeling of imposter binding to energetically inequivalent surface sites revealed that different molecular imposters inhibited crystal growth by a Cabrera-Vermilyea pinning mechanism and that imposters bind to a single binding site on the dissymmetric {1000} L-cystine surfaces. Collectively, these findings identify the key structural factors responsible for molecular recognition between molecular imposters and L-cystine crystal step sites, thereby articulating a strategy for stone prevention based on molecular design. The second part of this thesis describes the crystal growth and inhibition of a P2X3 receptor antagonist, denoted as DAPSA, recently reported as a non-opioid treatment of chronic pain. The low solubility of this compound results in the formation of drug-induced renal calculi (a.k.a. xenostones). in situ AFM of the morphologically significant (011) DAPSA surface revealed dislocation-actuated growth spirals with an anisotropic morphology, behavior that can be attributed to the non-uniform rate of solute attachment to eight crystallographically unique steps of the spiral, a direct consequence of the dissymmetry of this crystal surface. Eighteen molecular imposters were selected from the screening library to systematically investigate the roles of imposter substitute position, size, and functionality on the step velocities along the eight unique crystallographic directions. A non-uniform reduction in step velocities was observed, signaling site discrimination of imposter binding that can be attributed to stereochemical recognition of the imposters at specific crystal sites. The anisotropy of growth inhibition observed in the presence of the various imposters is consistent with binding energies calculated for the thirty-two crystallographically unique kink sites on steps advancing along predominant growth directions. These results provide insight to the design of growth inhibitors for molecular crystalline solids with complex and dissymmetric surfaces, while also suggesting a strategy for formulations containing congeners that can prevent harmful crystal growth in human renal structures. The last two crystalline systems discussed in this thesis are two isomorphous crystal systems that are ideal for the study of impurity incorporation at dissymmetric surfaces because their morphology is dominated by dissymmetric {101} growth faces. Growth processes on the dissymmetric (101) surfaces of these crystalline systems were investigated using metadynamics simulations to determine the free energy of adsorption for solute and impurity attachment to different flat, stepped, and kinked (101) surface terminations. Results suggest that growth occurs via a non-Kossel crystal growth mechanism, and highlights the need for dissymmetric surface structures (i.e. steps and kinks) for a higher fidelity in the orientation of adsorbed molecules. Overall, the results presented in this thesis suggest that growth of molecular crystals, particularly at dissymmetric surfaces, is complex and requires the combination of several experimental and computational techniques to decipher the mechanisms responsible for growth phenomena. The use of molecular imposters to inhibit growth can be useful for the development of therapeutics for pathological crystals, but can also inform processes by which crystal growth occurs at complex surfaces as a result of their site selectivity.

A study of crystal growth by solution technique

NASA Technical Reports Server (NTRS)

Lal, R. B.

1981-01-01

The mechanism of crystal growth by solution technique was studied. A low temperature solution crystal growth setup was developed. Crystals of triglycine sulfate (TGS) were grown using this arrangement. Some additional tasks were performed toward fabrication of experiments for future space flight.

Delta L: An Apparatus for Measuring Macromolecule Crystal Growth Rates in Microgravity

NASA Technical Reports Server (NTRS)

Judge, Russell A.; Whitaker, Ann F. (Technical Monitor)

2001-01-01

Strongly diffracting high quality macromolecule crystals of suitable volume are keenly sought for X-ray diffraction analysis so that high-resolution molecular structure data can be obtained. Such data is of tremendous value to medical research, agriculture and commercial biotechnology. In previous studies by many investigators microgravity has been reported in some instances to improve biological macromolecule X-ray crystal quality while little or no improvement was observed in other cases. A better understanding of processes effecting crystal quality improvement in microgravity will therefore be of great benefit in optimizing crystallization success in microgravity. In ground based research with the protein lysozyme we have previously shown that a population of crystals grown under the same solution conditions, exhibit a variation in X-ray diffraction properties (Judge et al., 1999). We have also observed that under the same solution conditions, individual crystals will grow at slightly different growth rates. This phenomenon is called growth rate dispersion. For small molecule materials growth rate dispersion has been directly related to crystal quality (Cunningham et al., 1991; Ristic et al., 1991). We therefore postulate that microgravity may act to improve crystal quality by reducing growth rate dispersion. If this is the case then as different, Materials exhibit different degrees of growth rate dispersion on the ground then growth rate dispersion could be used to screen which materials may benefit the most from microgravity crystallization. In order to assess this theory the Delta L hardware is being developed so that macromolecule crystal growth rates can be measured in microgravity. Crystal growth rate is defined as the change or delta in crystal size (defined as a characteristic length, L) over time; hence the name of the hardware. Delta L will consist of an optics, a fluids, and a data acquisition sub-assemblies. The optics assembly will consist of a video microscope camera mounted on three axis computer controlled translation stages. The fluids assembly consists of macromolecule and precipitant reservoirs, a temperature controlled growth cell and waste container, The data acquisition is achieved by using a frame-gabber, with images being stored on a hard drive. In operation, macromolecule and precipitant solution will be injected into the temperature controlled growth cell. As macromolecule crystals grow, the video microscope camera controlled by the translation stages, will be used to locate and record images of individual crystals, returning to the same crystals at specific time intervals. The images will be stored on the hard drive and used to calculate the crystal growth rate. To prevent vibrations interfering in the crystal growth rate measurements (Snell et al., 1997) Delta L will be used in connection with the Glovebox Integrated Microgravity Isolation Technology (g-LIMIT) inside the Microgravity Science Glovebox (MSG), onboard the International Space Station (ISS).

Influence of Containment on the Growth of Silicon-Germanium: A Materials Science Flight Project

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.; Croell, A.

2012-01-01

This investigation involves the comparison of results achieved from three types of crystal growth of germanium and germanium-silicon alloys: (1) Float zone growth (2) Bridgman growth (3) Detached Bridgman growth crystal The fundamental goal of the proposed research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon (GeSi) crystals (silicon concentration in the solid up to 5 at%) for three different growth configurations in order to quantitatively assess the improvements of crystal quality possible by detached growth.

Insights into crystal growth rates from a study of orbicular granitoids from western Australia

NASA Astrophysics Data System (ADS)

Zhang, J.; Lee, C. T.

2017-12-01

The purpose of this study is to develop new tools for constraining crystal growth rate in geologic systems. Of interest is the growth of crystals in magmatic systems because crystallization changes the rheology of a magma as well as provides surfaces on which bubbles can nucleate. To explore crystal growth in more detail, we conducted a case study of orbicular granitoids from western Australia. The orbicules occur as spheroids dispersed in a granitic matrix. Most orbicules have at least two to three concentric bands, composed of elongate and radially oriented hornblende surrounded by interstitial plagioclase. We show that mineral modes and hence bulk composition at the scale of the band is homogeneous from rim to core. Crystal number density decreases and crystal size increases from rim to core. These observations suggest that the orbicules crystallized rapidly from rim to core. We hypothesize that the orbicules are blobs of hot dioritic liquid injected into a cold granitic magma and subsequently cooled and solidified. Crystals stop growing when the mass transport rate tends to zero due to the low temperature. We estimated cooling timescales based on conductive cooling models, constraining crystal growth rates to be 10-6 to 10-5 m/s. We also show that the oscillatory banding is controlled by disequilibrium crystallization, wherein hornblende preferentially crystallizes, resulting in the diffusive growth of a chemical boundary layer enriched in plagioclase component, which in turns results in crystallization of plagioclase. We show that the correlation between the width of each crystallization couplet (band) with distance from orbicule rim is linear, with the slope corresponding to the square root of the ratio between chemical diffusivity in the growth medium and thermal diffusivity. We estimate chemical diffusivity of 2*10-7 m2/s, which is remarkably fast for silicate liquids but reasonable for diffusion in hot aqueous fluids, suggesting that crystallization occurred during water-saturated conditions. Combined with the estimate of the boundary layer thickness, we use the diffusivity to estimate the diffusive flux, arriving at crystal growth rates similar to that constrained by thermal modeling. In the presence of fluids, we show that crystal growth rates in magmatic systems may be under-estimated.

Process for Encapsulating Protein Crystals

NASA Technical Reports Server (NTRS)

Morrison, Dennis R.; Mosier, Benjamin

2003-01-01

A process for growing protein crystals encapsulated within membranes has been invented. This process begins with the encapsulation of a nearly saturated aqueous protein solution inside semipermeable membranes to form microcapsules. The encapsulation is effected by use of special formulations of a dissolved protein and a surfactant in an aqueous first liquid phase, which is placed into contact with a second, immiscible liquid phase that contains one or more polymers that are insoluble in the first phase. The second phase becomes formed into the semipermeable membranes that surround microglobules of the first phase, thereby forming the microcapsules. Once formed, the microcapsules are then dehydrated osmotically by exposure to a concentrated salt or polymer solution. The dehydration forms supersaturated solutions inside the microcapsules, thereby enabling nucleation and growth of protein crystals inside the microcapsules. By suitable formulation of the polymer or salt solution and of other physical and chemical parameters, one can control the rate of transport of water out of the microcapsules through the membranes and thereby create physicochemical conditions that favor the growth, within each microcapsule, of one or a few large crystals suitable for analysis by x-ray diffraction. The membrane polymer can be formulated to consist of low-molecular-weight molecules that do not interfere with the x-ray diffraction analysis of the encapsulated crystals. During dehydration, an electrostatic field can be applied to exert additional control over the rate of dehydration. This protein-crystal-encapsulation process is expected to constitute the basis of protein-growth experiments to be performed on the space shuttle and the International Space Station. As envisioned, the experiments would involve the exposure of immiscible liquids to each other in sequences of steps under microgravitational conditions. The experiments are expected to contribute to knowledge of the precise conditions under which protein crystals form. By enhancing the ability to grow crystals suitable for x-ray diffraction analysis, this knowledge can be expected to benefit not only the space program but also medicine and the pharmaceutical industry.

A framework for multi-scale simulation of crystal growth in the presence of polymers.

PubMed

Mandal, Taraknath; Huang, Wenjun; Mecca, Jodi M; Getchell, Ashley; Porter, William W; Larson, Ronald G

2017-03-01

We present a multi-scale simulation method for modeling crystal growth in the presence of polymer excipients. The method includes a coarse-grained (CG) model for small molecules of known crystal structure whose force field is obtained using structural properties from atomistic simulations. This CG model is capable of stabilizing the molecular crystal structure and capturing the crystal growth from the melt for a wide range of small organic molecules, as demonstrated by application of our method to the molecules isoniazid, urea, sulfamethoxazole, prilocaine, oxcarbazepine, and phenytoin. This CG model can also be used to study the effect of additives, such as polymers, on the inhibition of crystal growth by polymers, as exemplified by our simulation of suppression of the rate of crystal growth of phenytoin, an active pharmaceutical ingredient (API), by a cellulose excipient, functionalized with acetate (Ac), hydroxy-propyl (Hp) and succinate (Su) groups. We show that the efficacy of the cellulosic polymers in slowing crystal growth of small molecules strongly depends on the functional group substitution on the cellulose backbone, with the acetate substituent group slowing crystal growth more than does the deprotonated succinate group, which we confirm by experimental drug supersaturation studies.

Remote control system for high-perfomance computer simulation of crystal growth by the PFC method

NASA Astrophysics Data System (ADS)

Pavlyuk, Evgeny; Starodumov, Ilya; Osipov, Sergei

2017-04-01

Modeling of crystallization process by the phase field crystal method (PFC) - one of the important directions of modern computational materials science. In this paper, the practical side of the computer simulation of the crystallization process by the PFC method is investigated. To solve problems using this method, it is necessary to use high-performance computing clusters, data storage systems and other often expensive complex computer systems. Access to such resources is often limited, unstable and accompanied by various administrative problems. In addition, the variety of software and settings of different computing clusters sometimes does not allow researchers to use unified program code. There is a need to adapt the program code for each configuration of the computer complex. The practical experience of the authors has shown that the creation of a special control system for computing with the possibility of remote use can greatly simplify the implementation of simulations and increase the performance of scientific research. In current paper we show the principal idea of such a system and justify its efficiency.

Protein crystal growth

NASA Technical Reports Server (NTRS)

Bugg, Charles E.

1993-01-01

Proteins account for 50% or more of the dry weight of most living systems and play a crucial role in virtually all biological processes. Since the specific functions of essentially all biological molecules are determined by their three-dimensional structures, it is obvious that a detailed understanding of the structural makeup of a protein is essential to any systematic research pertaining to it. At the present time, protein crystallography has no substitute, it is the only technique available for elucidating the atomic arrangements within complicated biological molecules. Most macromolecules are extremely difficult to crystallize, and many otherwise exciting and promising projects have terminated at the crystal growth stage. There is a pressing need to better understand protein crystal growth, and to develop new techniques that can be used to enhance the size and quality of protein crystals. There are several aspects of microgravity that might be exploited to enhance protein crystal growth. The major factor that might be expected to alter crystal growth processes in space is the elimination of density-driven convective flow. Another factor that can be readily controlled in the absence of gravity is the sedimentation of growing crystal in a gravitational field. Another potential advantage of microgravity for protein crystal growth is the option of doing containerless crystal growth. One can readily understand why the microgravity environment established by Earth-orbiting vehicles is perceived to offer unique opportunities for the protein crystallographer. The near term objectives of the Protein Crystal Growth in a Microgravity Environment (PCG/ME) project is to continue to improve the techniques, procedures, and hardware systems used to grow protein crystals in Earth orbit.

Growth of 2 Inch Eu-doped SrI2 single crystals for scintillator applications

NASA Astrophysics Data System (ADS)

Yoshikawa, Akira; Shoji, Yasuhiro; Yokota, Yuui; Kurosawa, Shunsuke; Hayasaka, Shoki; Chani, Valery I.; Ito, Tomoki; Kamada, Kei; Ohashi, Yuji; Kochurikhin, Vladimir

2016-10-01

A vertical Bridgman (VB) crystal growth process was established using modified micro-pulling-down (μ-PD) crystal growth system with a removable chamber that was developed for the growth of deliquescent halide single crystals because conventional μ-PD method does not allow growth of large bulk single crystals. Eu:SrI2 crystals were grown from the melt of (Sr0.98Eu0.02)I2 composition using carbon crucibles. Undoped μ-PD SrI2 crystals were used as seeds that were affixed to the bottom of the crucible. All the preparations preceding the growths and the hot zone assembling were performed in a glove box with Ar gas. Then the removable chamber was taken out of the glove box, attached to the μ-PD system, connected with a Turbo Molecular pump, and evacuated down to 10-4 Pa at 300 °C. After the baking procedure, high purity Ar gas (6N) was injected into the chamber. The crucible was heated by a high frequency induction coil up to the melting point of Eu:SrI2. After melting the starting materials, the crucible was displaced in downward direction for the crystal growth and then cooled down to room temperature. Thus, 2 in. and crack-free Eu:SrI2 bulk crystals were produced. The crystals had high transparency and did not contain any visible inclusions. The crystals were cut and polished in the glove box and then sealed in an aluminum container with an optical window for characterization. The details of the crystal growth are discussed.

Effect of solvents on the bulk growth of 4-aminobenzophenone single crystals: A potential material for blue and green lasers

NASA Astrophysics Data System (ADS)

Natarajan, V.; Usharani, S.; Arivanandhan, M.; Anandan, P.; Hayakawa, Y.

2015-06-01

Although 4-aminobenzophenone (4-ABP) is the best derivative of benzophenone with 260 times higher second harmonic generation (SHG) efficiency than potassium dihydrogen phosphate (KDP), growth of high quality bulk crystal still remains a difficult task. In the present work, the effect of solvents on solubility and growth aspects of 4-ABP was investigated to grow inclusion free 4-ABP crystals. The growth processes were discussed based on solute-solvent interaction in two different growth media of ethyl acetate and ethanol. The growth rate and thereby solvent inclusions are relatively higher in ethyl acetate grown crystal than the crystal grown from ethanol. The structural, thermal and optical properties of 4-ABP crystals were studied. The enthalpy of 4-ABP melting process was estimated from differential thermal analysis. The optical transmission study shows that 4-ABP crystals grown from ethanol has high transparency compared to ethyl acetate grown sample due to solvent inclusion in the later crystal.

Reverse engineering the kidney: modelling calcium oxalate monohydrate crystallization in the nephron.

PubMed

Borissova, A; Goltz, G E; Kavanagh, J P; Wilkins, T A

2010-07-01

Crystallization of calcium oxalate monohydrate in a section of a single kidney nephron (distal convoluted tubule) is simulated using a model adapted from industrial crystallization. The nephron fluid dynamics is represented as a crystallizer/separator series with changing volume to allow for water removal along the tubule. The model integrates crystallization kinetics and crystal size distribution and allows the prediction of the calcium oxalate concentration profile and the nucleation and growth rates. The critical supersaturation ratio for the nucleation of calcium oxalate crystals has been estimated as 2 and the mean crystal size as 1 mum. The crystal growth order, determined as 2.2, indicates a surface integration mechanism of crystal growth and crystal growth dispersion. The model allows the exploration of the effect of varying the input calcium oxalate concentration and the rate of water extraction, simulating real life stressors for stone formation such as dietary loading and dehydration.

Protein Crystals and their Growth

NASA Technical Reports Server (NTRS)

Chernov, A. A.

2004-01-01

Recent results on binding between protein molecules in crystal lattice, crystal-solution surface energy, elastic properties and strength and spontaneous crystal cracking are reviewed and discussed in the first half of this paper (Sea 2-4). In the second par&, some basic approaches to solubility of proteins are followed by overview on crystal nucleation and growth (Sec 5). It is argued that variability of mixing in batch crystallization may be a source for scattering of crystal number ultimately appearing in the batch. Frequency at which new molecules join crystal lattice is measured by kinetic coefficient and related to the observable crystal growth rate. Numerical criteria to discriminate diffusion and kinetic limited growth are discussed on this basis in Sec 7. In Sec 8, creation of defects is discussed with the emphasis on the role of impurities and convection on macromolecular crystal I;erfection.

Kinetic Roughening and Energetics of Tetragonal Lysozyme Crystal Growth: A Preliminary Atomic Force Microscopy Investigation

NASA Technical Reports Server (NTRS)

Gorti, Sridhar; Forsythe, Elizabeth L.; Pusey, Marc L.

2004-01-01

We examined particulars of crystal growth from measurements obtained at both microscopic and molecular levels. The crystal growth measurements performed at the microscopic level are well characterized by a model that balances the flux of macromolecules towards the crystal surface with the flux of the crystal surface. Numerical evaluation of model with measurements of crystal growth, in time, provided accurate estimates for the average growth velocities. Growth velocities thus obtained were also interpreted using well-established phenomenological theories. Moreover, we find that microscopic measurements of growth velocity measurements obtained as a function of temperature best characterizes changes in crystal growth modes, when present. We also examined the possibility of detecting a change in crystal growth modes at the molecular level using atomic force microscopy, AFM. From preliminary AFM measurements performed at various supersaturations, we find that magnitude of surface height fluctuations, h(x), increases with supersaturation. Further examination of surface height fluctuations using methods established for fluctuation spectroscopy also enabled the discovery of the existence of a characteristic length, c, which may possibly determine the mode of crystal growth. Although the results are preliminary, we establish the non- critical divergence of 5 and the root-mean-square (rms) magnitude of height-height fluctuations as the kinetic roughening transition temperatures are approached. Moreover, we also examine approximate models for interpreting the non-critical behavior of both 6 and rms magnitude of height-height fluctuations, as the solution supersaturation is increased towards the kinetic roughening supersaturation.

Electromigration process for the purification of molten silicon during crystal growth

DOEpatents

Lovelace, Alan M. Administrator of the National Aeronautics and Space; Shlichta, Paul J.

1982-01-01

A process for the purification of molten materials during crystal growth by electromigration of impurities to localized dirty zones. The process has particular applications for silicon crystal growth according to Czochralski techniques and edge-defined film-fed growth (EFG) conditions. 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. In the EFG 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 are thereby migrated to one side only of the crystal ribbon. The impurities 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.

Growth morphologies of wax in the presence of kinetic inhibitors

NASA Astrophysics Data System (ADS)

Tetervak, Alexander A.

Driven by the need to prevent crystallization of normal alkanes from diesel fuels in cold climates, the petroleum industry has developed additives to slow the growth of these crystals and alter their morphologies. Although the utility of these kinetic inhibitors has been well demonstrated in the field, few studies have directly monitored their effect at microscopic morphology, and the mechanisms by which they act remain poorly understood. Here we present a study of the effects of such additives on the crystallization of long-chain n-alkanes from solution. The additives change the growth morphology from plate-like crystals to a microcrystalline mesh. When we impose a front velocity by moving the sample through a temperature gradient, the mesh growth may form a macroscopic banded pattern and also exhibit a burst-crystallization behavior. In this study, we characterize these crystallization phenomena and also two growth models: a continuum model that demonstrates the essential behavior of the banded crystallization, and a simple qualitative cellular automata model that captures basics of the burst-crystallization process. Keywords: solidification; mesh crystallization; kinetic inhibitor; burst growth.

Crystal Growth Technology

NASA Astrophysics Data System (ADS)

Scheel, Hans J.; Fukuda, Tsuguo

2004-06-01

This volume deals with the technologies of crystal fabrication, of crystal machining, and of epilayer production and is the first book on industrial and scientific aspects of crystal and layer production. The major industrial crystals are treated: Si, GaAs, GaP, InP, CdTe, sapphire, oxide and halide scintillator crystals, crystals for optical, piezoelectric and microwave applications and more. Contains 29 contributions from leading crystal technologists covering the following topics:

General aspects of crystal growth technology Silicon Compound semiconductors Oxides and halides Crystal machining Epitaxy and layer deposition Scientific and technological problems of production and machining of industrial crystals are discussed by top experts, most of them from the major growth industries and crystal growth centers. In addition, it will be useful for the users of crystals, for teachers and graduate students in materials sciences, in electronic and other functional materials, chemical and metallurgical engineering, micro-and optoelectronics including nanotechnology, mechanical engineering and precision-machining, microtechnology, and in solid-state sciences.

• Diffusion, Viscosity and Crystal Growth in Microgravity

  NASA Technical Reports Server (NTRS)

  Myerson, Allan S.

  1996-01-01

  The diffusivity of TriGlycine Sulfate (TGS), Potassium Dihydrogen Phosphate (KDP), Ammonium Dihydrogen Phosphate (ADF) and other compounds of interest to microgravity crystal growth, in supersaturated solutions as a function of solution concentration, 'age' and 'history was studied experimentally. The factors that affect the growth of crystals from water solutions in microgravity have been examined. Three non-linear optical materials have been studied, potassium dihydrogen phosphate (KDP), ammonium dihydrogen phosphate (ADP) and triglycine sulfate (TGC). The diffusion coefficient and viscosity of supersaturated water solutions were measured. Also theoretical model of diffusivity and viscosity in a metastable state, model of crystal growth from solution including non-linear time dependent diffusivity and viscosity effect and computer simulation of the crystal growth process which allows simulation of the microgravity crystal growth were developed.

• Fast surface crystallization of amorphous griseofulvin below T g.

  PubMed

  Zhu, Lei; Jona, Janan; Nagapudi, Karthik; Wu, Tian

  2010-08-01

  To study crystal growth rates of amorphous griseofulvin (GSF) below its glass transition temperature (T (g)) and the effect of surface crystallization on the overall crystallization kinetics of amorphous GSF. Amorphous GSF was generated by melt quenching. Surface and bulk crystal growth rates were determined using polarized light microscope. X-ray powder diffraction (XRPD) and Raman microscopy were used to identify the polymorph of the crystals. Crystallization kinetics of amorphous GSF powder stored at 40 degrees C (T (g)-48 degrees C) and room temperature (T (g)-66 degrees C) was monitored using XRPD. Crystal growth at the surface of amorphous GSF is 10- to 100-fold faster than that in the bulk. The surface crystal growth can be suppressed by an ultrathin gold coating. Below T (g), the crystallization of amorphous GSF powder was biphasic with a rapid initial crystallization stage dominated by the surface crystallization and a slow or suspended late stage controlled by the bulk crystallization. GSF exhibits the fastest surface crystallization kinetics among the known amorphous pharmaceutical solids. Well below T (g), surface crystallization dominated the overall crystallization kinetics of amorphous GSF powder. Thus, surface crystallization should be distinguished from bulk crystallization in studying, modeling and controlling the crystallization of amorphous solids.

• Experimental analysis and modeling of melt growth processes

  NASA Astrophysics Data System (ADS)

  Müller, Georg

  2002-04-01

  Melt growth processes provide the basic crystalline materials for many applications. The research and development of crystal growth processes is therefore driven by the demands which arise from these specific applications; however, common goals include an increased uniformity of the relevant crystal properties at the micro- and macro-scale, a decrease of deleterious crystal defects, and an increase of crystal dimensions. As melt growth equipment and experimentation becomes more and more expensive, little room remains for improvements by trial and error procedures. A more successful strategy is to optimize the crystal growth process by a combined use of experimental process analysis and computer modeling. This will be demonstrated in this paper by several examples from the bulk growth of silicon, gallium arsenide, indium phosphide, and calcium fluoride. These examples also involve the most important melt growth techniques, crystal pulling (Czochralski methods) and vertical gradient freeze (Bridgman-type methods). The power and success of the above optimization strategy, however, is not limited only to the given examples but can be generalized and applied to many types of bulk crystal growth.

• Crystal growth and molecular modeling studies of inhibition of struvite by phosphocitrate.

  PubMed

  Wierzbicki, A; Sallis, J D; Stevens, E D; Smith, M; Sikes, C S

  1997-09-01

  The inhibition by phosphocitrate of struvite crystal formation and growth has been examined in the present study. Crystal growth in a gel matrix was controlled by phosphocitrate in a dose-dependent manner. The effects of inhibition were followed using scanning electron microscopy, optical microscopy, and single crystal X-ray analysis. The presence of phosphocitrate induced very strong, crystal face specific inhibition of struvite, leading to total cessation of crystal growth when sufficient concentration of the inhibitor was made available. Crystal growth studies and results from molecular modeling indicated strong affinity of phosphocitrate to (101) faces of struvite. This in turn led to an alteration in the expression of these faces and the development of a characteristic arrowhead struvite morphology. Similar changes were not observed in the presence of identical concentrations of citrate, acetohydroxamic acid, and N-sulfo-2 amino tricarballylate (an analog of phosphocitrate), emphasizing the unique interaction of phosphocitrate with the struvite crystal lattice.

Patterned solid state growth of barium titanate crystals

NASA Astrophysics Data System (ADS)

Ugorek, Michael Stephen

An understanding of microstructure evolution in ceramic materials, including single crystal development and abnormal/enhanced grain growth should enable more controlled final ceramic element structures. In this study, two different approaches were used to control single crystal development in a patterned array. These two methods are: (1) patterned solid state growth in BaTiO 3 ceramics, and (2) metal-mediated single crystal growth in BaTiO 3. With the patterned solid state growth technique, optical photolithography was used to pattern dopants as well as [001] and [110] BaTiO3 single crystal template arrays with a 1000 microm line pattern array with 1000 microm spacings. These patterns were subsequently used to control the matrix grain growth evolution and single crystal development in BaTiO3. It was shown that the growth kinetics can be controlled by a small initial grain size, atmosphere conditions, and the introduction of a dopant at selective areas/interfaces. By using a PO2 of 1x10-5 atm during high temperature heat treatment, the matrix coarsening has been limited (to roughly 2 times the initial grain size), while retaining single crystal boundary motion up to 0.5 mm during growth for dwell times up to 9 h at 1300°C. The longitudinal and lateral growth rates were optimized at 10--15 microm/h at 1300°C in a PO2 of 1x10 -5 atm for single crystal growth with limited matrix coarsening. Using these conditions, a patterned microstructure in BaTiO3 was obtained. With the metal-mediated single crystal growth technique, a novel approach for fabricating 2-2 single crystal/polymer composites with a kerf < 5 microns was demonstrated. Surface templated grain growth was used to propagate a single crystal interface into a polycrystalline BaTiO3 or Ba(Zr0.05 Ti0.95)O3 matrix with lamellar nickel layers. The grain growth evolution and texture development were studied using both [001] and [110] BaTiO3 single crystals templates. By using a PO 2 of 1x10-11 atm during high temperature heat treatment, matrix coarsening was limited while enabling single crystal boundary motion up to 0.35 mm during growth between 1250°C and 1300°C with growth rates ˜ 3--4 microm/h for both single crystal orientations. By removing the inner electrodes, 2-2 single crystal (or ceramic) composites were prepared. The piezoelectric and dielectric properties of the composites of the two compositions were measured. The d33 and d31 of the composites were similar to the polycrystalline ceramic of the same composition.

The control of float zone interfaces by the use of selected boundary conditions

NASA Technical Reports Server (NTRS)

Foster, L. M.; Mcintosh, J.

1983-01-01

The main goal of the float zone crystal growth project of NASA's Materials Processing in Space Program is to thoroughly understand the molten zone/freezing crystal system and all the mechanisms that govern this system. The surface boundary conditions required to give flat float zone solid melt interfaces were studied and computed. The results provide float zone furnace designers with better methods for controlling solid melt interface shapes and for computing thermal profiles and gradients. Documentation and a user's guide were provided for the computer software.

Crystal Growth and Other Materials Physical Researches in Space Environment

NASA Astrophysics Data System (ADS)

Pan, Mingxiang

Material science researches in space environment are based on reducing the effects of buoyancy driven transport, the effects of atomic oxygen, radiation, extremes of heat and cold and the ultrahigh vacuum, so as to unveil the underlying fundamental phenomena, lead maybe to new potential materials or new industrial processes and develop space techniques. Currently, research program on materials sciences in Chinese Manned Space Engineering (CMSE) is going on. More than ten projects related to crystal growth and materials processes are selected as candidates to be executed in Shenzhou spacecraft, Tiangong Space Laboratory and Chinese Space Station. In this talk, we will present some examples of the projects, which are being prepared and executed in the near future flight tasks. They are both basic and applied research, from discovery to technology.

A simplified counter diffusion method combined with a 1D simulation program for optimizing crystallization conditions.

PubMed

Tanaka, Hiroaki; Inaka, Koji; Sugiyama, Shigeru; Takahashi, Sachiko; Sano, Satoshi; Sato, Masaru; Yoshitomi, Susumu

2004-01-01

We developed a new protein crystallization method has been developed using a simplified counter-diffusion method for optimizing crystallization condition. It is composed of only a single capillary, the gel in the silicon tube and the screw-top test tube, which are readily available in the laboratory. The one capillary can continuously scan a wide range of crystallization conditions (combination of the concentrations of the precipitant and the protein) unless crystallization occurs, which means that it corresponds to many drops in the vapor-diffusion method. The amount of the precipitant and the protein solutions can be much less than in conventional methods. In this study, lysozyme and alpha-amylase were used as model proteins for demonstrating the efficiency of this method. In addition, one-dimensional (1-D) simulations of the crystal growth were performed based on the 1-D diffusion model. The optimized conditions can be applied to the initial crystallization conditions for both other counter-diffusion methods with the Granada Crystallization Box (GCB) and for the vapor-diffusion method after some modification.

Measurements of Protein Crystal Face Growth Rates

NASA Technical Reports Server (NTRS)

Gorti, S.

2014-01-01

Protein crystal growth rates will be determined for several hyperthermophile proteins.; The growth rates will be assessed using available theoretical models, including kinetic roughening.; If/when kinetic roughening supersaturations are established, determinations of protein crystal quality over a range of supersaturations will also be assessed.; The results of our ground based effort may well address the existence of a correlation between fundamental growth mechanisms and protein crystal quality.

Growth of urea crystals by physical vapor transport

NASA Technical Reports Server (NTRS)

Feigelson, R. S.; Route, R. K.; Kao, T.-M.

1985-01-01

This work demonstrates that high optical quality crystals of urea can be grown by the physical vapor transport method. The unique features of this method are compared with growth from methanol/water solutions. High growth rates, exceeding 2.5 mm/day, were achieved, and cm-size optical quality single crystals were obtained. Details of the growth technique and the physical properties of the crystals are presented.

Phase-field study of grain boundary tracking behavior in crack-seal microstructures

NASA Astrophysics Data System (ADS)

Ankit, Kumar; Nestler, Britta; Selzer, Michael; Reichardt, Mathias

2013-12-01

In order to address the growth of crystals in veins, a multiphase-field model is used to capture the dynamics of crystals precipitating from a super-saturated solution. To gain a detailed understanding of the polycrystal growth phenomena in veins, we investigate the influence of various boundary conditions on crystal growth. In particular, we analyze the formation of vein microstructures resulting from the free growth of crystals as well as crack-sealing processes. We define the crystal symmetry by considering the anisotropy in surface energy to simulate crystals with flat facets and sharp corners. The resulting growth competition of crystals with different orientations is studied to deduce a consistent orientation selection rule in the free-growth regime. Using crack-sealing simulations, we correlate the grain boundary tracking behavior depending on the relative rate of crack opening, opening trajectory, initial grain size, and wall roughness. Further, we illustrate how these parameters induce the microstructural transition between blocky (crystals growing anisotropically) to fibrous morphology (isotropic) and formation of grain boundaries. The phase-field simulations of crystals in the free-growth regime (in 2D and 3D) indicate that the growth or consumption of a crystal is dependent on the orientation difference with neighboring crystals. The crack-sealing simulation results (in 2D and 3D) reveal that crystals grow isotropically and grain boundaries track the opening trajectory if the wall roughness is high, opening increments are small, and crystals touch the wall before the next crack increment starts. Further, we find that within the complete crack-seal regime, anisotropy in surface energy results in the formation of curved/oscillating grain boundaries (instead of straight) when the crack-opening velocity is increased and wall roughness is not sufficiently high. Additionally, the overall capability of phase-field method to simulate large-scale polycrystal growth in veins (in 3D) is demonstrated enumerating the main advantages of adopting the novel approach.

Translation effects on vertical Bridgman growth and optical, mechanical and surface analysis of 2-phenylphenol single crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sadhasivam, S., E-mail: sadha.phy1@gmail.com; Perumal, Rajesh Narayana

2-phenylphenol optical crystals were grown in cone ampoules using vertical Bridgman technique. Single crystal of 2-phenylphenol with 150 mm length has been grown. The inclination on the conical part of the ampoule reduces the growth defects in the 2-phenylphenol single crystal. The lattice parameters and structure studied using single crystal X-ray diffraction method. 2-phenylphenol single crystal belongs to orthorhombic space group Fdd2. The micro translation rate affects crystal growth of 2-phenylphenol crystal was studied. The translation rate dependent defects present in the crystal were investigated by transmittance, indentation and etching characterizations. The dislocation induced indentation crack lengths variations were studied. Etchmore » pits and striations observed for the selective etchants furnish significant information on growth aspects and degree of defect present in the crystal.« less

High-temperature electronics

NASA Technical Reports Server (NTRS)

Matus, Lawrence G.; Seng, Gary T.

1990-01-01

To meet the needs of the aerospace propulsion and space power communities, the high temperature electronics program at the Lewis Research Center is developing silicon carbide (SiC) as a high temperature semiconductor material. This program supports a major element of the Center's mission - to perform basic and developmental research aimed at improving aerospace propulsion systems. Research is focused on developing the crystal growth, characterization, and device fabrication technologies necessary to produce a family of SiC devices.

Predicting crystal growth via a unified kinetic three-dimensional partition model

NASA Astrophysics Data System (ADS)

Anderson, Michael W.; Gebbie-Rayet, James T.; Hill, Adam R.; Farida, Nani; Attfield, Martin P.; Cubillas, Pablo; Blatov, Vladislav A.; Proserpio, Davide M.; Akporiaye, Duncan; Arstad, Bjørnar; Gale, Julian D.

2017-04-01

Understanding and predicting crystal growth is fundamental to the control of functionality in modern materials. Despite investigations for more than one hundred years, it is only recently that the molecular intricacies of these processes have been revealed by scanning probe microscopy. To organize and understand this large amount of new information, new rules for crystal growth need to be developed and tested. However, because of the complexity and variety of different crystal systems, attempts to understand crystal growth in detail have so far relied on developing models that are usually applicable to only one system. Such models cannot be used to achieve the wide scope of understanding that is required to create a unified model across crystal types and crystal structures. Here we describe a general approach to understanding and, in theory, predicting the growth of a wide range of crystal types, including the incorporation of defect structures, by simultaneous molecular-scale simulation of crystal habit and surface topology using a unified kinetic three-dimensional partition model. This entails dividing the structure into ‘natural tiles’ or Voronoi polyhedra that are metastable and, consequently, temporally persistent. As such, these units are then suitable for re-construction of the crystal via a Monte Carlo algorithm. We demonstrate our approach by predicting the crystal growth of a diverse set of crystal types, including zeolites, metal-organic frameworks, calcite, urea and L-cystine.

A Study of Biomolecules as Growth Modifiers of Calcium Oxalate Crystals

NASA Astrophysics Data System (ADS)

Kwak, Junha John

Crystallization processes are ubiquitous in nature, science, and technology. Controlling crystal growth is pivotal in many industries as material properties and functions can be tailored by tuning crystal habits (e.g. size, shape, phase). In biomineralization, organisms exert excellent control over bottom-up synthesis and assembly of inorganic-organic structures (e.g. bones, teeth, exoskeletons). This is made possible by growth modifiers that range from small molecules to macromolecules, such as proteins. Molecular recognition of the mineral phase allows proteins to function as nucleation templates, matrices, and growth inhibitors or promoters. We are interested in taking a biomimetic approach to control crystallization via biomolecular growth modifiers. We investigated calcium oxalate monohydrate (COM), found in plants and kidney stones, as a model system of crystallization. We studied the effects of four common proteins on COM crystallization: bovine serum albumin (BSA), transferrin, lactoferrin, and lysozyme. Through kinetic studies of COM crystallization, we classified BSA and lysozyme as COM growth inhibitor and promoter respectively. Their inhibition and promotion effects were also evident in the macroscopic crystal habit. Through adsorption and microscopy experiments, we showed that BSA exhibits binding specificity for the apical surfaces of macroscopic COM crystals. Lysozyme, on the other, functions via a non-binding mechanism at the surface to accelerate the growth of the apical surfaces. We also synthesized and studied peptides derived from the protein primary sequences to identify putative domains responsible for these inhibition and promotion effects. Collectively, our study of physiologically relevant biomolecules suggests potential roles of COM modifiers in pathological crystallization and helps to develop guidelines for rational design of biomolecular growth modifiers for applications in crystal engineering.

Determination of the rate of crystal growth from the gas phase under conditions of turbulent free convection

NASA Astrophysics Data System (ADS)

Alad'Ev, S. I.

1987-04-01

Crystal growth in vertical and horizontal cylindrical vials, with the substrate and the source serving as the vial ends, is investigated analytically, assuming that the medium consists of a binary mixture of an active and an inert gas. The active gas is made up of the gaseous products of reactions taking place at the substrate and at the source. It is shown that turbulent free convection leads to an increase in crystal growth rate. All other conditions being equal, crystal growth in vertical vials is greater than that in horizontal ones; in both cases crystal growth rate increases with the vial radius, temperature gradient in the gas phase, and gas phase density. The results are compared with experimental data on the growth of Ge crystals in the Ge-GeI4 system.

Control of Protein Crystal Nucleation and Growth Using Stirring Solution

NASA Astrophysics Data System (ADS)

Niino, Ai; Adachi, Hiroaki; Takano, Kazufumi; Matsumura, Hiroyoshi; Kinoshita, Takayoshi; Warizaya, Masaichi; Inoue, Tsuyoshi; Mori, Yusuke; Sasaki, Takatomo

2004-11-01

We have previously developed a protein crystallization technique using a stirring protein solution and revealed that (i) continuous stirring prevents excess spontaneous nucleation and accelerates the growth of protein crystals and (ii) prestirring (solution stirring in advance) promotes the crystal nucleation of hen egg-white lysozyme. In bovine adenosine deaminase (ADA) crystallization, continuous stirring improves the crystal quality but elongates the nucleation time. In this paper, in order to control both the crystal nucleation and growth of ADA using a Micro-Stirring technique, we carried out five different stirring patterns such as (i) no stirring, (ii) continuous stirring, (iii) prestirring, (iv) poststirring (stirring late in the growth period) and (v) restirring (combined pre- and poststirring). The results showed that high-quality well-shaped crystals were obtained under the continuous stirring and restirring conditions and the nucleation time under the prestirring and restirring conditions was shorter than that under the continuous stirring and poststirring conditions. Consequently, high-quality crystals were promptly obtained under the restirring condition. These results suggest that we are able to control both the nucleation and growth of protein crystals with the stirring techniques.

Physical phenomena related to crystal growth in the space environment

NASA Technical Reports Server (NTRS)

Chu, T. L.

1973-01-01

The mechanism of crystal growth which may be affected by the space environment was studied. Conclusions as to the relative technical and scientific advantages of crystal growth in space over earth bound growth, without regard to economic advantage, were deduced. It was concluded that the crucibleless technique will most directly demonstrate the unique effects of the greatly reduced gravity in the space environment. Several experiments, including crucibleless crystal growth using solar energy and determination of diffusion coefficients of common dopants in liquid silicon were recommended.

Study of Interesting Solidification Phenomena on the Ground and in Space (MEPHISTO)

NASA Technical Reports Server (NTRS)

Alexander, J. Iwan D.; Favier, J.-J.; Garandet, J.-P.

1999-01-01

Real-time Seebeck voltage variations in a Sn-Bi melt during directional solidification in the MEPHISTO spaceflight experiment flown on the USMP-3 mission, have been correlated with well-characterized thruster firings and an Orbiter Main System (OMS) burn. The Seebeck voltage measurement is related to the response of the instantaneous average melt composition at the melt-crystal interface. This allowed us to make a direct comparison of numerical simulations with the experimentally obtained Seebeck signals. Based on the results of preflight and real-time computations, several well-defined thruster firing events were programmed to occur at specific times during the experiment. In particular, we simulated the effects of the thruster firings on melt and crystal composition in a directionally solidifying Sn-Bi alloy. The relative accelerations produced by the firings were simulated by impulsive accelerations of the same magnitude, duration and orientation as the requested firings. A comparison of the simulation results with the Seebeck signal indicates that there is a good agreement between the two. This unique opportunity allows us to make the first quantitative characterization of actual g-jitter effects on an actual crystal growth experiment and to calibrate our models of g-jitter effects on crystal growth.

Study of Interesting Solidification Phenomena on the Ground and in Space (MEPHISTO)

NASA Technical Reports Server (NTRS)

Favier, J.-J.; Iwan, J.; Alexander, D.; Garandet, J.-P.

1998-01-01

Real-time Seebeck voltage variations in a Sn-Bi melt during directional solidification in the MEPHISTO spaceflight experiment flown on the USMP-3 mission, can be correlated with well characterized thruster firings and an Orbiter Main System (OMS) burn. The Seebeck voltage measurement is related to the response of the instantaneous average melt composition at the melt-crystal interface. This allowed us to make a direct comparison of numerical simulations with the experimentally obtained Seebeck signals. Based on the results of preflight and real-time computations, several well-defined thruster firing events were programmed to occur at specific times during the experiment. In particular, we simulated the effects of the thruster firings on melt and crystal composition in a directionally solidifying Sn-Bi alloy. The relative accelerations produced by the firings were simulated by impulsive accelerations of the same magnitude, duration and orientation as the requested firings. A comparison of the simulation results with the Seebeck signal indicates that there is a good agreement between the two. This unique opportunity allows us, for the first time, to quantitatively characterize actual g-jitter effects on an actual crystal growth experiment and to properly calibrate our models of g-jitter effects on crystal growth.

High density protein crystal growth

NASA Technical Reports Server (NTRS)

Rouleau, Robyn (Inventor); Hedden, Douglas Keith (Inventor); Delucas, Lawrence (Inventor)

2004-01-01

A protein crystal growth assembly including a crystal growth cell and further including a cell body having a top side and a bottom side and a first aperture defined therethrough, the cell body having opposing first and second sides and a second aperture defined therethrough. A cell barrel is disposed within the cell body, the cell barrel defining a cavity alignable with the first aperture of the cell body, the cell barrel being rotatable within the second aperture. A reservoir is coupled to the bottom side of the cell body and a cap having a top side is disposed on the top side of the cell body. The protein crystal growth assembly may be employed in methods including vapor diffusion crystallization, liquid to liquid crystallization, batch crystallization, and temperature induction batch mode crystallization.

Modeling of dislocation dynamics in germanium Czochralski growth

NASA Astrophysics Data System (ADS)

Artemyev, V. V.; Smirnov, A. D.; Kalaev, V. V.; Mamedov, V. M.; Sidko, A. P.; Podkopaev, O. I.; Kravtsova, E. D.; Shimansky, A. F.

2017-06-01

Obtaining very high-purity germanium crystals with low dislocation density is a practically difficult problem, which requires knowledge and experience in growth processes. Dislocation density is one of the most important parameters defining the quality of germanium crystal. In this paper, we have performed experimental study of dislocation density during 4-in. germanium crystal growth using the Czochralski method and comprehensive unsteady modeling of the same crystal growth processes, taking into account global heat transfer, melt flow and melt/crystal interface shape evolution. Thermal stresses in the crystal and their relaxation with generation of dislocations within the Alexander-Haasen model have been calculated simultaneously with crystallization dynamics. Comparison to experimental data showed reasonable agreement for the temperature, interface shape and dislocation density in the crystal between calculation and experiment.

Kinetics of calcium oxalate crystal formation in urine.

PubMed

Laube, Norbert; Klein, Florian; Bernsmann, Falk

2017-04-01

It is routinely observed that persons with increased urinary stone risk factors do not necessarily form uroliths. Furthermore, stone formers can present with urinalyses that do not reflect the clinical picture. We explain this discrepancy by differences in crystallization kinetics. In 1162 urines, crystallization of Ca-oxalate was induced according to the BONN-Risk-Index (BRI) method. The urine's relative light transmissivity (RLT) was recorded from 100 % at start of titration to 95 % due to nuclei formation and crystal growth. From the RLT changes, a measure of the thermodynamic inhibition threshold of crystal formation (BRI) and of crystal growth kinetics is derived ("turbidity slope" after crystallization onset). On average, subjects presenting with a low inhibition threshold, i.e., high BRI, also present significantly higher crystal growth rates compared with subjects in lower BRI classes. Only subjects in the highest BRI class show a lower growth rate than expected, probably due to a depletion of supersaturation by massive initial nucleation. With increasing thermodynamic risk of crystal formation (i.e., increasing BRI) due to an imbalance between inhibitors and promoters of crystal formation, an increase in the imbalance between inhibitors and promoters of crystal growth (i.e., increasing growth rate) is observed. Both lead to an increased urolith formation risk. Healthy subjects with increased BRI are an exception to this trend: their urine is thermodynamically prone to form stones, but they show a kinetic inhibition preventing nuclei from significant growth.

Effects of doping impurity and growth orientation on dislocation generation in GaAs crystals grown from the melt: A qualitative finite-element study

NASA Astrophysics Data System (ADS)

Zhu, X. A.; Tsai, C. T.

2000-09-01

Dislocations in gallium arsenide (GaAs) crystals are generated by excessive thermal stresses induced during the crystal growth process. The presence of dislocations has adverse effects on the performance and reliability of the GaAs-based devices. It is well known that dislocation density can be significantly reduced by doping impurity atoms into a GaAs crystal during its growth process. A viscoplastic constitutive equation that couples the microscopic dislocation density with the macroscopic plastic deformation is employed in a crystallographic finite element model for calculating the dislocation density generated in the GaAs crystal during its growth process. The dislocation density is considered as an internal state variable and the drag stress caused by doping impurity is included in this constitutive equation. A GaAs crystal grown by the vertical Bridgman process is adopted as an example to study the influences of doping impurity and growth orientation on dislocation generation. The calculated results show that doping impurity can significantly reduce the dislocation density generated in the crystal. The level of reduction is also influenced by the growth orientation during the crystal growth process.

Nanoscale-driven crystal growth of hexaferrite heterostructures for magnetoelectric tuning of microwave semiconductor integrated devices.

PubMed

Hu, Bolin; Chen, Zhaohui; Su, Zhijuan; Wang, Xian; Daigle, Andrew; Andalib, Parisa; Wolf, Jason; McHenry, Michael E; Chen, Yajie; Harris, Vincent G

2014-11-25

A nanoscale-driven crystal growth of magnetic hexaferrites was successfully demonstrated at low growth temperatures (25-40% lower than the temperatures required often for crystal growth). This outcome exhibits thermodynamic processes of crystal growth, allowing ease in fabrication of advanced multifunctional materials. Most importantly, the crystal growth technique is considered theoretically and experimentally to be universal and suitable for the growth of a wide range of diverse crystals. In the present experiment, the conical spin structure of Co2Y ferrite crystals was found to give rise to an intrinsic magnetoelectric effect. Our experiment reveals a remarkable increase in the conical phase transition temperature by ∼150 K for Co2Y ferrite, compared to 5-10 K of Zn2Y ferrites recently reported. The high quality Co2Y ferrite crystals, having low microwave loss and magnetoelectricity, were successfully grown on a wide bandgap semiconductor GaN. The demonstration of the nanostructure materials-based "system on a wafer" architecture is a critical milestone to next generation microwave integrated systems. It is also practical that future microwave integrated systems and their magnetic performances could be tuned by an electric field because of the magnetoelectricity of hexaferrites.

Colloidal crystal growth monitored by Bragg diffraction interference fringes.

PubMed

Bohn, Justin J; Tikhonov, Alexander; Asher, Sanford A

2010-10-15

We monitored the crystal growth kinetics of crystallization of a shear melted crystalline colloidal array (CCA). The fcc CCA heterogeneously nucleates at the flow cell wall surface. We examined the evolution of the (1 1 1) Bragg diffraction peak, and, for the first time, quantitatively monitored growth by measuring the temporal evolution of the Bragg diffraction interference fringes. Modeling of the evolution of the fringe patterns exposes the time dependence of the increasing crystal thickness. The initial diffusion-driven linear growth is followed by ripening-driven growth. Between 80 and 90 microM NaCl concentrations the fcc crystals first linearly grow at rates between 1.9 and 4.2 microm/s until they contact homogeneously nucleated crystals in the bulk. At lower salt concentrations interference fringes are not visible because the strong electrostatic interactions between particles result in high activation barriers, preventing defect annealing and leading to a lower crystal quality. The fcc crystals melt to a liquid phase at >90 microM NaCl concentrations. Increasing NaCl concentrations slow the fcc CCA growth rate consistent with the expectation of the classical Wilson-Frenkel growth theory. The final thickness of wall-nucleated CCA, that is determined by the competition between growth of heterogeneously and homogenously nucleated CCA, increases with higher NaCl concentrations. Copyright 2010 Elsevier Inc. All rights reserved.

The Biological Macromolecule Crystallization Database and NASA Protein Crystal Growth Archive

PubMed Central

Gilliland, Gary L.; Tung, Michael; Ladner, Jane

1996-01-01

The NIST/NASA/CARB Biological Macromolecule Crystallization Database (BMCD), NIST Standard Reference Database 21, contains crystal data and crystallization conditions for biological macromolecules. The database entries include data abstracted from published crystallographic reports. Each entry consists of information describing the biological macromolecule crystallized and crystal data and the crystallization conditions for each crystal form. The BMCD serves as the NASA Protein Crystal Growth Archive in that it contains protocols and results of crystallization experiments undertaken in microgravity (space). These database entries report the results, whether successful or not, from NASA-sponsored protein crystal growth experiments in microgravity and from microgravity crystallization studies sponsored by other international organizations. The BMCD was designed as a tool to assist x-ray crystallographers in the development of protocols to crystallize biological macromolecules, those that have previously been crystallized, and those that have not been crystallized. PMID:11542472

Magnetic Control of Convection during Protein Crystallization

NASA Technical Reports Server (NTRS)

Ramachandran, N.; Leslie, F. W.

2004-01-01

An important component in biotechnology, particularly in the area of protein engineering and rational drug design is the knowledge of the precise three-dimensional molecular structure of proteins. The quality of structural information obtained from X-ray diffraction methods is directly dependent on the degree of perfection of the protein crystals. As a consequence, the growth of high quality macromolecular Crystals for diffraction analyses has been the central focus for bio-chemists, biologists, and bioengineers. Macromolecular crystals are obtained from solutions that contain the crystallizing species in equilibrium with higher aggregates, ions, precipitants, other possible phases of the protein, foreign particles, the walls of container, and a likely host of other impurities. By changing transport modes in general, i.e., reduction of convection and Sedimentation as is achieved in "microgravity", we have been able to dramatically affect the movement and distribution of macromolecules in the fluid, and thus their transport, f o d o n of crystal nuclei, and adsorption to the crystal surface. While a limited number of high quality crystals from space flights have been obtained, as the recent National Research Council (NRC) review of the NASA microgravity crystallization program pointed out, the scientific approach and research in crystallization of proteins has been mainly empirical yielding inconclusive results. We postulate that we can reduce convection in ground-based experiments and we can understand the different aspects of convection control through the use of strong magnetic fields and field gradients. We postulate that limited convection in a magnetic field will provide the environment for the growth of high quality crystals. The approach exploits the variation of fluid magnetic susceptibility with counteracts on for this purpose and the convective damping is realized by appropriately positioning the crystal growth cell so that the magnetic susceptibility force counteract terrestrial gravity. The genera1 objective is to test the hypothesis of convective control using a strong magnetic field and magnetic field gradient and to understand the nature of the various forces that come into play. Specifically we aim to delineate causative factors and to quantify them through experiments, analysis and numerical modeling. The paper will report on the experimental results using paramagentic salts and solutions in magnetic fields and compare them to analyticalprctions.

Convection effects in protein crystal growth

NASA Technical Reports Server (NTRS)

Roberts, Glyn O.

1988-01-01

Protein crystals for X-ray diffraction study are usually grown resting on the bottom of a hanging drop of a saturated protein solution, with slow evaporation to the air in a small enclosed cell. The evaporation rate is controlled by hanging the drop above a reservoir of water, with its saturation vapor pressure decreased by a low concentration of a passive solute. The drop has a lower solute concentration, and its volume shrinks by evaporation until the molecular concentrations match. Protein crystals can also be grown from a seed crystal suspended or supported in the interior of a supersaturated solution. The main analysis of this report concerns this case because it is less complicated than hanging-drop growth. Convection effects have been suggested as the reason for the apparent cessation of growth at a certain rather small crystal size. It seeems that as the crystal grows, the number of dislocations increases to a point where further growth is hindered. Growth in the microgravity environment of an orbiting space vehicle has been proposed as a method for obtaining larger crystals. Experimental observations of convection effects during the growth of protein crystals have been reported.

Lattice Boltzmann Simulation of Kinetic Isotope Effect During Snow Crystal Formation

NASA Astrophysics Data System (ADS)

Lu, G.; Depaolo, D. J.; Kang, Q.; Zhang, D.

2007-12-01

The isotopic composition of precipitation, especially that of snow, plays a special role in the global hydrological cycle and in reconstruction of past climates using polar ice cores. The fractionation of the major water isotope species (HHO, HDO, HHO-18) during ice crystal formation is critical to understanding the global distribution of isotopes in precipitation. Ice crystal growth in clouds is traditionally treated with a spherically-symmetric steady state diffusion model, with semi-empirical modifications added to account for ventilation and for complex crystal morphology. Although it is known that crystal growth rate, which depends largely on the degree of vapor over- saturation, determines crystal morphology, there are no quantitative models that relate morphology to the vapor saturation factor. Since kinetic (vapor phase diffusion-controlled) isotopic fractionation also depends on growth rate, there should be direct relationships between vapor saturation, crystal morphology, and crystal isotopic composition. We use a 2D lattice Boltzmann model to simulate diffusion-controlled ice crystal growth from vapor- oversaturated air. In the model, crystals grow solely according to the diffusive fluxes just above the crystal surfaces, and hence crystal morphology arises from the initial and boundary conditions in the model and does not need to be specified a priori. Crystal growth patterns can be varied between random growth and deterministic growth (along the maximum concentration gradient for example). The input parameters needed are the isotope- dependent vapor deposition rate constant (k) and the water vapor diffusivity in air (D). The values of both k and D can be computed from kinetic theory, and there are also experimentally determined values of D. The deduced values of k are uncertain to the extent that the condensation coefficient for ice is uncertain. The ratio D/k is a length (order 1 micron) that determines the minimum scale of dendritic growth features and allows us to scale the numerical calculations to atmospheric conditions. Our calculations confirm that the crystal/vapor isotopic fractionation approaches the equilibrium value, and the crystals are compact (circular in 2D) as the saturation factor approaches unity (S= 1.0). However, few natural crystals form under such conditions. At higher oversaturation (e.g. S = 1.2), dendritic crystals of millimeter size develop on timescales appropriate to cloud processes, and kinetic effects control isotopic fractionation. Fractionation factors for dendritic crystals are similar to those predicted by the spherical diffusion model, but the model also gives estimates of crystal heterogeneity. Dendritic crystals are constrained to be relatively large, with dimension much greater than about 20D/k. The most difficult aspect of the modeling is to account for the large density difference between air and ice, which requires us to use a fictitious higher density for the vapor-oversaturated air and scale the crystal growth time accordingly. An approach using a larger scale simulation and the domain decomposition method can provide a vapor flux for a nested smaller scale calculation. The results clarify the controls on crystal growth, and the relationships between saturation state, growth rate, crystal morphology and isotopic fractionation.

Single crystals of selected titanates and tungstates

NASA Technical Reports Server (NTRS)

Loiacono, G. M.

1972-01-01

The compound preparation and crystal growth of a number of mixed titanate compositions was investigated. None of the compounds studied were found to melt congruently and therefore, crystal growth was extremely difficult. Various single crystal preparation methods always resulted in mixed phases from which 1-2 mm size crystals could be separated. It is concluded from this study that before successful single crystal growth can be accomplished, a detailed study of the phase diagrams in each of the systems of interest must be completed.

A simple apparatus for controlling nucleation and size in protein crystal growth

NASA Technical Reports Server (NTRS)

Gernert, Kim M.; Smith, Robert; Carter, Daniel C.

1988-01-01

A simple device is described for controlling vapor equilibrium in macromolecular crystallization as applied to the protein crystal growth technique commonly referred to as the 'hanging drop' method. Crystal growth experiments with hen egg white lysozyme have demonstrated control of the nucleation rate. Nucleation rate and final crystal size have been found to be highly dependent upon the rate at which critical supersaturation is approached. Slower approaches show a marked decrease in the nucleation rate and an increase in crystal size.

Effects of cyclic structure inhibitors on the morphology and growth of tetrahydrofuran hydrate crystals

NASA Astrophysics Data System (ADS)

Li, Sijia; Wang, Yanhong; Lang, Xuemei; Fan, Shuanshi

2013-08-01

Morphology and growth of hydrate crystals with cyclic structure inhibitors at a hydrate-liquid interface were directly observed through a microscopic manipulating apparatus. Tetrahydrofuran (THF) hydrate was employed as an objective. The effects of four kind of cyclic structure inhibitors, polyvinylpyrrolidone (PVP), poly(N-vinyl-2-pyrrolidone-co-2-vinyl pyridine) (PVPP), poly(2-vinyl pyridine-co-N-vinylcaprolactam) (PVPC) and poly(N-vinylcaprolactam) (PVCap), were investigated. Morphological patterns between each hydrate crystal growth from hydrate-liquid interface into droplet were found differ significantly. Lamellar structure growth of hydrate crystal was observed without inhibitor, while with PVP was featheriness-like, PVPP was like long dendritic crystal, PVPC was Mimosa pudica leaf-like and PVCap was like weeds. The growth rate of hydrate crystal without inhibitor was 0.00498 mm3/s, while with PVPP, PVPC and PVCap, were 0.00339 mm3/s, 0.00350 mm3/s, 0.00386 mm3/s and 0.00426 mm3/s, respectively. Cyclic structure inhibitors can decrease the growth rate, degree of reduction in growth rate of hydrate crystals decrease with the increase of cylinder number.

Fabrication of graded index single crystal in glass

PubMed Central

Veenhuizen, Keith; McAnany, Sean; Nolan, Daniel; Aitken, Bruce; Dierolf, Volkmar; Jain, Himanshu

2017-01-01

Lithium niobate crystals were grown in 3D through localized heating by femtosecond laser irradiation deep inside 35Li2O-35Nb2O5-30SiO2 glass. Laser scanning speed and power density were systematically varied to control the crystal growth process and determine the optimal conditions for the formation of single crystal lines. EBSD measurements showed that, in principle, single crystals can be grown to unlimited lengths using optimal parameters. We successfully tuned the parameters to a growth mode where nucleation and growth occur upon heating and ahead of the scanning laser focus. This growth mode eliminates the problem reported in previous works of non-uniform polycrystallinity because of a separate growth mode where crystallization occurs during cooling behind the scanning laser focus. To our knowledge, this is the first report of such a growth mode using a fs laser. The crystal cross-sections possessed a symmetric, smooth lattice misorientation with respect to the c-axis orientation in the center of the crystal. Calculations indicate the observed misorientation leads to a decrease in the refractive index of the crystal line from the center moving outwards, opening the possibility to produce within glass a graded refractive index single crystal (GRISC) optically active waveguide. PMID:28287174

Modelling the growth of feather crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wood, H.J.; Hunt, J.D.; Evans, P.V.

1997-02-01

An existing numerical model of dendritic growth has been adapted to model the growth of twinned columnar dendrites (feather crystals) in a binary aluminium alloy, Examination of the effect of dendrite tip angle on growth has led to an hypothesis regarding the stability of a pointed tip morphology in these crystals.

Growth of triglycine sulfate (TGS) crystals by solution technique

NASA Technical Reports Server (NTRS)

Lal, R. B.; Kroes, R. L.; Wilcox, W. R.

1982-01-01

The growth of crystals from solution is greatly influenced by buoyancy driven convection. In a low-g environment, convection is greatly suppressed and diffusion becomes the predominant mechanism for thermal and mass transport. An experiment to grow TGS crystals by solution technique during the orbital Spacelab III mission has been designed. Crystals are grown by a new and unique technique of extracting heat from the crystal through a sting. The cooling at the sting tip is responsible for the desired supersaturation near the growing crystal. Calculations indicate that the cooled sting technique for solution crystal growth is necessary in low-g to maintain a maximum growth rate of 1 mm/day. Results of groundbased work in support of the flight experiment are discussed.

Ground based experiments on the growth and characterization of L-Arginine Phosphate (LAP) crystals

NASA Technical Reports Server (NTRS)

Rao, S. M.; Cao, C.; Batra, A. K.; Lal, R. B.; Mookherji, T. K.

1991-01-01

L-Arginine Phosphate (LAP) is a new nonlinear optical material with higher efficiency for harmonic generation compared to KDP. Crystals of LAP were grown in the laboratory from supersaturated solutions by temperature lowering technique. Investigations revealed the presence of large dislocation densities inside the crystals which are observed to produce refractive index changes causing damage at high laser powers. This is a result of the convection during crystal growth from supersaturated solutions. It is proposed to grow these crystals in a diffusion controlled growth condition under microgravity environment and compare the crystals grown in space with those grown on ground. Physical properties of the solutions needed for modelling of crystal growth are also presented.

Hydrothermal crystal growth of ABe 2BO 3F 2 (A=K, Rb, Cs, Tl) NLO crystals

NASA Astrophysics Data System (ADS)

McMillen, Colin D.; Kolis, Joseph W.

2008-04-01

Crystals of a family of compounds, ABe 2BO 3F 2 (ABBF, A=K, Rb, Cs, Tl), have been grown hydrothermally. Each of these materials was studied using the powder SHG technique and exhibited promising NLO behavior. Seeded crystal growth was demonstrated and the growth conditions were optimized by modifying the temperature, thermal gradient and mineralizer concentration. RbBe 2BO 3F 2 crystals possessed a particularly good combination of SHG intensity, favorable crystal habit and fast growth rates. High quality crystals suitable for advanced deep-UV NLO studies were grown at rates of 0.11 mm/day on (0 0 1) and 0.12 mm/day perpendicular to (0 0 1).

El Paso/Yslete schools Get-Away Special Space Shuttle student projects

NASA Technical Reports Server (NTRS)

Azar, S. S.

1984-01-01

Student projects for the Get Away Special (GAS) space shuttle program were summarized. Experimental topics included: seed germination, shrimp growth, liquid lasers, planaria regeneration, fluid dynamics (wicking), soil molds, antibiotics, crystallization, the symbiosis of yeast and fungi, and the performance of electronic chips. A brief experimental design is included for each project.

A theoretical model describing the one-dimensional growth of single crystals on free sustained substrates

NASA Astrophysics Data System (ADS)

Ye, Ziran; Wang, Ke; Lu, Chenxi; Jin, Ying; Sui, Chenghua; Yan, Bo; Gao, Fan; Cai, Pinggen; Lv, Bin; Li, Yun; Chen, Naibo; Sun, Guofang; Xu, Fengyun; Ye, Gaoxiang

2018-03-01

We develop a theoretical model that interprets the growth mechanism of zinc (Zn) crystal nanorods on a liquid substrate by thermal evaporation. During deposition, Zn atoms diffuse randomly on an isotropic and quasi-free sustained substrate, the nucleation of the atoms results in the primary nanorod (or seed crystal) growth. Subsequently, a characteristic one-dimensional atomic aggregation is proposed, which leads to the accelerating growth of the crystal nanorod along its preferential growth direction until the growth terminates. The theoretical results are in good agreement with the experimental findings.

Advantages of a Special Post-Growth THM Program for the Reduction of Inclusions in CdTe Crystals

NASA Astrophysics Data System (ADS)

Fochuk, P.; Zakharuk, Z.; Nykonyuk, Ye.; Rarenko, A.; Kolesnik, M.; Bolotnikov, A. E.; Yang, G.; James, R. B.

2016-06-01

CdTe crystals are used widely for manufacturing gamma-ray radiation sensors, and we can improve their properties if we eliminate as many as possible of their Te inclusions. In this paper, we describe our two modes of removing them; first, we used the traveling heater method for growing them, and then we applied post-growth cooling, for which we used a special slow-cooling program. Here, we placed the CdTe ingot, containing inclusions, into a quartz container, and moved a narrow heater zone along it. The molten inclusions moved together with the hot zone, and, at end of the process, they were concentrated heavily at the ingot's surface. Consequently, very few inclusions were observed in much of the CdTe ingot. Hall effect measurements showed that after such annealing the value of the carrier mobility was increased significantly, and the concentration of ionized centers was reduced. One major advantage of this treatment, compared to thermal annealing alone, is that both the inclusions and impurities are eliminated simultaneously.

Mechanisms of protein and virus crystal growth: An atomic force microscopy study of canavalin and STMV crystallization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Land, T.A.; De Yoreo, J.J.; Malkin, A.J.

1996-05-01

The evolution of surface morphology and step dynamics during growth of rhombohedral crystals of the protein canavalin and crystals of the cubic satellite tobacco mosaic virus (STMV) have been investigated for the first time by in situ atomic force microscopy. These two crystals were observed to grow by very different mechanisms. Growth of canavalin occurs on complex vicinal hillocks formed by multiple, independently acting screw dislocations. Small clusters were observed on the terraces. STMV on the other hand, was observed to grow by 2D nucleation of islands. No dislocations were found on the crystal. The results are used to determinemore » the growth mechanisms and estimate the fundamental materials parameters. The images also illustrate the important mechanism of defect incorporation and provide insight to the processes that limit the growth rate and uniformity of these crystals.« less

DKDP crystal growth controlled by cooling rate

NASA Astrophysics Data System (ADS)

Xie, Xiaoyi; Qi, Hongji; Shao, Jianda

2017-08-01

The performance of deuterated potassium dihydrogen phosphate (DKDP) crystal directly affects beam quality, energy and conversion efficiency in the Inertial Confinement Fusion（ICF）facility, which is related with the initial saturation temperature of solution and the real-time supersaturation during the crystal growth. However, traditional method to measure the saturation temperature is neither efficient nor accurate enough. Besides, the supersaturation is often controlled by experience, which yields the higher error and leads to the instability during the crystal growth. In this paper, DKDP solution with 78% deuteration concentration is crystallized in different temperatures. We study the relation between solubility and temperature of DKDP and fit a theoretical curve with a parabola model. With the model, the measurement of saturation temperature is simplified and the control precision of the cooling rate is improved during the crystal growth, which is beneficial for optimizing the crystal growth process.

Crystal growth methods dedicated to low solubility actinide oxalates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tamain, C., E-mail: christelle.tamain@cea.fr; Arab-Chapelet, B.; Rivenet, M.

Two novel crystal growth syntheses dedicated to low solubility actinide-oxalate systems and adapted to glove box handling are described. These methods based on the use of precursors of either actinide metal or oxalic acid have been optimized on lanthanide systems (analogue of actinides(III)) and then assessed on real actinide systems. They allow the synthesis of several actinide oxalate single crystals, Am{sub 2}(C{sub 2}O{sub 4}){sub 3}(H{sub 2}O){sub 3}·xH{sub 2}O, Th(C{sub 2}O{sub 4}){sub 2}·6H{sub 2}O, M{sub 2+x}[Pu{sup IV}{sub 2−x}Pu{sup III}{sub x}(C{sub 2}O{sub 4}){sub 5}]·nH{sub 2}O and M{sub 1−x}[Pu{sup III}{sub 1−x}Pu{sup IV}{sub x}(C{sub 2}O{sub 4}){sub 2}·H{sub 2}O]·nH{sub 2}O. It is the first timemore » that these well-known compounds are formed by crystal growth methods, thus enabling direct structural studies on transuranic element systems and acquisition of basic data beyond deductions from isomorphic (or not) lanthanide compounds. Characterizations by X-ray diffraction, UV–visible solid spectroscopy, demonstrate the potentialities of these two crystal growth methods to obtain oxalate compounds. - Graphical abstract: Two new single crystal growth methods dedicated to actinide oxalate compounds. - Highlights: • Use of diester as oxalate precursor for crystal growth of actinide oxalates. • Use of actinide oxide as precursor for crystal growth of actinide oxalates. • Crystal growth of Pu(III) and Am(III) oxalates. • Crystal growth of mixed Pu(III)/Pu(IV) oxalates.« less

Crystallization kinetics of the phase change material GeSb 6Te measured with dynamic transmission electron microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Winseck, M. M.; Cheng, H. -Y.; Campbell, G. H.

2016-03-30

GeSb 6Te is a chalcogenide-based phase change material that has shown great ptoential for use in solid-state memory devices. The crystallization kinetics of amorphous thin films of GeSb 6Te during laser crystallization were followed with dynamic transmission electron microscopy, a photo-emission electron microscopy technique with nanosecond-scale time resolution. Nine-frame movies of crystal growth were taken during laser crystallization. The nucleation rate is observed to be very low and the growth rates are very high, up to 10.8 m s –1 for amorphous as-deposited films and significantly higher for an amorphous film subject to sub-threshold laser annealing before crystallization. The measuredmore » growth rates exceed any directly measured growth rate of a phase change material. Here, the crystallization is reminiscent of explosive crystallization of elemental semiconductors both in the magnitude of the growth rate and in the resulting crystalline microstructures.« less

Protein crystal growth results from the United States Microgravity Laboratory-1 mission

NASA Technical Reports Server (NTRS)

Delucas, Lawrence J.; Moore, K. M.; Vanderwoerd, M.; Bray, T. L.; Smith, C.; Carson, M.; Narayana, S. V. L.; Rosenblum, W. M.; Carter, D.; Clark, A. D, Jr.

1994-01-01

Protein crystal growth experiments have been performed by this laboratory on 18 Space Shuttle missions since April, 1985. In addition, a number of microgravity experiments also have been performed and reported by other investigators. These Space Shuttle missions have been used to grow crystals of a variety of proteins using vapor diffusion, liquid diffusion, and temperature-induced crystallization techniques. The United States Microgravity Laboratory - 1 mission (USML-1, June 25 - July 9, 1992) was a Spacelab mission dedicated to experiments involved in materials processing. New protein crystal growth hardware was developed to allow in orbit examination of initial crystal growth results, the knowledge from which was used on subsequent days to prepare new crystal growth experiments. In addition, new seeding hardware and techniques were tested as well as techniques that would prepare crystals for analysis by x-ray diffraction, a capability projected for the planned Space Station. Hardware that was specifically developed for the USML-1 mission will be discussed along with the experimental results from this mission.

Semiconductor Crystal Growth in Static and Rotating Magnetic fields

NASA Technical Reports Server (NTRS)

Volz, Martin

2004-01-01

Magnetic fields have been applied during the growth of bulk semiconductor crystals to control the convective flow behavior of the melt. A static magnetic field established Lorentz forces which tend to reduce the convective intensity in the melt. At sufficiently high magnetic field strengths, a boundary layer is established ahead of the solid-liquid interface where mass transport is dominated by diffusion. This can have a significant effect on segregation behavior and can eliminate striations in grown crystals resulting from convective instabilities. Experiments on dilute (Ge:Ga) and solid solution (Ge-Si) semiconductor systems show a transition from a completely mixed convective state to a diffusion-controlled state between 0 and 5 Tesla. In HgCdTe, radial segregation approached the diffusion limited regime and the curvature of the solid-liquid interface was reduced by a factor of 3 during growth in magnetic fields in excess of 0.5 Tesla. Convection can also be controlled during growth at reduced gravitational levels. However, the direction of the residual steady-state acceleration vector can compromise this effect if it cannot be controlled. A magnetic field in reduced gravity can suppress disturbances caused by residual transverse accelerations and by random non-steady accelerations. Indeed, a joint program between NASA and the NHMFL resulted in the construction of a prototype spaceflight magnet for crystal growth applications. An alternative to the suppression of convection by static magnetic fields and reduced gravity is the imposition of controlled steady flow generated by rotating magnetic fields (RMF)'s. The potential benefits of an RMF include homogenization of the melt temperature and concentration distribution, and control of the solid-liquid interface shape. Adjusting the strength and frequency of the applied magnetic field allows tailoring of the resultant flow field. A limitation of RMF's is that they introduce deleterious instabilities above a critical magnetic field value. Growth conditions in which static magnetic fields rotational magnetic fields, and reduced gravitational levels can have a beneficial role will be described.

Zircon growth in shear zones

NASA Astrophysics Data System (ADS)

Kaulina, Tatiana

2013-04-01

The possibility of direct dating of the deformation process is critical for understanding of orogenic belts evolution. Establishing the age of deformation by isotopic methods is indispensable in the case of uneven deformation overlapping, when later deformation inherits the structural plan of the early strains, and to distinguish them on the basis of the structural data only is impossible. A good example of zircon from the shear zones is zircon formed under the eclogite facies conditions. On the one hand, the composition of zircon speaks about its formation simultaneously to eclogitic paragenesis (Rubatto, Herman, 1999; Rubatto et al., 2003). On the other hand, geological studies show that mineral reactions of eclogitization are often held only in areas of shear deformations, which provides access of fluid to the rocks (Austrheim, 1987; Jamtveit et al., 2000; Bingen et al., 2004). Zircons from mafic and ultramafic rocks of the Tanaelv and Kolvitsa belts (Kola Peninsula, the Baltic Shield) have showed that the metamorphic zircon growth is probably controlled by the metamorphic fluid regime, as evidenced by an increase of zircon quantity with the degree of shearing. The internal structure of zircon crystals can provide an evidence of zircon growth synchronous with shearing. The studied crystals have a sector zoning and often specific "patchy" zoning (Fig. 1), which speaks about rapid change of growth conditions. Such internal structure can be compared with the "snowball" garnet structure reflecting the rotation of crystals during their growth under a shift. Rapidly changing crystallization conditions can also be associated with a small amount of fluid, where supersaturation is changing even at a constant temperature. Thus, the growth of metamorphic zircon in shear zones is more likely to occur in the fluid flow synchronous with deformation. A distinctive feature of zircons in these conditions is isometric shape and sector "patchy" zoning. The work was supported by Russian Foundation of Basic Research (project: 13-05-00035.) and the DES-6 program.

Experiment Requirements and Implementation Plan (ERIP) for semiconductor materials growth in low-G environment experiment no. MPS-77F087

NASA Technical Reports Server (NTRS)

Crouch, R. K.; Fripp, A. L.; Debnam, W. J.; Clark, I. O.

1981-01-01

Crystals of the intermetallic compound Pb1-xSnxTe will be grown in furnaces on the Space Shuttle. The reasons for conducting this growth in space, the program of investigation to develop the space experiment and the requirements that are placed on the Space Shuttle furnace are discussed. Also included are relevent thermophysical properties of Pb1-xSnxTe to the degree which they are known.

Shape Evolution of Detached Bridgman Crystals Grown in Microgravity

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.

2015-01-01

A theory describing the shape evolution of detached Bridgman crystals in microgravity has been developed. A starting crystal of initial radius r0 will evolve to one of the following states: Stable detached gap; Attachment to the crucible wall; Meniscus collapse. Only crystals where alpha plus omega is great than 180 degrees will achieve stable detached growth in microgravity. Results of the crystal shape evolution theory are consistent with predictions of the dynamic stability of crystallization (Tatarchenko, Shaped Crystal Growth, Kluwer, 1993). Tests of transient crystal evolution are planned for ICESAGE, a series of Ge and GeSi crystal growth experiments planned to be conducted on the International Space Station (ISS).

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patil, Vidya, E-mail: vidya.patil@ruparel.edu; Patki, Mugdha, E-mail: mugdha.patki@ruparel.edu

Many nonlinear optical (NLO) crystals have been identified as potential candidates in optical and electro-optical devices. Use of NLO organic crystals is expected in photonic applications. Hence organic nonlinear optical materials have been intensely investigated due to their potentially high nonlinearities, and rapid response in electro-optic effect compared to inorganic NLO materials. There are many methods to grow organic crystals such as vapor growth method, melt growth method and solution growth method. Out of these methods, solution growth method is useful in providing constraint free crystal. Single crystals of Dopamine have been grown by evaporating the solvents from aqueous solution.more » Crystals obtained were of the size of orders of mm. The crystal structure of dopamine was determined using XRD technique. Images of crystals were obtained using FEG SEM Quanta Series under high vacuum and low KV.« less

Advanced Protein Crystallization Facility (APCF)

NASA Technical Reports Server (NTRS)

1998-01-01

This section of the Life and Microgravity Spacelab (LMS) publication contains articles entitled: (1) Crystallization of EGFR-EGF; (2) Crystallization of Apocrustacyanin C1; (3) Crystallization and X-ray Analysis of 5S rRNA and the 5S rRNA Domain A; (4) Growth of Lysozyme Crystals at Low Nucleation Density; (5) Comparative Analysis of Aspartyl tRNA-synthetase and Thaumatin Crystals Grown on Earth and In Microgravity; (6) Lysosome Crystal Growth in the Advanced Protein Crystallization Facility Monitored via Mach-Zehnder Interferometry and CCD Video; (7) Analysis of Thaumatin Crystals Grown on Earth and in Microgravity; (8) Crystallization of the Nucleosome Core Particle; (9) Crystallization of Photosystem I; (10) Mechanism of Membrane Protein Crystal Growth: Bacteriorhodopsin-mixed Micelle Packing at the Consolution Boundary, Stabilized in Microgravity; (11) Crystallization in a Microgravity Environment of CcdB, a Protein Involved in the Control of Cell Death; and (12) Crystallization of Sulfolobus Solfataricus

Investigation of crystal growth in zero gravity environment and investigation of metallic whiskers

NASA Technical Reports Server (NTRS)

Davis, J. H.; Lal, R. B.; Walter, H. U.; Castle, J. G., Jr.

1972-01-01

Theoretical and experimental work reported relates to the effects of near-zero gravity on growths of crystals and metallic whiskers during Skylab and Apollo flight experiments. Studies on growth and characterization of candidate materials for flight experiments cover indium-bismuth compounds, bismuth single crystals, gallium arsenide films and single crystals, and cadmium whiskers.

Theoretical and experimental morphologies of 4-aminobenzophenone (ABP) crystals

NASA Astrophysics Data System (ADS)

Wang, Qingwu; Sheen, D. B.; Shepherd, E. E. A.; Sherwood, J. N.; Simpson, G. S.; Hammond, R. B.

1997-11-01

The lattice energy (Elatt), slice energies (Eslice) and attachment energies (Eatt) of the different habit faces of ABP crystals have been calculated using the computer program HABIT. On the basis of the attachment energies of different crystal faces, the morphology was defined as {1 0 0}, {0 0 1}, {1 1 0}, {11bar0} and {1 01bar}. To confirm this theoretical prediction, we have grown ABP films and ABP crystals from the vapour phase. In both cases, the morphologically most important face was defined as {1 0 0} face using X-ray diffraction techniques. The remaining faces of the vapour-grown crystals were defined using a projection method, while the crystallites in the films were morphologically analysed by means of atomic force microscopy (AFM). The experimental morphologies are basically in agreement with the computation. Deviations from the equilibrium morphology can be ascribed to departure from equilibrium conditions during growth. For completeness, the results are compared with those for crystals grown from solutions for which deviations in morphology from the theoretical predictions can be ascribed to interaction between the crystal faces and solvent molecules.

The effect of tailor-made additives on crystal growth of methyl paraben: Experiments and modelling

NASA Astrophysics Data System (ADS)

Cai, Zhihui; Liu, Yong; Song, Yang; Guan, Guoqiang; Jiang, Yanbin

2017-03-01

In this study, methyl paraben (MP) was selected as the model component, and acetaminophen (APAP), p-methyl acetanilide (PMAA) and acetanilide (ACET), which share the similar molecular structure as MP, were selected as the three tailor-made additives to study the effect of tailor-made additives on the crystal growth of MP. HPLC results indicated that the MP crystals induced by the three additives contained MP only. Photographs of the single crystals prepared indicated that the morphology of the MP crystals was greatly changed by the additives, but PXRD and single crystal diffraction results illustrated that the MP crystals were the same polymorph only with different crystal habits, and no new crystal form was found compared with other references. To investigate the effect of the additives on the crystal growth, the interaction between additives and facets was discussed in detail using the DFT methods and MD simulations. The results showed that APAP, PMAA and ACET would be selectively adsorbed on the growth surfaces of the crystal facets, which induced the change in MP crystal habits.

Automated protein crystal growth facility

NASA Astrophysics Data System (ADS)

Donald, Stacey

A customer for the protein crystal growth facility fills the specially designed chamber with the correct solutions, fills the syringes with their quenching solutions, and submits the data needed for the proper growth of their crystal. To make sure that the chambers and syringes are filled correctly, a NASA representative may assist the customer. The data needed is the approximate growth time, the growth temperature, and the desired crystal size, but this data can be changed anytime from the ground, if needed. The chambers are gathered and placed into numbered slots in special drawers. Then, data is entered into a computer for each of the chambers. Technicians map out when each chamber's growth should be activated so that all of the chambers have enough time to grow. All of this data is up-linked to the space station when the previous growth session is over. Anti-vibrational containers need to be constructed for the high forces encountered during the lift off and the landing of the space shuttle, and though our team has not designed these containers, we do not feel that there is any reason why a suitable one could not be made. When the shuttle reaches the space station, an astronaut removes a drawer of quenched chambers from the growth facility and inserts a drawer of new chambers. All twelve of the drawers can be replaced in this fashion. The optical disks can also be removed this way. The old drawers are stored for the trip back to earth. Once inside the growth facility, a chamber is removed by the robot and placed in one of 144 active sites at a time previously picked by a technician. Growth begins when the chamber is inserted into an active site. Then, the sensing system starts to determine the size of the protein crystal. All during the crystal's growth, the customer can view the crystal and read all of the crystal's data, such as growth rate and crystal size. When the sensing system determines that the crystal has reached the predetermined size, the robot is told to pick up a syringe filled with the correct quenchant solution and inject it into the chamber to stop the crystal growth. The chamber is then removed from the active site and placed into its original storage slot.

Automated protein crystal growth facility

NASA Technical Reports Server (NTRS)

Donald, Stacey

1994-01-01

A customer for the protein crystal growth facility fills the specially designed chamber with the correct solutions, fills the syringes with their quenching solutions, and submits the data needed for the proper growth of their crystal. To make sure that the chambers and syringes are filled correctly, a NASA representative may assist the customer. The data needed is the approximate growth time, the growth temperature, and the desired crystal size, but this data can be changed anytime from the ground, if needed. The chambers are gathered and placed into numbered slots in special drawers. Then, data is entered into a computer for each of the chambers. Technicians map out when each chamber's growth should be activated so that all of the chambers have enough time to grow. All of this data is up-linked to the space station when the previous growth session is over. Anti-vibrational containers need to be constructed for the high forces encountered during the lift off and the landing of the space shuttle, and though our team has not designed these containers, we do not feel that there is any reason why a suitable one could not be made. When the shuttle reaches the space station, an astronaut removes a drawer of quenched chambers from the growth facility and inserts a drawer of new chambers. All twelve of the drawers can be replaced in this fashion. The optical disks can also be removed this way. The old drawers are stored for the trip back to earth. Once inside the growth facility, a chamber is removed by the robot and placed in one of 144 active sites at a time previously picked by a technician. Growth begins when the chamber is inserted into an active site. Then, the sensing system starts to determine the size of the protein crystal. All during the crystal's growth, the customer can view the crystal and read all of the crystal's data, such as growth rate and crystal size. When the sensing system determines that the crystal has reached the predetermined size, the robot is told to pick up a syringe filled with the correct quenchant solution and inject it into the chamber to stop the crystal growth. The chamber is then removed from the active site and placed into its original storage slot. Another chamber is then placed into the active site and the process is repeated in all of the active sites until all of the chambers have complted their growth. After ninety days (the scheduled time between shuttle visits), the crystal growth is completed, and the old drawers are replaced with new ones. Once the customer extracts the crystals, the chambers are retrieved for future customers.

Silicon web process development. [for low cost solar cells

NASA Technical Reports Server (NTRS)

Duncan, C. S.; Hopkins, R. H.; Seidensticker, R. G.; Mchugh, J. P.; Hill, F. E.; Heimlich, M. E.; Driggers, J. M.

1979-01-01

Silicon dendritic web, a single crystal ribbon shaped during growth by crystallographic forces and surface tension (rather than dies), is a highly promising base material for efficient low cost solar cells. The form of the product smooth, flexible strips 100 to 200 microns thick, conserves expensive silicon and facilitates automation of crystal growth and the subsequent manufacturing of solar cells. These characteristics, coupled with the highest demonstrated ribbon solar cell efficiency-15.5%-make silicon web a leading candidate to achieve, or better, the 1986 Low Cost Solar Array (LSA) Project cost objective of 50 cents per peak watt of photovoltaic output power. The main objective of the Web Program, technology development to significantly increase web output rate, and to show the feasibility for simultaneous melt replenishment and growth, have largely been accomplished. Recently, web output rates of 23.6 sq cm/min, nearly three times the 8 sq cm/min maximum rate of a year ago, were achieved. Webs 4 cm wide or greater were grown on a number of occassions.

Follow up on the crystal growth experiments of the LDEF

NASA Technical Reports Server (NTRS)

Nielsen, K. F.; Lind, M. D.

1993-01-01

The results of the 4 solution growth experiments on the LDEF have been published elsewhere. Both the crystals of CaCO3, which were large and well shaped, and the much smaller TTF-TCNQ crystals showed unusual morphological behavior. The follow up on these experiments was begun in 1981, when ESA initiated a 'Concept Definition Study' on a large, 150 kg, Solution Growth Facility (SGF) to be included in the payload of EURECA-1, the European Retrievable Carrier. This carrier was a continuation of the European Spacelab and at that time planned for launch in 1987. The long delay of the LDEF retrieval and of subsequent missions brought about reflections both on the concept of crystal growth in space and on the choice of crystallization materials that had been made for the LDEF. Already before the LDEF retrieval, research on TTF-TCNQ had been stopped, and a planned growth experiment with TTF-TCNQ on the SGF/EURECA had been cancelled. The target of the SGF investigation is now more fundamental in nature. None of the crystals to be grown here are, like TTF-TCNQ, in particular demand by science or industry, and the crystals only serve the purpose of model crystals. The real purpose of the investigation is to study the growth behavior. One of the experiments, the Soret Coefficient Measurement experiment is not growing crystals at all, but has it as its sole purpose to obtain accurate information on thermal diffusion, a process of importance in crystal growth from solution.

Crystallization mechanisms of acicular crystals

NASA Astrophysics Data System (ADS)

Puel, François; Verdurand, Elodie; Taulelle, Pascal; Bebon, Christine; Colson, Didier; Klein, Jean-Paul; Veesler, Stéphane

2008-01-01

In this contribution, we present an experimental investigation of the growth of four different organic molecules produced at industrial scale with a view to understand the crystallization mechanism of acicular or needle-like crystals. For all organic crystals studied in this article, layer-by-layer growth of the lateral faces is very slow and clear, as soon as the supersaturation is high enough, there is competition between growth and surface-activated secondary nucleation. This gives rise to pseudo-twinned crystals composed of several needle individuals aligned along a crystallographic axis; this is explained by regular over- and inter-growths as in the case of twinning. And when supersaturation is even higher, nucleation is fast and random. In an industrial continuous crystallization, the rapid growth of needle-like crystals is to be avoided as it leads to fragile crystals or needles, which can be partly broken or totally detached from the parent crystals especially along structural anisotropic axis corresponding to weaker chemical bonds, thus leading to slower growing faces. When an activated mechanism is involved such as a secondary surface nucleation, it is no longer possible to obtain a steady state. Therefore, the crystal number, size and habit vary significantly with time, leading to troubles in the downstream processing operations and to modifications of the final solid-specific properties. These results provide valuable information on the unique crystallization mechanisms of acicular crystals, and show that it is important to know these threshold and critical values when running a crystallizer in order to obtain easy-to-handle crystals.

The Effect of Additives on the Early Stages of Growth of Calcite Single Crystals

PubMed Central

Freeman, Colin L.; Gong, Xiuqing; Levenstein, Mark A.; Wang, Yunwei; Kulak, Alexander; Anduix‐Canto, Clara; Lee, Phillip A.; Li, Shunbo; Chen, Li; Christenson, Hugo K.

2017-01-01

Abstract As crystallization processes are often rapid, it can be difficult to monitor their growth mechanisms. In this study, we made use of the fact that crystallization proceeds more slowly in small volumes than in bulk solution to investigate the effects of the soluble additives Mg2+ and poly(styrene sulfonate) (PSS) on the early stages of growth of calcite crystals. Using a “Crystal Hotel” microfluidic device to provide well‐defined, nanoliter volumes, we observed that calcite crystals form via an amorphous precursor phase. Surprisingly, the first calcite crystals formed are perfect rhombohedra, and the soluble additives have no influence on the morphology until the crystals reach sizes of 0.1–0.5 μm for Mg2+ and 1–2 μm for PSS. The crystals then continue to grow to develop morphologies characteristic of these additives. These results can be rationalized by considering additive binding to kink sites, which is consistent with crystal growth by a classical mechanism. PMID:28767197

Silicon carbide - Progress in crystal growth

NASA Technical Reports Server (NTRS)

Powell, J. Anthony

1987-01-01

Recent progress in the development of two processes for producing large-area high-quality single crystals of SiC is described: (1) a modified Lely process for the growth of the alpha polytypes (e.g., 6H SiC) initially developed by Tairov and Tsvetkov (1978, 1981) and Ziegler et al. (1983), and (2) a process for the epitaxial growth of the beta polytype on single-crystal silicon or other substrates. Growth of large-area cubic SiC on Si is described together with growth of defect-free beta-SiC films on alpha-6H SiC crystals and TiC lattice. Semiconducting qualities of silicon carbide crystals grown by various techniques are discussed.

Floating zone growth of α-Na 0.90MnO 2 single crystals

DOE PAGES

Dally, Rebecca; Clement, Raphaele J.; Chisnell, Robin; ...

2016-12-03

Here, single crystal growth of α-Na xMnO 2 (x=0.90) is reported via the floating zone technique. The conditions required for stable growth and intergrowth-free crystals are described along with the results of trials under alternate growth atmospheres. Chemical and structural characterizations of the resulting α-Na 0.90MnO 2 crystals are performed using ICP-AES NMR, XANES, XPS, and neutron diffraction measurements. As a layered transition metal oxide with large ionic mobility and strong correlation effects, α-Na xMnO 2 is of interest to many communities, and the implications of large volume, high purity, single crystal growth are discussed.

Analytics of crystal growth in space

NASA Technical Reports Server (NTRS)

Wilcox, W. R.; Chang, C. E.; Shlichta, P. J.; Chen, P. S.; Kim, C. K.

1974-01-01

Two crystal growth processes considered for spacelab experiments were studied to anticipate and understand phenomena not ordinarily encountered on earth. Computer calculations were performed on transport processes in floating zone melting and on growth of a crystal from solution in a spacecraft environment. Experiments intended to simulate solution growth at micro accelerations were performed.

Advanced crystal growth techniques for thallium bromide semiconductor radiation detectors

NASA Astrophysics Data System (ADS)

Datta, Amlan; Becla, Piotr; Guguschev, Christo; Motakef, Shariar

2018-02-01

Thallium Bromide (TlBr) is a promising room-temperature radiation detector candidate with excellent charge transport properties. Currently, Travelling Molten Zone (TMZ) technique is widely used for growth of semiconductor-grade TlBr crystals. However, there are several challenges associated with this type of crystal growth process including lower yield, high thermal stress, and low crystal uniformity. To overcome these shortcomings of the current technique, several different crystal growth techniques have been implemented in this study. These include: Vertical Bridgman (VB), Physical Vapor Transport (PVT), Edge-defined Film-fed Growth (EFG), and Czochralski Growth (Cz). Techniques based on melt pulling (EFG and Cz) were demonstrated for the first time for semiconductor grade TlBr material. The viability of each process along with the associated challenges for TlBr growth has been discussed. The purity of the TlBr crystals along with its crystalline and electronic properties were analyzed and correlated with the growth techniques. Uncorrected 662 keV energy resolutions around 2% were obtained from 5 mm x 5 mm x 10 mm TlBr devices with virtual Frisch-grid configuration.

Applications of the second virial coefficient: protein crystallization and solubility

PubMed Central

Wilson, William W.; DeLucas, Lawrence J.

2014-01-01

This article begins by highlighting some of the ground-based studies emanating from NASA’s Microgravity Protein Crystal Growth (PCG) program. This is followed by a more detailed discussion of the history of and the progress made in one of the NASA-funded PCG investigations involving the use of measured second virial coefficients (B values) as a diagnostic indicator of solution conditions conducive to protein crystallization. A second application of measured B values involves the determination of solution conditions that improve or maximize the solubility of aqueous and membrane proteins. These two important applications have led to several technological improvements that simplify the experimental expertise required, enable the measurement of membrane proteins and improve the diagnostic capability and measurement throughput. PMID:24817708

The effect of temperature and gas flow on the physical vapour growth of mm-scale rubrene crystals for organic FETs

NASA Astrophysics Data System (ADS)

Ullah, A. R.; Micolich, A. P.; Cochrane, J. W.; Hamilton, A. R.

2007-12-01

There has recently been significant interest in rubrene single-crystals grown using physical vapour transport techniques due to their application in high-mobility organic field-effect transistor (OFET) devices. Despite numerous studies of the electrical properties of such crystals, there has only been one study to date focussing on characterising and optimising the crystal growth as a function of the relevant growth parameters. Here we present a study of the dependence of the yield of useful crystals (defined as crystals with at least one dimension of order 1 mm) on the temperature and volume flow of carrier gas used in the physical vapour growth process.

Asymptotic Analysis of Melt Growth for Antimonide-Based Compound Semiconductor Crystals in Magnetic and Electric Fields

DTIC Science & Technology

2006-10-01

F. Bliss, Gerald W. Iseler and Piotr Becla, "Combining static and rotating magnetic fields during modified vertical Bridgman crystal growth ," AIAA...Wang and Nancy Ma, "Semiconductor crystal growth by the vertical Bridgman process with rotating magnetic fields," ASME Journal of Heat Transfer...2005. 15. Stephen J. LaPointe, Nancy Ma and Donald W. Mueller, Jr., " Growth of binary alloyed semiconductor crystals by the vertical Bridgman

Inhibition of ice crystal growth in ice cream mix by gelatin hydrolysate.

PubMed

Damodaran, Srinivasan

2007-12-26

The inhibition of ice crystal growth in ice cream mix by gelatin hydrolysate produced by papain action was studied. The ice crystal growth was monitored by thermal cycling between -14 and -12 degrees C at a rate of one cycle per 3 min. It is shown that the hydrolysate fraction containing peptides in the molecular weight range of about 2000-5000 Da exhibited the highest inhibitory activity on ice crystal growth in ice cream mix, whereas fractions containing peptides greater than 7000 Da did not inhibit ice crystal growth. The size distribution of gelatin peptides formed in the hydrolysate was influenced by the pH of hydrolysis. The optimum hydrolysis conditions for producing peptides with maximum ice crystal growth inhibitory activity was pH 7 at 37 degrees C for 10 min at a papain to gelatin ratio of 1:100. However, this may depend on the type and source of gelatin. The possible mechanism of ice crystal growth inhibition by peptides from gelatin is discussed. Molecular modeling of model gelatin peptides revealed that they form an oxygen triad plane at the C-terminus with oxygen-oxygen distances similar to those found in ice nuclei. Binding of this oxygen triad plane to the prism face of ice nuclei via hydrogen bonding appears to be the mechanism by which gelatin hydrolysate might be inhibiting ice crystal growth in ice cream mix.

International Conference on Crystal Growth (10th) (ICCG-10) Held in San Diego, California on August 16 - 21, 1992

DTIC Science & Technology

1992-08-21

Synthetic Crystals. China82 The Growth of LaMgA],,O,,:Nd Large Crystals with High Quality B16 G, Wu. X Ma.* J. Xu. X Zhang and Y. Shen Crystal Growth and...Stolchlometry Problems of ZnSe for High Power Laser Y. ShIralshl Optical Components Kimura Metamelt Project. Japan E~ Kjause.* A. Moseal and H. Harmnn...Maki- Shanghai Institute of Ceramics. China Yokohama City University. Japa 023 CS Growth of High -CluaI~ty TI:A1202 Crystals for Solid-State Lase In

The use of heterogeneous and epitaxial nucleants to promote the growth of protein crystals

NASA Technical Reports Server (NTRS)

Mcpherson, Alexander; Shlichta, P.

1988-01-01

Fifty different mineral samples were tested as potential heterogeneous or epitaxial nucleants for four commonly crystallized proteins. It was found, using conventional protein crystallization techniques, that for each protein there was a set of mineral substrates that promoted nucleation of crystals at lower critical levels of supersaturation than required for spontaneous growth. In at least one case, the growth of lysozyme on the mineral apophyllite, it was shown by lattice analysis and X-ray diffraction that the nucleation and growth of the protein crystal on the mineral was likely to be truly epitaxial.

Space manufacturing in an automated crystal growth facility

NASA Technical Reports Server (NTRS)

Quinn, Alberta W.; Herrmann, Melody C.; Nelson, Pamela J.

1989-01-01

An account is given of a Space Station Freedom-based robotic laboratory system for crystal growth experiments; the robot must interface with both the experimental apparatus and such human input as may be required for control and display. The goal of the system is the simultaneous growth of several hundred protein crystals in microgravity. The robot possesses six degrees-of-freedom, allowing it to efficiently manipulate the cultured crystals as well as their respective growth cells; the crystals produced are expected to be of sufficiently high quality for complete structural determination on the basis of XRD.

The Release of Trapped Gases from Amorphous Solid Water Films: I. “Top-Down” Crystallization-Induced Crack Propagation Probed using the Molecular Volcano

DOE Office of Scientific and Technical Information (OSTI.GOV)

May, Robert A.; Smith, R. Scott; Kay, Bruce D.

In this (Paper I) and the companion paper (Paper II) we investigate the mechanisms for the release of trapped gases from underneath of amorphous solid water (ASW) films. In prior work, we reported the episodic release of trapped gases in concert with the crystallization ASW, a phenomenon that we termed the "molecular volcano". The observed abrupt desorption is due to the formation of cracks that span the film to form a connected pathway for release. In this paper we utilize the "molecular volcano" desorption peak to characterize the formation of crystallization-induced cracks. We find that the crack length and distributionmore » are independent of the trapped gas (Ar, Kr, Xe, CH4, N2, O2 or CO). Selective placement of the inert gas layer is used to show that cracks form near the top of the film and propagate downward into the film. Isothermal experiments reveal that, after some induction time, cracks propagate linearly in time with an Arrhenius dependent velocity corresponding to an activation energy of 54 kJ/mol. This value is consistent with the crystallization growth rate reported by others and establishes a direct connection between crystallization growth rate and the crack propagation rate. A two-step model in which nucleation and crystallization occurs in an induction zone near the top of the film followed by the propagation of a crystallization/crack front into the film is in good agreement with the temperature programmed desorption results.« less

Kinetic Controls on Formation of Textures in Rapidly Cooled Rocks

NASA Technical Reports Server (NTRS)

Lofgren, Gary E.

2006-01-01

The crystallization of silicate melts is a complex process involving melts usually produced by partial melting and cooling environments that are rapid in volcanic lavas or so slow as to be auto-metamorphic in plutonic regimes. The volcanic lavas are amenable to laboratory study as are chondrules that comprise the bulk of chondritic meteorites. Dynamic crystallization studies of basalt and chondrule melts have shown that nucleation has a more profound effect on the final texture than the cooling or crystal growth rates. The sequence of crystal shapes grown at increasing degrees of supercooling (DELTA T) or cooling rate demonstrates the effect of increasing growth rate. Equant or euhedral crystals become skeletal, then dendritic and ultimately spherulitic indicating the nucleation temperature and the DELTA T when growth began. Because crystals cannot grow until they nucleate, cooling rate does not always correlate with crystal growth rate and thus crystal shape. Silicate melts cooled at the same rate can have drastically different textures depending on the temperature of nucleation. A dynamic crystallization study of basaltic rocks shows that basaltic lavas must erupt with sufficient crystals present in the melt to act as nuclei and foster growth. With nuclei present, growth will begin when the temperature drops below the liquidus temperature and typical basaltic textures such as intersertal, intergranular or subophitic will form. If nuclei are not present, crystallization will not begin immediately and the DELTA T will increase until embryos in the melts become nuclei. The DELTA T present when grow begins dictates the growth rate and the crystal shapes and thus the rock texture. If nucleation is delayed, growth will take place at high DELTA T and the crystals will favor skeletal or dendritic shapes. Chondrules are usually considered crystallized melt droplets and clearly some are, but most are not. Most chondrules have porphyritic textures that cannot develop from totally melted droplets because nucleation is delayed during cooling and growth occurs at high DELTA T and the resulting textures are dendritic or spherulitic. The porphyritic textures will develop only if the chondrule is partially molten and begins to crystallize immediately upon cooling. Chondrule compositions are close to komatiites and these studies bear on the origin of their textures as well.

The growth of zinc selenide single crystals by physical vapor transport in microgravity

NASA Technical Reports Server (NTRS)

Anderson, Elmer E.; Rosenberger, Franz E.; Cheng, Hai-Yuin

1990-01-01

Growth and characterization studies will be performed on zinc selenide single crystals. The high temperature outgassing behavior of the silica ampoule material will be studied in order to develop a cleaning and bake-out procedure that will minimize the amount of impurities introduced into the vapor from the ampoule materials and in particular during the seal-off procedure. The outgassing behavior of the ZnSe starting material will be studied during high vacuum refinement at elevated temperatures in order to develop a temperature pressure program that will optimize the removal of impurities while minimizing a shift in stoichiometry due to preferred evaporation of the higher fugacity component. The mass spectrometer system was completed, and after calibration, will be used to perform the above tasks. The system and its operation is described in detail.

Oscillating-Crucible Technique for Silicon Growth

NASA Technical Reports Server (NTRS)

Daud, T.; Dumas, K. A.; Kim, K. M.; Schwuttke, G. H.; Smetana, P.

1984-01-01

Technique yields better mixing of impurities and superior qualiity crystals. Accellerated motion stirs melt which reduces temperature gradients and decreases boundary layer for diffusion of impurities near growing surface. Results better mixing of impurities into melt, decrease in tendency for dendritic growth or cellular growth and crystals with low dislocation density. Applied with success to solution growth and Czochralski growth, resulting in large crystals of superior quality.

Calcite crystal growth rate inhibition by polycarboxylic acids

USGS Publications Warehouse

Reddy, M.M.; Hoch, A.R.

2001-01-01

Calcite crystal growth rates measured in the presence of several polycarboxyclic acids show that tetrahydrofurantetracarboxylic acid (THFTCA) and cyclopentanetetracarboxylic acid (CPTCA) are effective growth rate inhibitors at low solution concentrations (0.01 to 1 mg/L). In contrast, linear polycarbocylic acids (citric acid and tricarballylic acid) had no inhibiting effect on calcite growth rates at concentrations up to 10 mg/L. Calcite crystal growth rate inhibition by cyclic polycarboxyclic acids appears to involve blockage of crystal growth sites on the mineral surface by several carboxylate groups. Growth morphology varied for growth in the absence and in the presence of both THFTCA and CPTCA. More effective growth rate reduction by CPTCA relative to THFTCA suggests that inhibitor carboxylate stereochemical orientation controls calcite surface interaction with carboxylate inhibitors. ?? 20O1 Academic Press.

Protein crystal growth in low gravity

NASA Technical Reports Server (NTRS)

Feigelson, Robert S.

1991-01-01

The objective of this research is to study the effect of low gravity on the growth of protein crystals and those parameters which will affect growth and crystal quality. The application of graphoepitaxy (artificial epitaxy) to proteins is detailed. The development of a method for the control of nucleation is discussed. The factor affecting the morphology of isocitrate lyase crystals is presented.

Direct Observation Through In Situ Transmission Electron Microscope of Early States of Crystallization in Nanoscale Metallic Glasses

NASA Astrophysics Data System (ADS)

Xie, Y.; Sohn, S.; Schroers, J.; Cha, J. J.

2017-11-01

Crystallization is a complex process that involves multiscale physics such as diffusion of atomic species over multiple length scales, thermodynamic energy considerations, and multiple possible intermediate states. In situ crystallization experiments inside a transmission electron microscope (TEM) using nanostructured metallic glasses (MGs) provide a unique platform to study directly crystallization kinetics and pathways. Here, we study the embryonic state of eutectic growth using Pt-Ni-Cu-P MG nanorods under in situ TEM. We directly observe the nucleation and growth of a Ni-rich polymorphic phase, followed by the nucleation and slower growth of a Cu-rich phase. The suppressed growth kinetics of the Cu-rich phase is attributed to locally changing chemical compositions. In addition, we show that growth can be controlled by incorporation of an entire nucleus instead of individual atoms. Such a nucleus has to align with the crystallographic orientation of a larger grain before it can be incorporated into the crystal. By directly observing the crystallization processes, particularly the early stages of non-polymorphic growth, in situ TEM crystallization studies of MG nanostructures provide a wealth of information, some of which can be applied to typical bulk crystallization.

The inhibition of calcium carbonate crystal growth by the cysteine-rich Mdm2 peptide.

PubMed

Dalas, E; Chalias, A; Gatos, D; Barlos, K

2006-08-15

The crystal growth of calcite, the most stable calcium carbonate polymorph, in the presence of the cysteine-rich Mdm2 peptide (containing 48 amino acids in the ring finger configuration), has been investigated by the constant composition technique. Crystallization took place exclusively on well-characterized calcite crystals in solutions supersaturated only with respect to this calcium carbonate salt. The kinetic results indicated a surface diffusion spiral growth mechanism. The presence of the Mdm2 peptide inhibited the crystal growth of calcite by 22-58% in the concentration range tested, through adsorption onto the active growth sites of the calcite crystal surface. The kinetic results favored a Langmuir-type adsorption model, and the value of the calculated affinity constant was k(aff)=147x10(4) dm(3)mol(-1), a(ads)=0.29.

Theory of the intermediate stage of crystal growth with applications to insulin crystallization

NASA Astrophysics Data System (ADS)

Barlow, D. A.

2017-07-01

A theory for the intermediate stage of crystal growth, where two defining equations one for population continuity and another for mass-balance, is used to study the kinetics of the supersaturation decay, the homogeneous nucleation rate, the linear growth rate and the final distribution of crystal sizes for the crystallization of bovine and porcine insulin from solution. The cited experimental reports suggest that the crystal linear growth rate is directly proportional to the square of the insulin concentration in solution for bovine insulin and to the cube of concentration for porcine. In a previous work, it was shown that the above mentioned system could be solved for the case where the growth rate is directly proportional to the normalized supersaturation. Here a more general solution is presented valid for cases where the growth rate is directly proportional to the normalized supersaturation raised to the power of any positive integer. The resulting expressions for the time dependent normalized supersaturation and crystal size distribution are compared with experimental reports for insulin crystallization. An approximation for the maximum crystal size at the end of the intermediate stage is derived. The results suggest that the largest crystal size in the distribution at the end of the intermediate stage is maximized when nucleation is restricted to be only homogeneous. Further, the largest size in the final distribution depends only weakly upon the initial supersaturation.

Influence of Containment on the Growth of Germanium-Silicon in Microgravity

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.; Croll, A.; Sorgenfrei, T.

2017-01-01

This investigation involves the comparison of results achieved from three types of crystal growth of germanium and germanium-silicon alloys: Float zone growth, Bridgman growth, and Detached Bridgman growth. The fundamental goal of the proposed research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon (GeSi) crystals (silicon concentration in the solid up to 5%) for three different growth configurations in order to quantitatively assess the improvements of crystal quality possible by detached growth.

Bulk Crystal Growth of Nonlinear Optical Organic Materials Using Inverted Vertical Gradient Freeze Method

NASA Technical Reports Server (NTRS)

Choi, J.; Cruz, Magda; Metzl, R.; Wang, W. S.; Aggarwal, M. D.; Penn, Benjamin G.; Frazier, Donald O.

1998-01-01

A new process for producing large bulk single crystals of benzil (C6H5COCOC6H5) is reported in this paper. Good quality crystals have been successfully grown using this approach to crystal growth. This method seems to be very promising for other thermally stable NLO organic materials also. The entire contents vycor crucible 1.5 inch in diameter and 2 inch deep was converted to single crystal. Purity of the starting growth material is also an important factor in the final quality of the grown crystals. The entire crystal can be very easily taken out of the crucible by simple maneuvering. Initial characterization of the grown crystals indicated that the crystals are as good as other crystals grown by conventional Bridgman Stockbarger technique.

Manipulating crystallization with molecular additives.

PubMed

Shtukenberg, Alexander G; Lee, Stephanie S; Kahr, Bart; Ward, Michael D

2014-01-01

Given the importance of organic crystals in a wide range of industrial applications, the chemistry, biology, materials science, and chemical engineering communities have focused considerable attention on developing methods to control crystal structure, size, shape, and orientation. Tailored additives have been used to control crystallization to great effect, presumably by selectively binding to particular crystallographic surfaces and sites. However, substantial knowledge gaps still exist in the fundamental mechanisms that govern the formation and growth of organic crystals in both the absence and presence of additives. In this review, we highlight research discoveries that reveal the role of additives, either introduced by design or present adventitiously, on various stages of formation and growth of organic crystals, including nucleation, dislocation spiral growth mechanisms, growth inhibition, and nonclassical crystal morphologies. The insights from these investigations and others of their kind are likely to guide the development of innovative methods to manipulate crystallization for a wide range of materials and applications.

Dewetting During the Crystal Growth of (Cd,Zn)Te:In Under Microgravity

NASA Astrophysics Data System (ADS)

Sylla, Lamine; Fauler, Alex; Fiederle, Michael; Duffar, Thierry; Dieguez, Ernesto; Zanotti, Lucio; Zappettini, Andrea; Roosen, GÉrald

2009-08-01

The phenomenon of ldquodewettingrdquo associated with the Vertical Bridgman (VB) crystal growth technique leads to the growth of a crystal without contact with the crucible. One dramatic consequence of this modified VB process is the reduction of structural defects within the crystal. It has been observed in several microgravity experiments for different semiconductor crystals. This work is concentrated on the growth of high resistivity (Cd,Zn)Te:In (CZT) crystals by achieving the phenomenon of dewetting under microgravity condition and its application in the processing of CZT detectors. Two Cd0.9Zn0.1Te:In crystals were grown in space on the Russian FOTON satellite in the POLIZON-M facility in September 2007 (mission M3). At the end of the preliminary melting phase of one crystal, a Rotating Magnetic Field (RMF) was applied in order to reduce the typical tellurium clusters within the melt before the pulling. The other crystal was superheated with 20 K above the melting point before the pulling. A third reference crystal has been grown on the ground in similar thermal conditions. Profiles measurements of the space grown crystals surface gave the evidence of a successful dewetting during the crystal growth. Characterization methods such as IR microscopy and CoReMa have been performed on the three crystals. CZT detectors have been processed from the grown part of the different crystals. The influence of the dewetting on the material quality and the detector properties completes the study.

The Nucleation and Growth of Protein Crystals

NASA Technical Reports Server (NTRS)

Pusey, Marc

2004-01-01

Obtaining crystals of suitable size and high quality continues to be a major bottleneck in macromolecular crystallography. Currently, structural genomics efforts are achieving on average about a 10% success rate in going from purified protein to a deposited crystal structure. Growth of crystals in microgravity was proposed as a means of overcoming size and quality problems, which subsequently led to a major NASA effort in microgravity crystal growth, with the agency also funding research into understanding the process. Studies of the macromolecule crystal nucleation and growth process were carried out in a number of labs in an effort to understand what affected the resultant crystal quality on Earth, and how microgravity improved the process. Based upon experimental evidence, as well as simple starting assumptions, we have proposed that crystal nucleation occurs by a series of discrete self assembly steps, which 'set' the underlying crystal symmetry. This talk will review the model developed, and its origins, in our laboratory for how crystals nucleate and grow, and will then present, along with preliminary data, how we propose to use this model to improve the success rate for obtaining crystals from a given protein.

Effect of polyglycerol esters additive on palm oil crystallization using focused beam reflectance measurement and differential scanning calorimetry.

PubMed

Saw, M H; Hishamuddin, E; Chong, C L; Yeoh, C B; Lim, W H

2017-01-01

The effect of 0.1-0.7% (w/w) of polyglycerol esters (PGEmix-8) on palm oil crystallization was studied using focused beam reflectance measurement (FBRM) to analyze the in-line changes of crystal size distribution during the crystallization. FBRM results show that 0.1-0.5% (w/w) of PGEmix-8 did not significantly affect nucleation but slightly retarded crystal growth. The use of 0.7% (w/w) additive showed greater heterogeneous nucleation compared to those with lower dosages of additive. Crystal growth was also greatly reduced when using 0.7% (w/w) dosage. The morphological study indicated that the palm oil crystals were smaller and more even in size than when more additive was added. Isothermal crystallization studies using differential scanning calorimetry (DSC) showed increased inhibitory effects on palm oil crystal growth with increasing concentration of PGEmix-8. These results imply that PGEmix-8 is a nucleation enhancing and crystal growth retarding additive in palm oil crystallization at 0.7% (w/w) dosage. Copyright © 2016 The Author(s). Published by Elsevier Ltd.. All rights reserved.

Interface Shape and Growth Rate Analysis of Se/GaAs Bulk Crystals Grown in the NASA Crystal Growth Furnace (CGF)

NASA Technical Reports Server (NTRS)

Bly, J. M.; Kaforey, M. L.; Matthiesen, D. H.; Chait, A.

1997-01-01

Selenium-doped gallium arsenide, Se/GaAs, bulk crystals have been grown on earth using NASA's crystal growth furnace (CGF) in preparation for microgravity experimentation on the USML-2 spacelab mission. Peltier cooling pulses of 50 ms duration, 2040 A magnitude, and 0.0033 Hz frequency were used to successfully demark the melt-solid interface at known times during the crystal growth process. Post-growth characterization included interface shape measurement, growth rate calculation, and growth rate transient determinations. It was found that the interface shapes were always slightly concave into the solid. The curvature of the seeding interfaces was typically 1.5 mm for the 15 mm diameter samples. This was in agreement with the predicted interface shapes and positions relative to the furnace determined using a numerical model of the sample/ampoule/cartridge assembly (SACA).

Understanding the barriers to crystal growth: dynamical simulation of the dissolution and growth of urea from aqueous solution.

PubMed

Piana, Stefano; Gale, Julian D

2005-02-16

Both the dissolution and growth of a molecular crystalline material, urea, has been studied using dynamical atomistic simulation. The kinetic steps of dissolution and growth are clearly identified, and the activation energies for each possible step are calculated. Our molecular dynamics simulations indicate that crystal growth on the [001] face is characterized by a nucleation and growth mechanism. Nucleation on the [001] urea crystal face is predicted to occur at a very high rate, followed by rapid propagation of the steps. The rate-limiting step for crystallization is actually found to be the removal of surface defects, rather than the initial formation of the next surface layer. Through kinetic Monte Carlo modeling of the surface growth, it is found that this crystal face evolves via a rough surface topography, rather than a clean layer-by-layer mechanism.

A Low-Cost System Based on Image Analysis for Monitoring the Crystal Growth Process.

PubMed

Venâncio, Fabrício; Rosário, Francisca F do; Cajaiba, João

2017-05-31

Many techniques are used to monitor one or more of the phenomena involved in the crystallization process. One of the challenges in crystal growth monitoring is finding techniques that allow direct interpretation of the data. The present study used a low-cost system, composed of a commercial webcam and a simple white LED (Light Emitting Diode) illuminator, to follow the calcium carbonate crystal growth process. The experiments were followed with focused beam reflectance measurement (FBRM), a common technique for obtaining information about the formation and growth of crystals. The images obtained in real time were treated with the red, blue, and green (RGB) system. The results showed a qualitative response of the system to crystal formation and growth processes, as there was an observed decrease in the signal as the growth process occurred. Control of the crystal growth was managed by increasing the viscosity of the test solution with the addition of monoethylene glycol (MEG) at 30% and 70% in a mass to mass relationship, providing different profiles of the RGB average curves. The decrease in the average RGB value became slower as the concentration of MEG was increased; this reflected a lag in the growth process that was proven by the FBRM.

Characterization and In-Situ Monitoring of ZnSe Crystal Growth by Seeded PVT for Microgravity Applications

NASA Technical Reports Server (NTRS)

Feth, Shari T.

2001-01-01

Crystal growth from the vapor phase continues to play a significant role in the production of II-VI semiconductor compounds (ZnO, ZnTe, CdTe, etc.) and SiC. As compared to melt growth methods (where available) the advantages are: (1) lower growth temperature(s); (2) reduction in defect concentration; (3) additional purification; and (4) enhanced crystal perfection. A powerful tool in determining the mechanism of PVT is microgravity. Under normal gravity conditions the transport mechanism is a superposition of diffusive and convective fluxes. Microgravity offers the possibility of studying the transport properties without the influence of convective effects. Research on the crystal growth of ZnSe by PVT (P.I.: Su of NASA/MSFC) will help to clarify the effects of convection on crystal growth. A crystal growth furnace with in-situ and real time optical monitoring capabilities was constructed and used to monitor the vapor composition and growing crystal surface morphology during the PVT growth of ZnSe. Using photoluminescence and SIMS, ex-situ, the incorporation of point defects (Zn vacancy) and impurities was found to be correlated to the gravity vector due to the influence of the convective flow. A summary of the results to date will be presented.

Time-Lapse, in Situ Imaging of Ice Crystal Growth Using Confocal Microscopy

PubMed Central

2016-01-01

Ice crystals nucleate and grow when a water solution is cooled below its freezing point. The growth velocities and morphologies of the ice crystals depend on many parameters, such as the temperature of ice growth, the melting temperature, and the interactions of solutes with the growing crystals. Three types of morphologies may appear: dendritic, cellular (or fingerlike), or the faceted equilibrium form. Understanding and controlling which type of morphology is formed is essential in several domains, from biology to geophysics and materials science. Obtaining, in situ, three dimensional observations without introducing artifacts due to the experimental technique is nevertheless challenging. Here we show how we can use laser scanning confocal microscopy to follow in real-time the growth of smoothed and faceted ice crystals in zirconium acetate solutions. Both qualitative and quantitative observations can be made. In particular, we can precisely measure the lateral growth velocity of the crystals, a measure otherwise difficult to obtain. Such observations should help us understand the influence of the parameters that control the growth of ice crystals in various systems. PMID:27917410

Time-Lapse, in Situ Imaging of Ice Crystal Growth Using Confocal Microscopy.

PubMed

Marcellini, Moreno; Noirjean, Cecile; Dedovets, Dmytro; Maria, Juliette; Deville, Sylvain

2016-11-30

Ice crystals nucleate and grow when a water solution is cooled below its freezing point. The growth velocities and morphologies of the ice crystals depend on many parameters, such as the temperature of ice growth, the melting temperature, and the interactions of solutes with the growing crystals. Three types of morphologies may appear: dendritic, cellular (or fingerlike), or the faceted equilibrium form. Understanding and controlling which type of morphology is formed is essential in several domains, from biology to geophysics and materials science. Obtaining, in situ, three dimensional observations without introducing artifacts due to the experimental technique is nevertheless challenging. Here we show how we can use laser scanning confocal microscopy to follow in real-time the growth of smoothed and faceted ice crystals in zirconium acetate solutions. Both qualitative and quantitative observations can be made. In particular, we can precisely measure the lateral growth velocity of the crystals, a measure otherwise difficult to obtain. Such observations should help us understand the influence of the parameters that control the growth of ice crystals in various systems.

Synthesis and characterization of colloidal CdTe nanocrystals

NASA Astrophysics Data System (ADS)

Semendy, Fred; Jaganathan, Gomatam; Dhar, Nibir; Trivedi, Sudhir; Bhat, Ishwara; Chen, Yuanping

2008-08-01

We synthesized CdTe nano crystals (NCs) in uniform sizes and in good quality as characterized by photoluminescence (PL), AFM, and X-ray diffraction. In this growth procedure, CdTe nano-crystal band gap is strongly dependent on the growth time and not on the injection temperature or organic ligand concentration. This is very attractive because of nano-crystal size can be easily controlled by the growth time only and is very attractive for large scale synthesis. The color of the solution changes from greenish yellow to light orange then to deep orange and finally grayish black to black over a period of one hour. This is a clear indication of the gradual growth of different size (and different band gap) of CdTe nano-crystals as a function of the growth time. In other words, the size of the nano-crystal and its band gap can be controlled by adjusting the growth time after injection of the tellurium. The prepared CdTe NCs were characterized by absorption spectra, photoluminescence (PL), AFM and X-ray diffraction. Measured absorption maxima are at 521, 560, 600 and 603 nm corresponding to band gaps of 2.38, 2.21,2,07 and 2.04 eV respectively for growth times of 15, 30, 45 and 60 minutes. From the absorption data nano-crystal growth size saturates out after 45 minutes. AFM scanning of these materials indicate that the size of these particles is between 4 - 10 nm in diameter for growth time of 45 minutes. XD-ray diffraction indicates that these nano crystals are of cubic zinc blende phase. This paper will present growth and characterization data on CdTe nano crystals for various growth times.

Imaging System For Measuring Macromolecule Crystal Growth Rates in Microgravity

NASA Technical Reports Server (NTRS)

Corder, Eric L.; Briscoe, Jeri

2004-01-01

In order to determine how macromolecule crystal quality improvement in microgravity is related to crystal growth characteristics, a team of scientists and engineers at NASA's Marshal Space Flight Center (MSFC) developed flight hardware capable of measuring the crystal growth rates of a population of crystals growing under the same conditions. As crystal growth rate is defined as the change or delta in a defined dimension or length (L) of crystal over time, the hardware was named Delta-L. Delta-L consists of three sub assemblies: a fluid unit including a temperature-controlled growth cell, an imaging unit, and a control unit (consisting of a Data Acquisition and Control Unit (DACU), and a thermal control unit). Delta-L will be used in connection with the Glovebox Integrated Microgravity Isolation Technology (g-LIMIT) inside the Microgravity Science Glovebox (MSG), onboard the International Space Station. This paper will describe the Delta-L imaging system. The Delta-L imaging system was designed to locate, resolve, and capture images of up to 10 individual crystals ranging in size from 10 to 500 microns with a point-to-point accuracy of +/- 2.0 microns within a quartz growth cell observation area of 20 mm x 10 mm x 1 mm. The optical imaging system is comprised of a video microscope camera mounted on computer controlled translation stages. The 3-axis translation stages and control units provide crewmembers the ability to search throughout the growth cell observation area for crystals forming in size of approximately 10 microns. Once the crewmember has selected ten crystals of interest, the growth of these crystals is tracked until the size reaches approximately 500 microns. In order to resolve these crystals an optical system with a magnification of 10X was designed. A black and white NTSC camera was utilized with a 20X microscope objective and a 0.5X custom designed relay lens with an inline light to meet the magnification requirement. The design allows a 500 pm crystal to be viewed in the vertical dimension on a standard NTSC monitor (4:3 aspect ratio). Images of the 10 crystals are collected periodically and stored in sets by the DACU.

Crystal growth of artificial snow

NASA Technical Reports Server (NTRS)

Kimura, S.; Oka, A.; Taki, M.; Kuwano, R.; Ono, H.; Nagura, R.; Narimatsu, Y.; Tanii, J.; Kamimiytat, Y.

1984-01-01

Snow crystals were grown onboard the space shuttle during STS-7 and STS-8 to facilitate the investigation of crystal growth under conditions of weightlessness. The experimental design and hardware are described. Space-grown snow crystals were polyhedrons looking like spheres, which were unlike snow crystals produced in experiments on Earth.

Bulk crystal growth of Ga2O3

NASA Astrophysics Data System (ADS)

Kuramata, Akito; Koshi, Kimiyoshi; Watanabe, Shinya; Yamaoka, Yu; Masui, Takekazu; Yamakoshi, Shigenobu

2018-02-01

This paper describes the bulk crystal growth of β-Ga2O3 using edge-defined film-fed growth (EFG) process. We first describe the method of the crystal growth and show that large-size crystal with width of up to 6 inch can be grown. Then, we discuss the way to control electrical properties. In the discussion, we give some experimental results of residual impurity measurement, intentional doping using Si and Sn for n-type doping and Fe for insulating doping.

Mesoscopic homogenization of semi-insulating GaAs by two-step post growth annealing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hoffmann, B.; Jurisch, M.; Koehler, A.

1996-12-31

Mesoscopic homogenization of the electrical properties of s.i. LEC-GaAs is commonly realized by thermal treatment of the crystals including the steps of dissolution of arsenic precipitates, homogenization of excess As and re-precipitation by creating a controlled supersaturation. Caused by the inhomogeneous distribution of dislocations and the corresponding cellular structure along and across LEC-grown crystals a proper choice of the time-temperature program is necessary to minimize fluctuations of mesoscopic homogeneity. A modified two-step ingot annealing process is demonstrated to ensure the homogeneous distribution of mesoscopic homogeneity.

Using the Binary Phase-Field Crystal Model to Describe Non-Classical Nucleation Pathways in Gold Nanoparticles

NASA Astrophysics Data System (ADS)

Smith, Nathan; Provatas, Nikolas

Recent experimental work has shown that gold nanoparticles can precipitate from an aqueous solution through a non-classical, multi-step nucleation process. This multi-step process begins with spinodal decomposition into solute-rich and solute-poor liquid domains followed by nucleation from within the solute-rich domains. We present a binary phase-field crystal theory that shows the same phenomology and examine various cross-over regimes in the growth and coarsening of liquid and solid domains. We'd like to the thank Canada Research Chairs (CRC) program for funding this work.

Models of Mass Transport During Microgravity Crystal Growth of Alloyed Semiconductors in a Magnetic Field

NASA Technical Reports Server (NTRS)

Ma, Nancy

2003-01-01

Alloyed semiconductor crystals, such as germanium-silicon (GeSi) and various II-VI alloyed crystals, are extremely important for optoelectronic devices. Currently, high-quality crystals of GeSi and of II-VI alloys can be grown by epitaxial processes, but the time required to grow a certain amount of single crystal is roughly 1,000 times longer than the time required for Bridgman growth from a melt. Recent rapid advances in optoelectronics have led to a great demand for more and larger crystals with fewer dislocations and other microdefects and with more uniform and controllable compositions. Currently, alloyed crystals grown by bulk methods have unacceptable levels of segregation in the composition of the crystal. Alloyed crystals are being grown by the Bridgman process in space in order to develop successful bulk-growth methods, with the hope that the technology will be equally successful on earth. Unfortunately some crystals grown in space still have unacceptable segregation, for example, due to residual accelerations. The application of a weak magnetic field during crystal growth in space may eliminate the undesirable segregation. Understanding and improving the bulk growth of alloyed semiconductors in microgravity is critically important. The purpose of this grant to to develop models of the unsteady species transport during the bulk growth of alloyed semiconductor crystals in the presence of a magnetic field in microgravity. The research supports experiments being conducted in the High Magnetic Field Solidification Facility at Marshall Space Flight Center (MSFC) and future experiments on the International Space Station.

Compositional segregation and electrical properties characterization of [001]- and [011]-oriented co-growth Pb(In1/2Nb1/2)O3-Pb(Mg1/3Nb2/3)O3-PbTiO3 single crystal

NASA Astrophysics Data System (ADS)

Song, Kexin; Li, Zhenrong; Guo, Haisheng; Xu, Zhuo; Fan, Shiji

2018-04-01

A Pb(In1/2Nb1/2)O3-Pb(Mg1/3Nb2/3)O3-PbTiO3 relaxor ferroelectric single crystal boule of 3 in. diameter was grown using [001]- and [011]-oriented co-growth crystals as seeds by the modified Bridgman method. The as-grown crystal boule was divided into two growth regions [001] and [011]. The composition and the electrical properties of samples of the two regions were characterized in detail along the growth direction in the whole crystal boule. The PT content of [001]-grown samples increased from 27.7 to 36.8 mol. % along the growth direction, especially they are averagely higher about 0.7 mol. % than those of [011]-grown samples at the same growth position. The PMN content of [001]-grown samples decreased from 43.0 to 34.8 mol. %, which is lower than that of the corresponding [011]-grown samples. The compositional segregation behavior along [001] and [011] growth directions was discussed based on the crystal growth theories. Variations in the rhombohedral to tetragonal phase transition temperature (TRT), the piezoelectric properties, the coercive electric field and the remnant polarization of [001] samples were discussed according to changes in compositional segregation and crystal anisotropy. Under the exact same growth conditions, the [011]-grown crystal has a larger composition segregation effect than that of the [001]-grown crystal. This result provides a positive effect on analysing the nature and reducing the effect of compositional segregation.

Temperature cycling vapor deposition HgI.sub.2 crystal growth

DOEpatents

Schieber, Michael M.; Beinglass, Israel; Dishon, Giora

1977-01-01

A method and horizontal furnace for vapor phase growth of HgI.sub.2 crystals which utilizes controlled axial and radial airflow to maintain the desired temperature gradients. The ampoule containing the source material is rotated while axial and radial air tubes are moved in opposite directions during crystal growth to maintain a desired distance and associated temperature gradient with respect to the growing crystal, whereby the crystal interface can advance in all directions, i.e., radial and axial according to the crystallographic structure of the crystal. Crystals grown by this method are particularly applicable for use as room-temperature nuclear radiation detectors.

Frazil-ice growth rate and dynamics in mixed layers and sub-ice-shelf plumes

NASA Astrophysics Data System (ADS)

Rees Jones, David W.; Wells, Andrew J.

2018-01-01

The growth of frazil or granular ice is an important mode of ice formation in the cryosphere. Recent advances have improved our understanding of the microphysical processes that control the rate of ice-crystal growth when water is cooled beneath its freezing temperature. These advances suggest that crystals grow much faster than previously thought. In this paper, we consider models of a population of ice crystals with different sizes to provide insight into the treatment of frazil ice in large-scale models. We consider the role of crystal growth alongside the other physical processes that determine the dynamics of frazil ice. We apply our model to a simple mixed layer (such as at the surface of the ocean) and to a buoyant plume under a floating ice shelf. We provide numerical calculations and scaling arguments to predict the occurrence of frazil-ice explosions, which we show are controlled by crystal growth, nucleation, and gravitational removal. Faster crystal growth, higher secondary nucleation, and slower gravitational removal make frazil-ice explosions more likely. We identify steady-state crystal size distributions, which are largely insensitive to crystal growth rate but are affected by the relative importance of secondary nucleation to gravitational removal. Finally, we show that the fate of plumes underneath ice shelves is dramatically affected by frazil-ice dynamics. Differences in the parameterization of crystal growth and nucleation give rise to radically different predictions of basal accretion and plume dynamics, and can even impact whether a plume reaches the end of the ice shelf or intrudes at depth.

Single crystals of metal solid solutions: A study

NASA Technical Reports Server (NTRS)

Miller, J. F.; Gelles, S. H.

1975-01-01

Report describes growth of silver-alloy crystals under widely varying conditions of growth rate, temperature gradient, and magnetic field. Role of gravitation and convection on crystal substructure is analyzed, as well as influence of magnetic fields applied during crystallization.

Progress in the Growth of Yb:S-FAP Laser Crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schaffers, K I; Tassano, J B; Waide, P A

The crystal growth of Yb:S-FAP [Yb{sup 3+}:Sr{sub 5}(PO{sub 4}){sub 3}F] is being studied for 1.047-{micro}m laser operation. These crystals are not yet routinely available and the growth of high optical quality, low loss crystals poses a challenge due to a number of crystal growth issues, including, cloudiness, bubble core defects, anomalous absorption, low-angle grain boundaries, and cracking. At this time, a growth process has been formulated to simultaneously eliminate or greatly diminish each of the defects yielding high quality material. Laser slabs of dimension 4.0 x 6.0 x 0.75 cm are being fabricated from sub-scale pieces using the diffusion bondingmore » technique.« less

High-pressure floating-zone growth of perovskite nickelate LaNiO 3 single crystals

DOE PAGES

Zhang, Junjie; Zheng, Hong; Ren, Yang; ...

2017-04-07

We report the first single crystal growth of the correlated metal LaNiO 3 using a high-pressure optical-image floating zone furnace. The crystals were studied using single crystal/powder X-ray diffraction, resistivity, specific heat, and magnetic susceptibility. The availability of bulk LaNiO 3 crystals will (i) promote deep understanding in this correlated material, including the mechanism of enhanced paramagnetic susceptibility, and (ii) provide rich opportunities as a substrate for thin film growth such as important ferroelectric and/or multiferroic materials. As a result, this study demonstrates the power of high pO 2 single crystal growth of nickelate perovskites and correlated electron oxides moremore » generally.« less

Experiment 3: Zeolite Crystal Growth in Microgravity- The USML-2 Mission

NASA Technical Reports Server (NTRS)

Bac, Nurcan; Warzywoda, Juliusz; Sacco, Albert, Jr.

1998-01-01

The extensive use of zeolites and their impact on the world's economy leads to many efforts to characterize their structure, and to improve the knowledge base for nucleation and growth of these crystals. The Zeolite Crystal Growth (ZCG) experiment on USML-2 aims to enhance the understanding of nucleation and growth of zeolite crystals while attempting to provide a means of controlling the defect concentration in microgravity. Zeolites A, X, Beta, and Silicalite were grown during the 16-day USML-2 mission. The solutions where the nucleation event was controlled yielded larger and more uniform crystals of better morphology and purity than their terrestrial/control counterparts. Space-grown Beta crystals were free of line defects while terrestrial/controls had substantial defects.

Modified floating-zone growth of organic single crystals

NASA Astrophysics Data System (ADS)

Kou, S.; Chen, C. P.

1994-04-01

For organic materials floating-zone crystal growth is superior to other melt growth processes in two significant respects: (1) the absence of crucible-induced mechanical damage and (2) minimum heating-induced chemical degradation. Due to the rather low surface tension of organic melts, however, floating-zone crystal growth under normal gravity has not been possible so far but microgravity is ideal for such a purpose. With the help of a modified floating-zone technique, organic single crystals of small cross-sections were test grown first under normal gravity. These small crystals were round and rectangular single crystals of benzil and salol, up to about 7 cm long and 6 mm in diameter or 9 mm × 3 mm in cross-section.

Melt growth of organic 4-(2-Phenylisopropyl) phenol single crystal and its structural, thermal, dielectric permittivity and optical properties

NASA Astrophysics Data System (ADS)

Sadhasivam, S.; Rajesh, N. P.

2017-12-01

A nonlinear optical (NLO) organic crystal 4-(2-Phenylisopropyl) phenol has been grown by a top seeded melt growth technique. The melt growth kinetics of solid-liquid (molten) interface and facets formation in melt growth were studied. The melt grown crystal has the (001), (00 1 bar),(110)(1 bar 1 bar 0) ,(1 bar 20),(1 2 bar 0),(2 bar 10) and(2 1 bar 0) different morphological face. The morphological characteristics of melt grown crystal helps to better infer the kinetic influence of melt and hone growth of organic material. The rhombohedral lattice cell parameters were measured by single crystal X-ray diffraction. 4-(2-Phenylisopropyl) phenol crystallizes in space group of R 3 bar . Thermal study shows that solid to liquid transition occurring at 350 K and decomposes at 597 K. The grown crystal was optically transparent in the wavelength range of 300-1100 nm. The low dielectric constant (9-11) was measured in the [001] of 4-(2-Phenylisopropyl) phenol crystal.

A simple 2D composite image analysis technique for the crystal growth study of L-ascorbic acid.

PubMed

Kumar, Krishan; Kumar, Virender; Lal, Jatin; Kaur, Harmeet; Singh, Jasbir

2017-06-01

This work was destined for 2D crystal growth studies of L-ascorbic acid using the composite image analysis technique. Growth experiments on the L-ascorbic acid crystals were carried out by standard (optical) microscopy, laser diffraction analysis, and composite image analysis. For image analysis, the growth of L-ascorbic acid crystals was captured as digital 2D RGB images, which were then processed to composite images. After processing, the crystal boundaries emerged as white lines against the black (cancelled) background. The crystal boundaries were well differentiated by peaks in the intensity graphs generated for the composite images. The lengths of crystal boundaries measured from the intensity graphs of composite images were in good agreement (correlation coefficient "r" = 0.99) with the lengths measured by standard microscopy. On the contrary, the lengths measured by laser diffraction were poorly correlated with both techniques. Therefore, the composite image analysis can replace the standard microscopy technique for the crystal growth studies of L-ascorbic acid. © 2017 Wiley Periodicals, Inc.

Protein crystal growth in low gravity

NASA Technical Reports Server (NTRS)

Feigelson, Robert S.

1993-01-01

This Final Technical Report for NASA Grant NAG8-774 covers the period from April 27, 1989 through December 31, 1992. It covers five main topics: fluid flow studies, the influence of growth conditions on the morphology of isocitrate lyase crystals, control of nucleation, the growth of lysozyme by the temperature gradient method and graphoepitaxy of protein crystals. The section on fluid flow discusses the limits of detectability in the Schlieren imaging of fluid flows around protein crystals. The isocitrate lyase study compares crystals grown terrestrially under a variety of conditions with those grown in space. The controlling factor governing the morphology of the crystals is the supersaturation. The lack of flow in the interface between the drop and the atmosphere in microgravity causes protein precipitation in the boundary layer and a lowering of the supersaturation in the drop. This lowered supersaturation leads to improved crystal morphology. Preliminary experiments with lysozyme indicated that localized temperature gradients could be used to nucleate crystals in a controlled manner. An apparatus (thermonucleator) was designed to study the controlled nucleation of protein crystals. This apparatus has been used to nucleate crystals of materials with both normal (ice-water, Rochelle salt and lysozyme) and retrograde (horse serum albumin and alpha chymotrypsinogen A) solubility. These studies have lead to the design of an new apparatus that small and more compatible with use in microgravity. Lysozyme crystals were grown by transporting nutrient from a source (lysozyme powder) to the crystal in a temperature gradient. The influence of path length and cross section on the growth rate was demonstrated. This technique can be combined with the thermonucleator to control both nucleation and growth. Graphoepitaxy utilizes a patterned substrate to orient growing crystals. In this study, silicon substrates with 10 micron grooves were used to grow crystals of catalase, lysozyme and canavalin. In all cases, the crystals grew oriented to the substrate. The supersaturation needed for nucleation and growth was lower on the patterned substrates. In some cases, isolated, large crystals were grown.

Observations on the crystallization of spodumene from aqueous solutions in a hydrothermal diamond-anvil cell

USGS Publications Warehouse

Li, Jianking; Chou, I-Ming; Yuan, Shunda; Burruss, Robert A.

2013-01-01

Crystallization experiments were conducted in a new type of hydrothermal diamond-anvil cell (HDAC; type V) using LiAlSi2O6 (S) gel and H2O (W) as starting materials. A total of 21 experiments were performed at temperatures up to 950°C and pressures up to 788 MPa. In the samples with relatively low W/S ratios, many small crystals formed in the melt phase during cooling. In those with high W/S ratios, only a few crystals with smooth surfaces crystallized from the aqueous fluid in the presence of melt droplets, which were gradually consumed during crystal growth, indicating rapid transfer of material from the melt to the crystals through the aqueous fluid. The nucleation of crystals started at 710 (±70)°C and 520 (±80) MPa, and crystal growth ended at 570 (±40)°C and 320 (±90) MPa, with the cooling P-T path within the stability field of spodumene + quartz in the S-W system. The observed linear crystal growth rates in the aqueous phase, calculated by dividing the maximum length of a single crystal by the duration of the entire growth step, were 4.7 × 10−6 and 5.7 × 10−6 cm s−1 for the cooling rates of 0.5 and 1°C min−1, respectively. However, a rapid crystal growth rate of 3.6 × 10−5 cm s−1 in the aqueous fluid was observed when the components were supplied by nearby melt droplets. Our results show that when crystals nucleate in the aqueous fluid instead of the melt phase, there are fewer nuclei formed, and they grow much faster due to the low viscosity of the aqueous fluid, which accelerates diffusion of components for the growth of crystals. Therefore, the large crystals in granitic pegmatite can crystallize directly from aqueous fluids rather than hydrosilicate melt.

Single crystal growth of submillimeter diameter sapphire tube by the micro-pulling down method

NASA Astrophysics Data System (ADS)

Kamada, Kei; Murakami, Rikito; Kochurikhin, Vladimir V.; Luidmila, Gushchina; Jin Kim, Kyoung; Shoji, Yasuhiro; Yamaji, Akihiro; Kurosawa, Shunsuke; Ohashi, Yuji; Yokota, Yuui; Yoshikawa, Akira

2018-06-01

This paper addresses several aspects of the μ-PD growth technology as applied to submillimeter diameter sapphire tubes for UFD application. The μ-PD method has been successfully adapted for single crystal sapphire tube growth. A compound crucible made possible the growth of single crystal sapphire tube as small as around 0.70-0.72 mm in outer diameter and 0.28-0.29 in inner diameter over 160 mm in length at growth rate of 2-4 mm/min along 〈0 0 1〉 direction. An Ir crucible with a die composed of an equivalent hole and Ir wire was heated by RF coil in N2 atmosphere. The μ-PD method has been successfully adapted for single crystal sapphire tube growth. Grown crystal tube showed good XRC value of 30.2 arcsec.

Astronauts Lodewijk van den Berg observes growth of crystals in VCGS

NASA Image and Video Library

1985-04-30

51B-06-010 (29 April-6 May 1985) --- Lodewijk van den Berg, 51-B payload specialist, observes the growth of mercuric iodide crystal in the vapor crystal growth system (VCGS) on the Spacelab 3 science module aboard the Space Shuttle Challenger.

Astronauts Don Lind observes growth of crystals in VCGS aboard orbiter

NASA Image and Video Library

1985-04-30

51B-01-007 (30 April 1985) --- Astronaut Don L. Lind, 51-B Spacelab 3 mission specialist, observes the growth of mercuric iodide crystal in the vapor crystal growth system (VCGS) on the Spacelab 3 science module aboard the orbiter Challenger.

Study of Fluid Flow Control In Protein Crystallization Using Strong Magnetic Fields

NASA Technical Reports Server (NTRS)

Ramachandran, N.; Leslie, F.; Ciszak, E.; Curreri, Peter A. (Technical Monitor)

2002-01-01

An important component in biotechnology, particularly in the area of protein engineering and rational drug design is the knowledge of the precise three-dimensional molecular structure of proteins. The quality of structural information obtained from X-ray diffraction methods is directly dependent on the degree of perfection of the protein crystals. As a consequence, the growth of high quality macromolecular crystals for diffraction analyses has been the central focus for biochemists, biologists, and bioengineers. Macromolecular crystals are obtained from solutions that contain the crystallizing species in equilibrium with higher aggregates, ions, precipitants, other possible phases of the protein, foreign particles, the walls of the container, and a likely host of other impurities. By changing transport modes in general, i.e., reduction of convection and sedimentation, as is achieved in 'microgravity', researchers have been able to dramatically affect the movement and distribution of macromolecules in the fluid, and thus their transport, formation of crystal nuclei, and adsorption to the crystal surface. While a limited number of high quality crystals from space flights have been obtained, as the recent National Research Council (NRC) review of the NASA microgravity crystallization program pointed out, the scientific approach and research in crystallization of proteins has been mainly empirical yielding inconclusive results. We postulate that we can reduce convection in ground-based experiments and we can understand the different aspects of convection control through the use of strong magnetic fields and field gradients. Whether this limited convection in a magnetic field will provide the environment for the growth of high quality crystals is still a matter of conjecture that our research will address. The approach exploits the variation of fluid magnetic susceptibility with concentration for this purpose and the convective damping is realized by appropriately positioning the crystal growth cell so that the magnetic susceptibility force counteracts terrestrial gravity. The general objective is to test the hypothesis of convective control using a strong magnetic field and magnetic field gradient and to understand the nature of the various forces that come into play. Specifically we aim to delineate causative factors and to quantify them through experiments, analysis and numerical modeling. Once the basic understanding is obtained, the study will focus on testing the hypothesis on proteins of pyruvate dehydrogenase complex (PDC), proteins E1 and E3. Obtaining high crystal quality of these proteins is of great importance to structural biologists since their structures need to be determined.

New developments on size-dependent growth applied to the crystallization of sucrose

NASA Astrophysics Data System (ADS)

Martins, P. M.; Rocha, F.

2007-12-01

The effect of crystal size on the growth rate of sucrose (C 12H 22O 11) at 40 °C is investigated from a theoretical and an experimental point of view. Based on new perspectives resulting from the recently introduced spiral nucleation model [P.M. Martins, F. Rocha, Surf. Sci. 601 (2007) 3400], crystal growth rates are expressed in terms of mass deposition per time and crystal volume units. This alternative definition is demonstrated to be size-independent over the considered supersaturation range. The conventional overall growth rate expressed per surface area units is found to be linearly dependent on crystal size. The advantages of the "volumetric" growth rate concept are discussed. Sucrose dissolution rates were measured under reciprocal conditions of the growth experiments in order to investigate the two-way effect of crystal size on mass transfer rates and on the integration kinetics. Both effects are adequately described by combining a well-established diffusion-integration model and the spiral nucleation mechanism.

Influence of Polymers on the Crystal Growth Rate of Felodipine: Correlating Adsorbed Polymer Surface Coverage to Solution Crystal Growth Inhibition.

PubMed

Schram, Caitlin J; Taylor, Lynne S; Beaudoin, Stephen P

2015-10-20

The bioavailability of orally administered drugs that exhibit poor aqueous solubility can be enhanced with the use of supersaturating dosage forms. Stabilization of these forms by preventing or inhibiting crystallization in solution is an important area of study. Polymers can be used to stabilize supersaturated systems; however, the properties that impact their effectiveness as crystal growth rate inhibitors are not yet fully understood. In this study, the impact of various polymers on the crystal growth rate of felodipine and the conformation of these polymers adsorbed to crystalline felodipine was investigated in order to gain a mechanistic understanding of crystal growth inhibition. It was determined that polymer hydrophobicity impacted polymer adsorption as well as adsorbed polymer conformation. Polymer conformation impacts its surface coverage, which was shown to directly correlate to the polymer's effectiveness as a growth rate inhibitor. By modeling this correlation, it is possible to predict polymer effectiveness given the surface coverage of the polymer.

Growth of micro-crystals in solution by in-situ heating via continuous wave infrared laser light and an absorber

NASA Astrophysics Data System (ADS)

Pathak, Shashank; Dharmadhikari, Jayashree A.; Thamizhavel, A.; Mathur, Deepak; Dharmadhikari, Aditya K.

2016-01-01

We report on growth of micro-crystals such as sodium chloride (NaCl), copper sulphate (CuSO4), potassium di-hydrogen phosphate (KDP) and glycine (NH2CH2COOH) in solution by in-situ heating using continuous wave Nd:YVO4 laser light. Crystals are grown by adding single walled carbon nanotubes (SWNT). The SWNTs absorb 1064 nm light and act as an in-situ heat source that vaporizes the solvent producing microcrystals. The temporal dynamics of micro-crystal growth is investigated by varying experimental parameters such as SWNT bundle size and incident laser power. We also report crystal growth without SWNT in an absorbing medium: copper sulphate in water. Even though the growth dynamics with SWNT and copper sulphate are significantly different, our results indicate that bubble formation is necessary for nucleation. Our simple method may open up new vistas for rapid growth of seed crystals especially for examining the crystallizability of inorganic and organic materials.

Vapor crystal growth technology development: Application to cadmium telluride

NASA Technical Reports Server (NTRS)

Rosenberger, Franz; Banish, Michael; Duval, Walter M. B.

1991-01-01

Growth of bulk crystals by physical vapor transport was developed and applied to cadmium telluride. The technology makes use of effusive ampoules, in which part of the vapor contents escapes to a vacuum shroud through defined leaks during the growth process. This approach has the advantage over traditional sealed ampoule techniques that impurity vapors and excess vapor constituents are continuously removed from the vicinity of the growing crystal. Thus, growth rates are obtained routinely at magnitudes that are rather difficult to achieve in closed ampoules. Other advantages of this effusive ampoule physical vapor transport (EAPVT) technique include the predetermination of transport rates based on simple fluid dynamics and engineering considerations, and the growth of the crystal from close to congruent vapors, which largely alleviates the compositional nonuniformities resulting from buoyancy driven convective transport. After concisely reviewing earlier work on improving transport rates, nucleation control, and minimization of crystal wall interactions in vapor crystal growth, a detail account is given of the largely computer controlled EAPVT experimentation.

Shallow melt apparatus for semicontinuous czochralski crystal growth

DOEpatents

Wang, Tihu; Ciszek, Theodore F.

2006-01-10

In a single crystal pulling apparatus for providing a Czochralski crystal growth process, the improvement of a shallow melt In a single crystal pulling apparatus for providing a Czochralski crystal growth process, the improvement of a shallow melt crucible (20) to eliminate the necessity supplying a large quantity of feed stock materials that had to be preloaded in a deep crucible to grow a large ingot, comprising a gas tight container a crucible with a deepened periphery (25) to prevent snapping of a shallow melt and reduce turbulent melt convection; source supply means for adding source material to the semiconductor melt; a double barrier (23) to minimize heat transfer between the deepened periphery (25) and the shallow melt in the growth compartment; offset holes (24) in the double barrier (23) to increase melt travel length between the deepened periphery (25) and the shallow growth compartment; and the interface heater/heat sink (22) to control the interface shape and crystal growth rate.

Crystallization of DNA-coated colloids

PubMed Central

Wang, Yu; Wang, Yufeng; Zheng, Xiaolong; Ducrot, Étienne; Yodh, Jeremy S.; Weck, Marcus; Pine, David J.

2015-01-01

DNA-coated colloids hold great promise for self-assembly of programmed heterogeneous microstructures, provided they not only bind when cooled below their melting temperature, but also rearrange so that aggregated particles can anneal into the structure that minimizes the free energy. Unfortunately, DNA-coated colloids generally collide and stick forming kinetically arrested random aggregates when the thickness of the DNA coating is much smaller than the particles. Here we report DNA-coated colloids that can rearrange and anneal, thus enabling the growth of large colloidal crystals from a wide range of micrometre-sized DNA-coated colloids for the first time. The kinetics of aggregation, crystallization and defect formation are followed in real time. The crystallization rate exhibits the familiar maximum for intermediate temperature quenches observed in metallic alloys, but over a temperature range smaller by two orders of magnitude, owing to the highly temperature-sensitive diffusion between aggregated DNA-coated colloids. PMID:26078020

In-Situ Crystallization of a Lithium Disilicate Glass--Effect of Pressure on Crystal Growth Rate

NASA Technical Reports Server (NTRS)

Fuss, T.; Ray, C. S.; Lesher, C. E.; Day, D. E.

2006-01-01

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.

Effects of impurities on crystal growth in fructose crystallization

NASA Astrophysics Data System (ADS)

Chu, Y. D.; Shiau, L. D.; Berglund, K. A.

1989-10-01

The influence of impurities on the crystallization of anhydrous fructose from aqueous solution was studied. The growth kinetics of fructose crystals in the fructose-water-glucose and fructose-water-difructose dianhydrides systems were investigated using photomicroscopic contact nucleation techniques. Glucose is the major impurity likely to be present in fructose syrup formed during corn wet milling, while several difructose dianhydrides are formed in situ under crystallization conditions and have been proposed as a cause in the decrease of overall yields. Both sets of impurities were found to cause inhibition of crystal growth, but the mechanisms responsible in each case are different. It was found that the presence of glucose increases the solubility of fructose in water and thus lowers the supersaturation of the solution. This is probably the main effect responsible for the decrease of crystal growth. Since the molecular structures of difructose dianhydrides are similar to that of fructose, they are probably "tailor-made" impurities. The decrease of crystal growth is probably caused by the incorporation of these impurities into or adsorption to the crystal surface which would accept fructose molecules in the orientation that existed in the difructose dianhydride.

Low temperature growth of Ga 1- xIn xP bulk crystals from InSb-rich melt

NASA Astrophysics Data System (ADS)

Gennett, A.; Lewis, D.; Dutta, P. S.

2010-04-01

Bulk growth of phosphorus and arsenic based ternary III-V semiconductor crystals using pseudo-binary melts such as GaP-InP, GaP-GaAs, AlAs-GaAs, etc. is significantly challenging due to the high vapor pressures of group V species in conjunction with slow growth rates and the need for melt replenishment and mixing during growth. Lowering the growth temperature is desirable such that the vapor pressures of P and As can be easily handled. Low growth temperatures could be achieved by using Ga or In rich solutions. However, this approach is less attractive for growing bulk crystals due to several experimental difficulties including sticking of the growth solution to the crucible wall and to the grown crystal, making it challenging for crystal extraction. Growth of ternary crystals from low temperature quaternary melts has been found to be attractive. In this paper, we will present a new method for the growth of Ga 1- xIn xP from InSb rich Ga 1- xIn xP ySb 1- y melts at low growth temperatures in the range of 800-1050 °C. Thermodynamic phase diagrams calculated at various temperatures using a Gibbs free energy minimization software and materials databases commercially available from Thermo-Calc software will be presented along with experimental validation for Ga 1- xIn xP crystals grown at 1000 °C.

Influence of Containment on the Growth of Silicon-Germanium (ICESAGE): A Materials Science Investigation

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.; Croll, A.

2014-01-01

A series of Ge Si crystal growth experiments are planned to be conducted in the Low 1-x x Gradient Furnace (LGF) onboard the International Space Station. The primary objective of the research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and "detached" Bridgman methods and the ground-based float zone technique. Crystals grown without being in contact with a container have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in crystals. "Detached" or "dewetted" Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. Long duration reduced gravity is essential to test the proposed theory of detached growth. Detached growth requires the establishment of a meniscus between the crystal and the ampoule wall. The existence of this meniscus depends on the ratio of the strength of gravity to capillary forces. On Earth, this ratio is large and stable detached growth can only be obtained over limited conditions. Crystals grown detached on the ground exhibited superior structural quality as evidenced by measurements of etch pit density, synchrotron white beam X-ray topography and double axis X-ray diffraction.

Thermal Modeling of Bridgman Crystal Growth

NASA Technical Reports Server (NTRS)

Cothran, E.

1983-01-01

Heat Flow modeled for moving or stationary rod shaped sample inside directional-solidification furnace. Program effectively models one-dimensional heat flow in translating or motionless rod-shaped sample inside of directionalsolidification furnace in which adiabatic zone separates hot zone and cold zone. Applicable to systems for which Biot numbers in hot and cold zones are less than unity.

Method of Promoting Single Crystal Growth During Melt Growth of Semiconductors

NASA Technical Reports Server (NTRS)

Su, Ching-Hua (Inventor)

2013-01-01

The method of the invention promotes single crystal growth during fabrication of melt growth semiconductors. A growth ampoule and its tip have a semiconductor source material placed therein. The growth ampoule is placed in a first thermal environment that raises the temperature of the semiconductor source material to its liquidus temperature. The growth ampoule is then transitioned to a second thermal environment that causes the semiconductor source material in the growth ampoule's tip to attain a temperature that is below the semiconductor source material's solidus temperature. The growth ampoule so-transitioned is then mechanically perturbed to induce single crystal growth at the growth ampoule's tip.

Cirrus properties deduced from CO2 lidar observations of zenith-enhanced backscatter from oriented crystals

NASA Technical Reports Server (NTRS)

Eberhard, Wynn L.

1993-01-01

Many lidar researchers have occasionally observed zenith-enhanced backscatter (ZEB) from middle and high clouds. The ZEB signature consists of strong backscatter when the lidar is pointed directly at zenith and a dramatic decline in backscatter as the zenith angle dips slightly off zenith. Mirror-like reflection from horizontal facets of oriented crystals (especially plates) is generally accepted as the cause. It was found during a 3-year observation program that approximately 50 percent of ice clouds had ZEB, regardless of cloud height. The orientation of crystals and the ZEB they cause are important to study and understand for several reasons. First, radiative transfer in clouds with oriented crystals is different than if the same particles were randomly oriented. Second, crystal growth depends partly on the orientation of the particles. Third, ZEB measurements may provide useful information about cirrus microphysical and radiative properties. Finally, the remarkable effect of ZEB on lidar signals should be understood in order to properly interpret lidar data.

Single crystal growth in spin-coated films of polymorphic phthalocyanine derivative under solvent vapor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Higashi, T.; Ohmori, M.; Ramananarivo, M. F.

2015-12-01

The effects of solvent vapor on spin-coated films of a polymorphic phthalocyanine derivative were investigated. Growth of single crystal films via redissolving organic films under solvent vapor was revealed by in situ microscopic observations of the films. X-ray diffraction measurement of the films after exposing to solvent vapor revealed the phase transition of polymorphs under solvent vapor. The direction of crystal growth was clarified by measuring the crystal orientation in a grown monodomain film. The mechanism of crystal growth based on redissolving organic films under solvent vapor was discussed in terms of the different solubilities of the polymorphs.

Solid-phase crystallization of amorphous Si films on glass and Si wafer

NASA Astrophysics Data System (ADS)

Lee, Dong Nyung

2011-11-01

When amorphous silicon films deposited on glass by physical or chemical vapor deposition are annealed, they undergo crystallization by nucleation and growth. The growth rate of Si crystallites is the highest in their <111> directions along or nearly along the film surface. The directed crystallization is likely to develop the <110>//ND or <111>//ND oriented Si crystallites. As the annealing temperature increases, the equiaxed crystallization increases, which in turn increases the random orientation. When amorphous Si is under a stress of the order of 0.1 GPa at about 540 °C, the tensile stress increases the growth rate of Si grains, whereas the compressive stress decreases the growth rate. However, the crystal growth rate increases with the increasing hydrostatic pressure, when the pressure is of the order of GPa at 530-540 °C. These phenomena have been discussed based on the directed crystallization model advanced before, which has been further elaborated.

Growth of organic crystals via attachment and transformation of nanoscopic precursors

NASA Astrophysics Data System (ADS)

Jiang, Yuan; Kellermeier, Matthias; Gebaue, Denis; Lu, Zihao; Rosenberg, Rose; Moise, Adrian; Przybylski, Michael; Cölfen, Helmut

2017-06-01

A key requirement for the understanding of crystal growth is to detect how new layers form and grow at the nanoscale. Multistage crystallization pathways involving liquid-like, amorphous or metastable crystalline precursors have been predicted by theoretical work and have been observed experimentally. Nevertheless, there is no clear evidence that any of these precursors can also be relevant for the growth of crystals of organic compounds. Herein, we present a new growth mode for crystals of DL-glutamic acid monohydrate that proceeds through the attachment of preformed nanoscopic species from solution, their subsequent decrease in height at the surface and final transformation into crystalline 2D nuclei that eventually build new molecular layers by further monomer incorporation. This alternative mechanism provides a direct proof for the existence of multistage pathways in the crystallization of molecular compounds and the relevance of precursor units larger than the monomeric constituents in the actual stage of growth.

Single Crystals Grown Under Unconstrained Conditions

NASA Astrophysics Data System (ADS)

Sunagawa, Ichiro

Based on detailed investigations on morphology (evolution and variation in external forms), surface microtopography of crystal faces (spirals and etch figures), internal morphology (growth sectors, growth banding and associated impurity partitioning) and perfection (dislocations and other lattice defects) in single crystals, we can deduce how and by what mechanism the crystal grew and experienced fluctuation in growth parameters through its growth and post-growth history under unconstrained condition. The information is useful not only in finding appropriate way to growing highly perfect and homogeneous single crystals, but also in deciphering letters sent from the depth of the Earth and the Space. It is also useful in discriminating synthetic from natural gemstones. In this chapter, available methods to obtain molecular information are briefly summarized, and actual examples to demonstrate the importance of this type of investigations are selected from both natural minerals (diamond, quartz, hematite, corundum, beryl, phlogopite) and synthetic crystals (SiC, diamond, corundum, beryl).

Preliminary investigations of protein crystal growth using the Space Shuttle

NASA Technical Reports Server (NTRS)

Delucas, L. J.; Suddath, F. L.; Snyder, R.; Naumann, R.; Broom, M. B.; Pusey, M.; Yost, V.; Herren, B .; Carter, D.

1986-01-01

Four preliminary Shuttle experiments are described which have been used to develop prototype hardware for a more advanced system that will evaluate effects of gravity on protein crystal growth. The first phase of these experiments has centered on the development of micromethods for protein crystal growth by vapor-diffusion techniques (using a space version of the hanging-drop method) and on dialysis using microdialysis cells. Results suggest that the elimination of density-driven sedimentation can effect crystal morphology. In the dialysis experiment, space-grown crystals of concanavalin B were three times longer and 1/3 the thickness of earth-grown crystals.

Isothermal crystallization kinetic modeling of poly(etherketoneketone) (PEKK)

NASA Astrophysics Data System (ADS)

Choupin, T.; Paris, C.; Cinquin, J.; Fayolle, B.; Régnier, G.

2016-05-01

Isothermal melt and cold crystallization kinetics of poly(etherketoneketone) (PEKK) have been investigated by differential scanning calorimetry. A modified Avrami model has been used to describe the two-stage crystallization of PEKK. The primary crystallization stage is assumed to be a two dimensional nucleation growth with an Avrami exponent of 2 whereas the secondary stage is assumed to be a one dimensional nucleation growth with an Avrami exponent of 1. The evolution of the crystallization constant rates depending on temperature has been modeled with the Hoffman and Lauritzen growth equation. The activation energy of nucleation constants Kg for both crystallizations are presented.

Can Solution Supersaturation Affect Protein Crystal Quality?

NASA Technical Reports Server (NTRS)

Gorti, Sridhar

2013-01-01

The formation of large protein crystals of "high quality" is considered a characteristic manifestation of microgravity. The physical processes that predict the formation of large, high quality protein crystals in the microgravity environment of space are considered rooted in the existence of a "depletion zone" in the vicinity of crystal. Namely, it is considered reasonable that crystal quality suffers in earth-grown crystals as a result of the incorporation of large aggregates, micro-crystals and/or large molecular weight "impurities", processes which are aided by density driven convective flow or mixing at the crystal-liquid interface. Sedimentation and density driven convection produce unfavorable solution conditions in the vicinity of the crystal surface, which promotes rapid crystal growth to the detriment of crystal size and quality. In this effort, we shall further present the hypothesis that the solution supersaturatoin at the crystal surface determines the growth mechanism, or mode, by which protein crystals grow. It is further hypothesized that protein crystal quality is affected by the mechanism or mode of crystal growth. Hence the formation of a depletion zone in microgravity environment is beneficial due to inhibition of impurity incorporatoin as well as preventing a kinetic roughening transition. It should be noted that for many proteins the magnitude of neither protein crystal growth rates nor solution supersaturation are predictors of a kinetic roughening transition. That is, the kinetic roughening transition supersaturation must be dtermined for each individual protein.

Automation of Space Processing Applications Shuttle payloads

NASA Technical Reports Server (NTRS)

Crosmer, W. E.; Neau, O. T.; Poe, J.

1975-01-01

The Space Processing Applications Program is examining the effect of weightlessness on key industrial materials processes, such as crystal growth, fine-grain casting of metals, and production of unique and ultra-pure glasses. Because of safety and in order to obtain optimum performance, some of these processes lend themselves to automation. Automation can increase the number of potential Space Shuttle flight opportunities and increase the overall productivity of the program. Five automated facility design concepts and overall payload combinations incorporating these facilities are presented.

Growth Angle - a Microscopic View

NASA Technical Reports Server (NTRS)

Mazurak, K.; Volz, M. P.; Croll, A.

2017-01-01

The growth angle that is formed between the side of the growing crystal and the melt meniscus is an important parameter in the detached Bridgman crystal growth method, where it determines the extent of the crystal-crucible wall gap, and in the Czochralski and float zone methods, where it influences the size and stability of the crystals. The growth angle is a non-equilibrium parameter, defined for the crystal growth process only. For a melt-crystal interface translating towards the crystal (melting), there is no specific angle defined between the melt and the sidewall of the solid. In this case, the corner at the triple line becomes rounded, and the angle between the sidewall and the incipience of meniscus can take a number of values, depending on the position of the triple line. In this work, a microscopic model is developed in which the fluid interacts with the solid surface through long range van der Waals or Casimir dispersive forces. This growth angle model is applied to Si and Ge and compared with the macroscopic approach of Herring. In the limit of a rounded corner with a large radius of curvature, the wetting of the melt on the crystal is defined by the contact angle. The proposed microscopic approach addresses the interesting issue of the transition from a contact angle to a growth angle as the radius of curvature decreases.

Compound semi-conductors and controlled doping thereof

NASA Technical Reports Server (NTRS)

Larkin, David J. (Inventor); Neudeck, Philip G. (Inventor); Powell, J. Anthony (Inventor); Matus, Lawrence G. (Inventor)

1998-01-01

A method of controlling the amount of impurity incorporation in a crystal grown by a chemical vapor deposition process. Conducted in a growth chamber, the method includes the controlling of the concentration of the crystal growing components in the growth chamber to affect the demand of particular growth sites within the growing crystal thereby controlling impurity incorporation into the growth sites.

Evolution of the Shape of Detached GeSi Crystals in Microgravity

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.

2013-01-01

A series of GeSi crystal growth experiments are planned to be conducted in the Low Gradient Furnace (LGF) onboard the International Space Station. An objective of these experiments is to understand the mechanisms of detached Bridgman growth, a process in which a gap exists between the growing semiconductor crystal and the crucible wall. Crystals grown without wall contact have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in crystals. Numerical calculations are used to determine the conditions in which a gap can exist. According to crystal shape stability theory, only some of these gap widths will be dynamically stable. Beginning with a crystal diameter that differs from stable conditions, the transient crystal growth process is analyzed. In microgravity, dynamic stability depends only on capillary effects and is decoupled from heat transfer. Depending on the initial conditions and growth parameters, the crystal shape will evolve towards the crucible wall, towards a stable gap width, or towards the center of the crucible, collapsing the meniscus.

Zeolite Crystal Growth (ZCG) Flight on USML-2

NASA Technical Reports Server (NTRS)

Sacco, Albert, Jr.; Bac, Nurcan; Warzywoda, Juliusz; Guray, Ipek; Marceau, Michelle; Sacco, Teran L.; Whalen, Leah M.

1997-01-01

The extensive use of zeolites and their impact on the world's economy has resulted in many efforts to characterize their structure, and improve the knowledge base for nucleation and growth of these crystals. The zeolite crystal growth (ZCG) experiment on USML-2 aimed to enhance the understanding of nucleation and growth of zeolite crystals, while attempting to provide a means of controlling the defect concentration in microgravity. Zeolites A, X, Beta, and Silicalite were grown during the 16 day - USML-2 mission. The solutions where the nucleation event was controlled yielded larger and more uniform crystals of better morphology and purity than their terrestrial/control counterparts. The external surfaces of zeolite A, X, and Silicalite crystals grown in microgravity were smoother (lower surface roughness) than their terrestrial controls. Catalytic studies with zeolite Beta indicate that crystals grown in space exhibit a lower number of Lewis acid sites located in micropores. This suggests fewer structural defects for crystals grown in microgravity. Transmission electron micrographs (TEM) of zeolite Beta crystals also show that crystals grown in microgravity were free of line defects while terrestrial/controls had substantial defects.

Wafer-scale single-crystal perovskite patterned thin films based on geometrically-confined lateral crystal growth

PubMed Central

Lee, Lynn; Baek, Jangmi; Park, Kyung Sun; Lee, Yong-EunKoo; Shrestha, Nabeen K.; Sung, Myung M.

2017-01-01

We report a facile roll-printing method, geometrically confined lateral crystal growth, for the fabrication of large-scale, single-crystal CH3NH3PbI3 perovskite thin films. Geometrically confined lateral crystal growth is based on transfer of a perovskite ink solution via a patterned rolling mould to a heated substrate, where the solution crystallizes instantly with the immediate evaporation of the solvent. The striking feature of this method is that the instant crystallization of the feeding solution under geometrical confinement leads to the unidirectional lateral growth of single-crystal perovskites. Here, we fabricated single-crystal perovskites in the form of a patterned thin film (3 × 3 inch) with a high carrier mobility of 45.64 cm2 V−1 s−1. We also used these single-crystal perovskite thin films to construct solar cells with a lateral configuration. Their active-area power conversion efficiency shows a highest value of 4.83%, which exceeds the literature efficiency values of lateral perovskite solar cells. PMID:28691697

Direct observation of nanowire growth and decomposition.

PubMed

Rackauskas, Simas; Shandakov, Sergey D; Jiang, Hua; Wagner, Jakob B; Nasibulin, Albert G

2017-09-26

Fundamental concepts of the crystal formation suggest that the growth and decomposition are determined by simultaneous embedding and removal of the atoms. Apparently, by changing the crystal formation conditions one can switch the regimes from the growth to decomposition. To the best of our knowledge, so far this has been only postulated, but never observed at the atomic level. By means of in situ environmental transmission electron microscopy we monitored and examined the atomic layer transformation at the conditions of the crystal growth and its decomposition using CuO nanowires selected as a model object. The atomic layer growth/decomposition was studied by varying an O 2 partial pressure. Three distinct regimes of the atomic layer evolution were experimentally observed: growth, transition and decomposition. The transition regime, at which atomic layer growth/decomposition switch takes place, is characterised by random nucleation of the atomic layers on the growing {111} surface. The decomposition starts on the side of the nanowire by removing the atomic layers without altering the overall crystal structure, which besides the fundamental importance offers new possibilities for the nanowire manipulation. Understanding of the crystal growth kinetics and nucleation at the atomic level is essential for the precise control of 1D crystal formation.

Isothermal dendritic growth: A low gravity experiment

NASA Technical Reports Server (NTRS)

Glicksman, M. E.; Hahn, R. C.; Lograsso, T. A.; Rubinstein, E. R.; Selleck, M. E.; Winsa, E.

1988-01-01

The Isothermal Dendritic Growth Experiment is an active crystal growth experiment designed to test dendritic growth theory at low undercoolings where convection prohibits such studies at 1 g. The experiment will be essentially autonomous, though limited in-flight interaction through a computer interface is planned. One of the key components of the apparatus will be a crystal growth chamber capable of achieving oriented single crystal dendritic growth. Recent work indicates that seeding the chamber with a crystal of the proper orientation will not, in and of itself, be sufficient to meet this requirement. Additional flight hardware and software required for the STS flight experiment are currently being developed at NASA Lewis Research Center and at Rensselaer Polytechnic Institute.

Vapor Growth of Binary and Ternary Chalcogenides in Preparation for Microgravity Experiments

NASA Technical Reports Server (NTRS)

Su, C.; Whitaker, Ann F. (Technical Monitor)

2001-01-01

In the bulk crystal growth of some technologically important semiconducting chalcopyrites, such as ZnTe, CdS, ZnSe and ZnS, vapor growth techniques have significant advantages over melt growth techniques due to the high melting points of these materials. The realization of routine production of high-quality single crystals of these semiconductors requires a fundamental, systematic and in-depth study on the PVT growth process and crystal growth by vapor transport in low gravity offers a set of unique conditions for this study. Previously, two reasons have been put forward to account for this. The first is weight-related reductions in crystal strain and defects. These are thought to be caused by the weight of the crystals during processing at elevated temperatures and retained on cooling, particularly for materials with a low yield strength. The second, and more general, reason is related to the reduction in density-gradient driven convection. The PVT crystal growth process consists of essentially three processes: sublimation of the source material, transport of the vapor species and condensation of the vapor species to form the crystal. The latter two processes can be affected by the convection caused by gravitational accelerations on Earth. Reductions in such convection in low gravity is expected to yield a nearly diffusion-limited growth condition which results in more uniform growth rates (on the microscopic scale) and hence greater crystalline perfection and compositional homogeneity. The reduction of convective contamination by performing flight experiments in a reduced gravity environment will help to understand the relation between fluid phase processes (growth parameters) and defect and impurity incorporation in grown crystals.

On melt solutions for the growth of CaTiO3 crystals

NASA Astrophysics Data System (ADS)

Klimm, Detlef; Schmidt, Max; Wolff, Nora; Guguschev, Christo; Ganschow, Steffen

2018-03-01

When calcium titanate crystals are grown from stoichiometric melts, they crystallize in the cubic perovskite structure. Upon cooling to room temperature they undergo subsequent phase transitions to tetragonal and orthorhombic modifications. These phase transitions are disruptive and result in severely damaged crystals. This paper presents differential thermal analysis data for several prospective solvents, with the aim to identify a system offering the possibility to perform crystal growth of undistorted CaTiO3 crystals by crystallizing them significantly below the melting point directly in the low temperature modification. From mixtures CaF2:TiO2:CaTiO3 = 3:1:1 (molar ratio) the growth of undistorted, at least millimeter-sized CaTiO3 crystals is possible.

Hydrothermal crystal growth of oxides for optical applications

NASA Astrophysics Data System (ADS)

McMillen, Colin David

2007-12-01

The manipulation of light has proven to be an integral part of today's technology-based society. In particular, there is great interest in obtaining coherent radiation in all regions of the optical spectrum to advance technology in military, medical, industrial, scientific and consumer fields. Exploring new crystal growth techniques as well as the growth of new optical materials is critical in the advancement of solid state optics. Surprisingly, the academic world devotes little attention to the growth of large crystals. This shortcoming has left gaps in the optical spectrum inaccessible by solid state devices. This dissertation explores the hydrothermal crystal growth of materials that could fill two such gaps. The first gap exists in the deep-UV region, particularly below 200 nm. Some materials such as LiB3O5 and beta-BaB2O4 can generate coherent light at wavelengths as low as 205 nm. The growth of these materials was explored to investigate the feasibility of the hydrothermal method as a new technique for growing these crystals. Particular attention was paid to the descriptive chemistry surrounding these systems, and several novel structures were elucidated. The study was also extended to the growth of materials that could be used for the generation of coherent light as low as 155 nm. Novel synthetic schemes for Sr2Be2B2O7 and KBe2BO 3F2 were developed and the growth of large crystals was explored. An extensive study of the structures, properties and crystal growth of related compounds, RbBe2BO3F2 and CsBe2BO 3F2, was also undertaken. Optimization of a number of parameters within this family of compounds led to the hydrothermal growth of large, high quality single crystal at rates suitable for large-scale growth. The second gap in technology is in the area of high average power solid state lasers emitting in the 1 mum and eye-safe (>1.5 mum) regions. A hydrothermal technique was developed to grow high quality crystals of Sc 2O3 and Sc2O3 doped with suitable lanthanide activator ions. Preliminary spectroscopic studies were performed and large crystals were again grown at rates suitable for commercial production. The synthesis of ultra-high purity Ln2O3 (Ln = Sc, Y, La-Lu) nanoparticles was also explored to advance the development of ceramic-based solid state lasers. Crystal growth is a complex task involving a great number of intricacies that must be understood and balanced. This dissertation has advanced the art and science of growing crystals, and documented the development of large, high quality crystals of advanced optical materials The materials and hydrothermal crystal growth techniques developed over the course of this work represent important progress toward controlling the optical spectrum.

Growth Temperature Dependence of Morphology of GaN Single Crystals in the Na-Li-Ca Flux Method

NASA Astrophysics Data System (ADS)

Wu, Xi; Hao, Hangfei; Li, Zhenrong; Fan, Shiji; Xu, Zhuo

2018-02-01

In this paper, the effect of growth temperature on the morphology and transparency of the GaN crystals obtained by the Li-Ca-added Na Flux method was studied. Addition of Li-Ca was attempted to control the growth habit and further improve transparency of GaN crystals. The samples with wurtzite structure of GaN were confirmed by the x-ray powder diffraction analysis. GaN single crystal with maximum size of about 6 mm was grown at 750°C. As the growth temperature was increased from 700°C to 850°C, the morphology of the crystals changed from pyramid to prism, and their surfaces became smooth. It was found that high growth temperature was beneficial to obtain a transparent crystal, but the evaporation of sodium would suppress its further growth. The E 2 (high) mode in the Raman spectra was at 568 cm-1, and the full-width at half-maximum values of this peak for the crystals obtained at 700°C, 750°C, 800°C, and 850°C were 7.5 cm-1, 10.3 cm-1, 4.4 cm-1, and 4.0 cm-1, respectively. It indicates that all the crystals are stress free and the transparent crystal grown at high temperature has high structural quality or low impurity concentrations.

The perfection and defect structure of organic hourglass inclusion K 2SO 4 crystals

NASA Astrophysics Data System (ADS)

Vetter, William M.; Totsuka, Hirono; Dudley, Michael; Kahr, Bart

2002-06-01

Hourglass inclusion crystals of K 2SO 4 were grown from aqueous solutions containing the dye acid fuchsin, and studied by synchrotron white-beam X-ray topography and reciprocal space mapping. Both self-nucleated and larger, seeded dye-included crystals were prepared, as well as comparable undoped crystals. While the dye modified the crystals' habit strongly, X-ray topographs showed it had no influence on their dislocation configurations, which were typical for solution-grown crystals. No kinematical contrast arising from the presence of the dye was observed that indicated dye-induced strain in the crystal lattice. Growth sector boundaries were visible in the dyed crystals but not in undoped crystals, implying there was a slightly higher lattice mismatch across growth sector boundaries in the dye-included crystals. Reciprocal space maps of small areas on an hourglass inclusion crystal within either a dye-included growth sector or an undoped growth sector showed single peaks with the same perfect crystal rocking curve width and no dilatation or tilt of the host lattice resulting from the dye's presence. These results showed hourglass inclusion crystals can be grown in which the presence of the dye disturbs the crystalline structure of the host salt minimally, and that hourglass inclusions have the nature of a solid solution.

Growth of InSb and InI Crystals on Earth and in Microgravity

NASA Technical Reports Server (NTRS)

Ostrogorsky, A. G.; Churilov, A.; Volz, M. P.; Riabov, V.; Van den Berg, L.

2015-01-01

During the past 40 years, dozens of semiconductor crystal growth experiments have been conducted in space laboratories. The subsequent analysis of the space-grown crystals revealed (i) that weak convection existed in virtually all melt-growth experiments, (ii) de-wetting significantly reduced the level of stress-induced defects, and (iii) particularly encouraging results were obtained in vapor-growth experiments. In 2002, following a decade of ground based research in growing doped Ge and GaSb crystals, a series of crystal growth experiments was performed at the ISS, within the SUBSA (Solidification Using a Baffle in Sealed Ampoules) investigation. Te- and Zn-doped InSb crystals were grown from the melt. The specially designed furnace provided a side-view of the melt and precise seeding measurement of the growth rate. At present, under sponsorship of CASIS (Center for the Advancement of Science in Space, www.iss-casis.org), we are conducting ground-based experiments with indium mono-iodide (InI) in preparation for the "SUBSA II" ISS investigation, planned for 2017. The experiments include: i) Horizontal Bridgman (HB) growth and ii) Vapor Transport (VT) growth. Finite element modeling will also be conducted, to optimize the design of the flight ampoules, for vapor and melt growth.

Fluid Physics and Macromolecular Crystal Growth in Microgravity

NASA Technical Reports Server (NTRS)

Pusey, M.; Snell, E.; Judge, R.; Chayen, N.; Boggon, T.; Helliwell, J.; Rose, M. Franklin (Technical Monitor)

2000-01-01

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.

ICCG-10: Tenth International Conference on Crystal Growth. Oral presentation abstracts

NASA Technical Reports Server (NTRS)

1992-01-01

Oral presentation abstracts from the tenth International Conference on Crystal Growth (ICCG) (Aug. 16-21, 1992) are provided. Topics discussed at the conference include superconductors, semiconductors, nucleation, crystal growth mechanisms, and laser materials. Organizing committees, ICCG advisory board and officers, and sponsors of the conference are also included.

Validation of mathematical model for CZ process using small-scale laboratory crystal growth furnace

NASA Astrophysics Data System (ADS)

Bergfelds, Kristaps; Sabanskis, Andrejs; Virbulis, Janis

2018-05-01

The present material is focused on the modelling of small-scale laboratory NaCl-RbCl crystal growth furnace. First steps towards fully transient simulations are taken in the form of stationary simulations that deal with the optimization of material properties to match the model to experimental conditions. For this purpose, simulation software primarily used for the modelling of industrial-scale silicon crystal growth process was successfully applied. Finally, transient simulations of the crystal growth are presented, giving a sufficient agreement to experimental results.

Erbium Distribution in Single Crystal YAG Fibers Grown by Laser-Heated Pedestal Growth Technique

DTIC Science & Technology

2015-08-28

single crystal YAG fibers grown by laser - heated pedestal growth technique Single crystal (SC) yttrium aluminum garnet (YAG, Y3Al5O12) as a host...inserted into a SC YAG tube. This rod-in-tube was used as a preform in our laser -heated pedestal growth (LHPG) apparatus to grow a fiber with a radial...fibers grown by laser -heated pedestal growth technique Report Title Single crystal (SC) yttrium aluminum garnet (YAG, Y3Al5O12) as a host material has

Preliminary Work in Obtaining Site-Directed Mutants of Hen Egg White Lysozyme

NASA Technical Reports Server (NTRS)

Holmes, Leonard D.

1996-01-01

Protein crystal growth studies are recognized as a critical endeavor in the field of molecular biotechnology. The scientific applications of this field include the understanding of how enzymes function and the accumulation of accurate information of atomic structures, a key factor in the process of rational drug design. NASA has committed substantial investment and resources to the field of protein crystal growth and has conducted many microgravity protein crystal growth experiments aboard shuttle flights. Crystals grown in space tend to be larger, denser and have a more perfect habit and geometry. These improved properties gained in the microgravity environment of space result largely from the reduction of solutal convection, and the elimination of sedimentation at the growing crystal surface. Shuttle experiments have yielded many large, high quality crystals that are suitable for high resolution X-ray diffraction analysis. Examples of biologically important macromolecules which have been successfully crystallized during shuttle missions include: lysozyme, isocitrate lyase, gamma-interferon, insulin, human serum albumin and canavalin. Numerous other examples are also available. In addition to obtaining high quality crystals, investigators are also interested in learning the mechanisms by which the growth events take place. Crystallization experiments indicate that for the enzyme HEWL, measured growth rates do not follow mathematical models for 2D nucleation and dislocation-led growth of tetragonal protein crystals. As has been suggested by the laboratory of Marc L. Pusey, a possible explanation for the disagreement between observation and data is that HEWL tetraconal crystals form by aggregated units of lysozyme in supersaturated solutions. Surface measurement data was shown to fit very well with a model using an octamer unit cell as the growth unit. According to this model, the aggregation pathway and subsequent crystal growth is described by: monomer < ------ > dimer < ------- > tetramer < ------ > octamer < ------ > higher order. It is believed that multimer aggregation of lysozyme occurs by interaction at specific binding sites on the surface of the protein crystals. If the presence of discrete binding sites and the aggregation hypothesis is true, then it follows that the alteration of the binding site(s) should have significant effect on the measurements obtained during growth experiments. Site-directed mutagenesis allows the specific alteration of proteins by replacement, deletion or addition of specific amino acid residues. This report outlines the approach for this strategy and the progress made thus far toward that end.

Uncovering molecular details of urea crystal growth in the presence of additives.

PubMed

Salvalaglio, Matteo; Vetter, Thomas; Giberti, Federico; Mazzotti, Marco; Parrinello, Michele

2012-10-17

Controlling the shape of crystals is of great practical relevance in fields like pharmacology and fine chemistry. Here we examine the paradigmatic case of urea which is known to crystallize from water with a needle-like morphology. To prevent this undesired effect, inhibitors that selectively favor or discourage the growth of specific crystal faces can be used. In urea the most relevant faces are the {001} and the {110} which are known to grow fast and slow, respectively. The relevant growth speed difference between these two crystal faces is responsible for the needle-like structure of crystals grown in water solution. To prevent this effect, additives are used to slow down the growth of one face relative to another, thus controlling the shape of the crystal. We study the growth of fast {001} and slow {110} faces in water solution and the effect of shape controlling inhibitors like biuret. Extensive sampling through molecular dynamics simulations provides a microscopic picture of the growth mechanism and of the role of the additives. We find a continuous growth mechanism on the {001} face, while the slow growing {110} face evolves through a birth and spread process, in which the rate-determining step is the formation on the surface of a two-dimensional crystalline nucleus. On the {001} face, growth inhibitors like biuret compete with urea for the adsorption on surface lattice sites; on the {110} face instead additives cannot interact specifically with surface sites and play a marginal sterical hindrance of the crystal growth. The free energies of adsorption of additives and urea are evaluated with advanced simulation methods (well-tempered metadynamics) allowing a microscopic understanding of the selective effect of additives. Based on this case study, general principles for the understanding of the anisotropic growth of molecular crystals from solutions are laid out. Our work is a step toward a rational development of novel shape-affecting additives.

Hot zone design for controlled growth to mitigate cracking in laser crystal growth

NASA Astrophysics Data System (ADS)

Zhang, Hui; Zheng, Lili; Fang, Haisheng

2011-03-01

Cracking is a major problem during large diameter crystal growth. The objective of this work is to design an effective hot zone for a controlled growth of Yb:S-FAP [Yb3+:Sr5(PO4)3F] laser crystal by the Czochralski technology and effective cooling that can reduce stress. Theoretical and numerical analyses are performed to study the causes of cracking, mitigate the major cracking, as well as reduce cooling time. In the current system, three locations in the crystal are prone to crack, such as the top shoulder of the crystal, the middle portion above the crucible edge, and the bottom tail portion. Based on numerical simulations, we propose a new hot zone design and cooling procedure to grow and cool large diameter crystal without cracking.

Growth of PBI 2 single crystals from stoichiometric and Pb excess melts

NASA Astrophysics Data System (ADS)

Hayashi, T.; Kinpara, M.; Wang, J. F.; Mimura, K.; Isshiki, M.

2008-01-01

We have successfully grown high-purity and -quality PbI 2 single crystals by the vertical Bridgman method. The rocking curves of four-crystal X-ray diffraction (XRD) show 120 arcsec in full-width at half-maximum (FWHM). The photoluminescence (PL) spectra at 7.8 K show the resolved intensive exciton emission line and the weak DAP emission band. The deep-level emissions are not observed. The measurement of the electrical and radiographic properties show that Leadiodide (PbI 2) single crystal has a resistivity of 5×10 10 Ω cm and imager lag is 8 s, respectively. In order to improve the controllability of crystal growth, PbI 2 single crystals were also grown from a lead (Pb) excess PbI 2 source. The experimental results show very good reproducibility. In addition, the growth models of crystal are proposed, and the growth mechanism is discussed.

Retardation of ice crystallization by short peptides

NASA Astrophysics Data System (ADS)

Kim, Jun Soo; Yethiraj, Arun

2009-03-01

The effect of short peptides on the growth of ice crystals is studied using molecular dynamics simulations. The simulations focus on two sequences (Gly-Pro-Ala-Gly and Gly-Gly-Ala-Gly) that are found in collagen hydrolysate, a substance that is known to retard crystal growth. In the absence of peptides, the growth of ice crystal in the solution with the ice/water interface is observed in at a rate comparable to the experimental data. When peptides are present in the liquid phase, the crystal growth is retarded to a significant extent compared to the pure water. It is found that Gly-Pro-Ala-Gly is more effective (crystallization is up to 5 times slower than in its absence) than Gly-Gly-Ala-Gly (up to 3 times slower) implying that the role of the proline residue is important. The mechanism can be understood in the nature of binding of the peptides to the growing crystal.

Nucleation and Crystallization of Globular Proteins: What we Know and What is Missing

NASA Technical Reports Server (NTRS)

Rosenberger, F.; Vekilov, P. G.; Muschol, M.; Thomas, B. R.

1996-01-01

Recently. much progress has been made in understanding the nucleation and crystallization of globular proteins, including the formation of compositional and structural crystal defects, Insight into the interactions of (screened) protein macro-ions in solution, obtained from light scattering, small angle X-ray scattering and osmotic pressure studies. can guide the search for crystallization conditions. These studies show that the nucleation of globular proteins is governed by the same principles as that of small molecules. However, failure to account for direct and indirect (hydrodynamic) protein interactions in the solutions results in unrealistic aggregation scenarios. Microscopic studies of numerous proteins reveal that crystals grow by the attachment of growth units through the same layer-spreading mechanisms as inorganic crystals. Investigations of the growth kinetics of hen-egg-white lysozyme (HEWL) reveal non-steady behavior under steady external conditions. Long-term variations in growth rates are due to changes in step-originating dislocation groups. Fluctuations on a shorter timescale reflect the non-linear dynamics of layer growth that results from the interplay between interfacial kinetics and bulk transport. Systematic gel electrophoretic analyses suggest that most HEWL crystallization studies have been performed with material containing other proteins at percent levels. Yet, sub-percent levels of protein impurities impede growth step propagation and play a role in the formation of structural/compositional inhomogeneities. In crystal growth from highly purified HEWL solutions, however, such inhomogeneities are much weaker and form only in response to unusually large changes in growth conditions. Equally important for connecting growth conditions to crystal perfection and diffraction resolution are recent advances in structural characterization through high-resolution Bragg reflection profiling and X-ray topography.

Calcium Carbonate Crystal Growth in Porous Media, in the presence of Water Miscible and Non-Miscible Organic Fluids

NASA Astrophysics Data System (ADS)

Jaho, Sofia; Sygouni, Varvara; Paraskeva, Christakis A.

2015-04-01

The deposition of sparingly soluble salts (scaling) within porous media is a major problem encountered in many industrial and environmental applications. In the oil industry scaling causes severe operational malfunctions and, therefore, increasing the total operating and maintenance cost [1]. The most common types of sparingly soluble salts located in oil fields include carbonate and sulfate salts of calcium, strondium and barium[1,2]. Multiple phase flow and tubing surface properties are some of the factors affecting scale formation [3]. The main purpose of the present work was the investigation of the precipitation mechanisms of calcium carbonate (CaCO3) through in situ mixing of two soluble salt solutions in a flow granular medium, in the presence of water miscible organic fluid (ethylene glycol) or non-miscible organic fluid (n-dodecane). All series of experiments were carried out in a two dimensional porous medium made of Plexiglas. For all solutions used in the experiments, the contact angles with the surface of the porous medium and the interfacial tensions were measured. During the experiments, the calcium carbonate crystal growth was continuously monitored and recorded through an optical microscope equipped with a digital programmed video camera. The snap-shots were taken within specific time intervals and their detailed procession gave information concerning the crystal growth rate and kinetics. The pH of the effluent was measured and fluids samples were collected for calcium analysis using Atomic Absorption Spectroscopy (AAS). In all experiments effluent calcium concentration decreased as a function of time, suggesting that CaCO3 precipitation took place inside the porous medium. Crystals of the precipitated salt were identified using Infrared Spectroscopy (IR) and the morphology of the crystals was examined using Scanning Electron Microscopy (SEM). The induction time for precipitation of CaCO3 crystals in the presence of n-dodecane was significantly reduced compared to the induction time where no oil phase was present. The interface of n-dodecane and supersaturated solutions seems to be very active and favored the formation of the CaCO3 crystalline enhancing the heterogeneous nucleation which generally demands a decreased energy barrier. Acknowledgments This research was partially funded by the European Union (European Social Fund-ESF) and Greek National Funds through the Operational Program "Education and Lifelong Learning" under the action Aristeia II (Code No4420). References 1. Merdhah A. B. and Yassin A. A., Scale formation in oil reservoir during water injection at high-salinity formation water, Journal of Applied Sciences, 7, 3198-3207 (2007). 2. Moghadasi J., Muller-Steinhagen H., Jamialahmadi M. and Sharif A., Model study on the kinetics of oil field formation damage due to salt precipitation from injection, Journal of Petroleum Science and Engineering, 43, 201-217 (2004). 3. Nancollas G. H. and Reddy M. M., The crystallization of calcium carbonate II. Calcite growth mechanism, Journal of Colloid and Interface Science, 37, 824-830 (1971).

A physicist's view of biotechnology. [small molecule crystal growth in space

NASA Technical Reports Server (NTRS)

Kroes, Roger L.

1987-01-01

Theories and techniques for small molecule crystal growth are reviewed, with emphasis on space processing possibilities, particularly for protein crystal growth. The general principles of nucleation, growth, and mass and heat transport are first discussed. Optical systems using schlieren, shadowgraph, and holographic techniques are considered, and are illustrated with the example of the NASA developed Fluids Experiment System flow aboard Spacelab 3.

Continuous Czochralski growth: Silicon sheet growth development of the large area sheet task of the low cost silicon solar array project

NASA Technical Reports Server (NTRS)

Johnson, C. M.

1980-01-01

The growth of 100 kg of silicon single crystal material, ten cm in diameter or greater, and 150 kg of silicon single crystal material 15 cm or greater utilizing one common silicon container material (one crucible) is investigated. A crystal grower that is recharged with a new supply of polysilicon material while still under vacuum and at temperatures above the melting point of silicon is developed. It accepts large polysilicon charges up to 30 kg, grows large crystal ingots (to 15 cm diameter and 25 kg in weight), and holds polysilicon material for recharging (rod or lump) while, at the same time, growing crystal ingots. Special equipment is designed to recharge polysilicon rods, recharge polysilicon lumps, and handle and store large, hot silicon crystal ingots. Many continuous crystal growth runs were performed lasting as long as 109 hours and producing as many as ten crystal ingots, 15 cm with weights progressing to 27 kg.

Boron Arsenide and Boron Phosphide for High Temperature and Luminescent Devices. [semiconductor devices - crystal growth/crystal structure

NASA Technical Reports Server (NTRS)

Chu, T. L.

1975-01-01

The crystal growth of boron arsenide and boron phosphide in the form of bulk crystals and epitaxial layers on suitable substrates is discussed. The physical, chemical, and electrical properties of the crystals and epitaxial layers are examined. Bulk crystals of boron arsenide were prepared by the chemical transport technique, and their carrier concentration and Hall mobility were measured. The growth of boron arsenide crystals from high temperature solutions was attempted without success. Bulk crystals of boron phosphide were also prepared by chemical transport and solution growth techniques. Techniques required for the fabrication of boron phosphide devices such as junction shaping, diffusion, and contact formation were investigated. Alloying techniques were developed for the formation of low-resistance ohmic contacts to boron phosphide. Four types of boron phosphide devices were fabricated: (1) metal-insulator-boron phosphide structures, (2) Schottky barriers; (3) boron phosphide-silicon carbide heterojunctions; and (4) p-n homojunctions. Easily visible red electroluminescence was observed from both epitaxial and solution grown p-n junctions.

Cylindrically symmetric Green's function approach for modeling the crystal growth morphology of ice.

PubMed

Libbrecht, K G

1999-08-01

We describe a front-tracking Green's function approach to modeling cylindrically symmetric crystal growth. This method is simple to implement, and with little computer power can adequately model a wide range of physical situations. We apply the method to modeling the hexagonal prism growth of ice crystals, which is governed primarily by diffusion along with anisotropic surface kinetic processes. From ice crystal growth observations in air, we derive measurements of the kinetic growth coefficients for the basal and prism faces as a function of temperature, for supersaturations near the water saturation level. These measurements are interpreted in the context of a model for the nucleation and growth of ice, in which the growth dynamics are dominated by the structure of a disordered layer on the ice surfaces.

JAXA protein crystallization in space: ongoing improvements for growing high-quality crystals

PubMed Central

Takahashi, Sachiko; Ohta, Kazunori; Furubayashi, Naoki; Yan, Bin; Koga, Misako; Wada, Yoshio; Yamada, Mitsugu; Inaka, Koji; Tanaka, Hiroaki; Miyoshi, Hiroshi; Kobayashi, Tomoyuki; Kamigaichi, Shigeki

2013-01-01

The Japan Aerospace Exploration Agency (JAXA) started a high-quality protein crystal growth project, now called JAXA PCG, on the International Space Station (ISS) in 2002. Using the counter-diffusion technique, 14 sessions of experiments have been performed as of 2012 with 580 proteins crystallized in total. Over the course of these experiments, a user-friendly interface framework for high accessibility has been constructed and crystallization techniques improved; devices to maximize the use of the microgravity environment have been designed, resulting in some high-resolution crystal growth. If crystallization conditions were carefully fixed in ground-based experiments, high-quality protein crystals grew in microgravity in many experiments on the ISS, especially when a highly homogeneous protein sample and a viscous crystallization solution were employed. In this article, the current status of JAXA PCG is discussed, and a rational approach to high-quality protein crystal growth in microgravity based on numerical analyses is explained. PMID:24121350

Growth of GaN single crystals by a Ca- and Ba-added Na flux method

NASA Astrophysics Data System (ADS)

Ukegawa, H.; Konishi, Y.; Fujimori, T.; Miyoshi, N.; Imade, M.; Yoshimura, M.; Kitaoka, Y.; Sasaki, T.; Mori, Y.

2011-02-01

GaN substrates are desirable for fabricating ultra-violet LEDs and LDs, and high-power and high-frequency transistors. High-quality GaN single crystals can be obtained by using Na flux method, but the growth habit of bulk crystals must be controlled. In this study, we investigated the effects of additives (Ca, Ba) on the growth habit and impurity concentration in the crystals. The aspect ratio (c/a) of the crystals was increased by increasing the amount of additives, showing that the growth habit could be changed from the pyramidal shape to the prism shape. Ba concentration was below the detection limit (1x1015 atoms/cm3).

Influence of Containment on the Growth of Silicon-Germanium (ICESAGE): A Materials Science ISS Investigation

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.; Croll, A.

2014-01-01

A series of Ge(1-x)Si(x) crystal growth experiments are planned to be conducted in the Low Gradient Furnace (LGF) onboard the International Space Station. The primary objective of the research is to determine the influence of containment on the processinginduced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and "detached" Bridgman methods and the ground-based float zone technique. Crystals grown without being in contact with a container have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in crystals. "Detached" or "dewetted" Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. Long duration reduced gravity is essential to test the proposed theory of detached growth. Detached growth requires the establishment of a meniscus between the crystal and the ampoule wall. The existence of this meniscus depends on the ratio of the strength of gravity to capillary forces. On Earth, this ratio is large and stable detached growth can only be obtained over limited conditions. Crystals grown detached on the ground exhibited superior structural quality as evidenced by measurements of etch pit density, synchrotron white beam X-ray topography and double axis X-ray diffraction. The plans for the flight experiments will be described.

Influence of Containment on the Growth of Silicon-Germanium: A Materials Science Flight Project

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.; Croell, A.

2012-01-01

A series of Ge(1-x)Si(x) crystal growth experiments are planned to be conducted in the Low Gradient Furnace (LGF) onboard the International Space Station. The primary objective of the research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and "detached" Bridgman methods and the ground-based float zone technique. Crystals grown without being in contact with a container have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in crystals. "Detached" or "dewetted" Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. Long duration reduced gravity is essential to test the proposed theory of detached growth. Detached growth requires the establishment of a meniscus between the crystal and the ampoule wall. The existence of this meniscus depends on the ratio of the strength of gravity to capillary forces. On Earth, this ratio is large and stable detached growth can only be obtained over limited conditions. Crystals grown detached on the ground exhibited superior structural quality as evidenced by measurements of etch pit density, synchrotron white beam X-ray topography and double axis X-ray diffraction. The plans for the flight experiments will be described.

Effect of L-Valine on the growth and characterization of Sodium Acid Phthalate (SAP) single crystals.

PubMed

Nirmala, L Ruby; Thomas Joseph Prakash, J

2013-06-01

Undoped and amino acid doped good quality single crystals of Sodium Acid Phthalate crystals (SAP) were grown by slow evaporation solution growth technique which are semiorganic in nature. The effect of amino acid (L-Valine) dopant on the growth and the properties of SAP single crystal was investigated. The single crystal X-ray diffraction studies and FT-IR studies were carried out to identify the crystal structure and the presence of functional groups in undoped and L-Valine doped SAP crystals. The transparent nature of the grown crystal was observed using UV-Visible spectrum. The thermal decomposition of the doped SAP crystals was investigated by thermo gravimetric analysis (TGA) and differential thermal analysis (DTA). The enhancement in the NLO property of the undoped and L-Valine doped SAP crystals using KDP crystal as a reference was studied using SHG measurements. Vickers micro hardness measurements are used for the study of mechanical strength of the grown crystals. Copyright © 2013 Elsevier B.V. All rights reserved.

Solar energy concentrator system for crystal growth and zone refining in space

NASA Technical Reports Server (NTRS)

Mcdermit, J. H.

1975-01-01

The technological feasibility of using solar concentrators for crystal growth and zone refining in space has been performed. Previous studies of space-deployed solar concentrators were reviewed for their applicability to materials processing and a new state-of-the-art concentrator-receiver radiation analysis was developed. The radiation analysis is in the form of a general purpose computer program. It was concluded from this effort that the technology for fabricating, orbiting and deploying large solar concentrators has been developed. It was also concluded that the technological feasibility of space processing materials in the focal region of a solar concentrator depends primarily on two factors: (1) the ability of a solar concentrator to provide sufficient thermal energy for the process and (2) the ability of a solar concentrator to provide a thermal environment that is conductive to the processes of interest. The analysis indicate that solar concentrators can satisfactorily provide both of these factors.

Numerical Modeling of Physical Vapor Transport in Contactless Crystal Growth Geometry

NASA Technical Reports Server (NTRS)

Palosz, W.; Lowry, S.; Krishnam, A.; Przekwas, A.; Grasza, K.

1998-01-01

Growth from the vapor under conditions of limited contact with the walls of the growth ampoule is beneficial for the quality of the growing crystal due to reduced stress and contamination which may be caused by interactions with the growth container. The technique may be of a particular interest for studies on crystal growth under microgravity conditions: elimination of some factors affecting the crystal quality may make interpretation of space-conducted processes more conclusive and meaningful. For that reason, and as a part of our continuing studies on 'contactless' growth technique, we have developed a computational model of crystal growth process in such system. The theoretical model was built, and simulations were performed using the commercial computational fluid dynamics code, (CFD) ACE. The code uses an implicit finite volume formulation with a gray discrete ordinate method radiation model which accounts for the diffuse absorption and reflection of radiation throughout the furnace. The three-dimensional model computes the heat transfer through the crystal, quartz, and gas both inside and outside the ampoule, and mass transport from the source to the crystal and the sink. The heat transport mechanisms by conduction, natural convection, and radiation, and mass transport by diffusion and convection are modeled simultaneously and include the heat of the phase transition at the solid-vapor interfaces. As the thermal boundary condition, temperature profile along the walls of the furnace is used. For different thermal profiles and furnace and ampoule dimensions, the crystal growth rate and development of the crystal-vapor and source-vapor interfaces (change of the interface shape and location with time) are obtained. Super/under-saturation in the ampoule is determined and critical factors determining the 'contactless' growth conditions are identified and discussed. The relative importance of the ampoule dimensions and geometry, the furnace dimensions and its temperature, and the properties of the grown material are analyzed. The results of the simulations are compared with related experimental results on growth of CdTe, CdZnTe, ZnTe, PbTe, and PbSnTe crystals by this technique.

Modeling the Growth Rates of Tetragonal Lysozyme Crystal Faces

NASA Technical Reports Server (NTRS)

Li, Meirong; Nadarajah, Arunan; Pusey, Marc L.

1998-01-01

The measured macroscopic growth rates of the (110) and (101) faces of tetragonal lysozyme show an unexpectedly complex dependence on the supersaturation. The growth rates decay asymptotically to zero when the supersaturation is lowered to zero and increase rapidly when the supersaturation is increased. When supersaturations are increased still further the growth rates attain a maximum before starting to decrease. However, growth of these crystals is known to proceed by the classical dislocation and 2D nucleation growth mechanisms. This anomaly can be explained if growth is assumed to occur not by monomer units but by lysozyme aggregates. Analysis of the molecular packing of these crystals revealed that they were constructed of strongly bonded 4(sub 3) helices, while weaker bonds were responsible for binding the helices to each other. It follows that during crystal growth the stronger bonds are formed before the weaker ones. Thus, the growth of these crystals could be viewed as a two step process: aggregate growth units corresponding to the 4(sub 3) helix are first formed in the bulk solution by stronger intermolecular bonds and then attached to the crystal face by weaker bonds on dislocation hillocks or 2D islands. This will lead to a distribution of aggregates in the solution with monomers and lower order aggregates being predominant at low supersaturations and higher order aggregates being predominant at high supersaturations. If the crystal grows mostly by higher order aggregates, such as tetramers and octamers, it would explain the anomalous dependence of the growth rates on the supersaturation. Besides the analysis of molecular packing, a comprehensive analysis of the measured (110) and (101) growth rates was also undertaken in this study. The distribution of aggregates in lysozyme nutrient solutions at various solution conditions were determined from reversible aggregation reactions at equilibrium. The supersaturation was defined for each aggregate species with respect to its concentration at saturation in order to apply growth rate models to this process. The measured growth rates were then compared with the predicted ones from several dislocation and 2D nucleation growth models, employing tetramer and octamer growth units in polydisperse solutions and monomer units in monodisperse solutions. For the (110) face, the calculations consistently showed that the measured growth rates followed the expected model relations with octamer growth units. For the (101) face, it is not possible to obtain a clear agreement between the predicted and measured growth rates for a single growth unit as done for the (110) face. However, the calculations do indicate that the average size of the growth unit is between a tetramer and an octamer. This suggests that tetramers, octamers and other intermediate size growth units all participate in the growth process for this face. These calculations show that it is possible to model the macroscopic protein crystal growth rates if the molecular level processes can be account for, particularly protein aggregation processes in the bulk solution. Our recent investigations of tetragonal lysozyme crystals employing high resolution atomic force microscopy scans have further confirmed the growth of these crystals by aggregate growth units corresponding to 4(sub 3) helices.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jones, B.; Renaut, R.W.

Skeletal crystals are hollow crystals that develop because their outer walls grow before their cores. The presence of skeletal crystals of calcite (three types--trigonal prisms, hexagonal prisms, and plates) and trona in hot (> 90 C) spring deposits in New Zealand (Waikite Springs and Ohaaki Pool) and Kenya (Lorusio hot springs) shows that they can form in natural sedimentary regimes. Analysis of samples from these deposits shows that this crystal morphology develops under disequilibrium conditions that are unrelated to a specific environmental or diagenetic setting. Skeletal crystals transform into solid crystals when subsequent precipitation fills their hollow cores. In somemore » cases, this may involve precipitation of crystalline material that has a sieve-like texture. In other examples, the skeletal crystal provides a framework upon which other materials can be precipitated. Walls in the skeletal trigonal calcite prisms from Waikite Springs are formed of subcrystals that mimic the shape of the parent crystal. Similarly, plate-like skeletal crystals from Lorusio are formed of densely packed subcrystals that are < 0.5 {micro}m long. Conversely, the walls of the skeletal hexagonal calcite crystals from Ohaaki Pool and the skeletal trona crystals from Lorusio are not formed of subcrystals. Recognition of skeletal crystals is important because they represent growth that follows the reverse pattern of normal growth. Failure to recognize that crystal growth followed the skeletal motif may lead to false interpretations concerning the growth of a crystal.« less

Optical diagnostics of mercuric iodide crystal growth

NASA Astrophysics Data System (ADS)

Burger, A.; Morgan, S. H.; Silberman, E.; Nason, D.

Two optical methods were recently developed for in situ monitoring of the growth process of mercuric iodide crystals. The first method uses resonance fluorescence spectroscopy (RFS) for the determination of iodine vapor present in the growth ampule, which is an important parameter in determining the stoichiometry, and therefore the quality of the crystals. The second method, Reflectance Spectroscopy Thermometry (RST) measures the crystal face temperature with a percent accuracy of plus or minus 1.5 C.

Optical diagnostics of mercuric iodide crystal growth

NASA Astrophysics Data System (ADS)

Burger, Arnold; Morgan, Steven H.; Silberman, Enrique; Nason, Donald

1991-12-01

Two optical methods were recently developed for in situ monitoring of the growth process of mercuric iodide crystals. The first method uses resonance fluorescence spectroscopy (RFS) for the determination of iodine vapor present in the growth ampule, which is an important parameter in determining the stoichiometry, and therefore the quality of the crystals. The second method, reflectance spectroscopy thermometry (RST) measures the crystal face temperature with a present accuracy of +/- 1.5 degree(s)C.

Numerical simulation and growth of Li2Zn2(MoO4)3 single crystals by the top seeded solution growth technique

NASA Astrophysics Data System (ADS)

Sukharev, V.; Sukhanova, E.; Mozhevitina, E.; Sadovsky, A.; Avetissov, I.

2017-06-01

Li2O - ZnO - MoO3 pseudo ternary system was used for the growth of Li2Zn2(MoO4)3 crystals by the top seeded solution growth technique in which MoO3 was used as a solvent. Properties of the melts (density, viscosity) have been experimentally measured at different temperatures and compositions of Li2O - ZnO - MoO3 pseudo ternary system. Heat mass transfer in the crystal growth setup was numerically simulated. Using the simulation results a real growth setup was made, Li2Zn2(MoO4)3 crystals were grown and their properties were studied.

New simulation model of multicomponent crystal growth and inhibition.

PubMed

Wathen, Brent; Kuiper, Michael; Walker, Virginia; Jia, Zongchao

2004-04-02

We review a novel computational model for the study of crystal structures both on their own and in conjunction with inhibitor molecules. The model advances existing Monte Carlo (MC) simulation techniques by extending them from modeling 3D crystal surface patches to modeling entire 3D crystals, and by including the use of "complex" multicomponent molecules within the simulations. These advances makes it possible to incorporate the 3D shape and non-uniform surface properties of inhibitors into simulations, and to study what effect these inhibitor properties have on the growth of whole crystals containing up to tens of millions of molecules. The application of this extended MC model to the study of antifreeze proteins (AFPs) and their effects on ice formation is reported, including the success of the technique in achieving AFP-induced ice-growth inhibition with concurrent changes to ice morphology that mimic experimental results. Simulations of ice-growth inhibition suggest that the degree of inhibition afforded by an AFP is a function of its ice-binding position relative to the underlying anisotropic growth pattern of ice. This extended MC technique is applicable to other crystal and crystal-inhibitor systems, including more complex crystal systems such as clathrates.

Radiative heat transport during the vertical Bridgman growth of oxide single crystals: slabs versus cylinders

NASA Astrophysics Data System (ADS)

Virozub, Alexander; Brandon, Simon

1998-10-01

Internal radiative heat transport in oxide crystals during their growth via the vertical Bridgman technique is known to promote severely deflected melt/crystal interface shapes. These highly curved interfaces are likely to encourage unwanted phenomena such as inhomogeneous distribution of impurities in the solidified crystalline material. Past computational analyses of oxide growth systems have mostly been confined to cylindrical geometries. In this letter a two-dimensional finite-element model, describing the growth of slab-shaped oxide crystals via the vertical Bridgman technique, is presented; internal radiative heat transport through the transparent crystalline phase is accounted for in the formulation. Comparison with calculations of cylindrical-shaped crystal growth systems shows a strong dependence of thermal fields and of melt/crystal interface shapes on the crystal geometry. Specifically, the interface position is strongly shifted toward the hot zone and its curvature dramatically increases in slab-shaped systems compared to what is observed in cylindrical geometries. This significant qualitative difference in interface shapes is shown to be linked to large quantitative differences in values of the viewing angle between the hot melt/crystal interface and the cold part of the crucible.

Numerical modeling of Czochralski growth of Li2MoO4 crystals for heat-scintillation cryogenic bolometers

NASA Astrophysics Data System (ADS)

Stelian, Carmen; Velázquez, Matias; Veber, Philippe; Ahmine, Abdelmounaim; Sand, Jean-Baptiste; Buşe, Gabriel; Cabane, Hugues; Duffar, Thierry

2018-06-01

Lithium molybdate Li2MoO4 (LMO) crystals of mass ranging between 350 and 500 g are excellent candidates to build heat-scintillation cryogenic bolometers likely to be used for the detection of rare events in astroparticle physics. In this work, numerical modeling is applied in order to investigate the Czochralski growth of Li2MoO4 crystals in an inductive furnace. The numerical model was validated by comparing the numerical predictions of the crystal-melt interface shape to experimental visualization of the growth interface. Modeling was performed for two different Czochralski furnaces that use inductive heating. The simulation of the first furnace, which was used to grow Li2MoO4 crystals of 3-4 cm in diameter, reveals non-optimal heat transfer conditions for obtaining good quality crystals. The second furnace, which will be used to grow crystals of 5 cm in diameter, was numerically optimized in order to reduce the temperature gradients in the crystal and to avoid fast crystallization of the bath at the later stages of the growth process.

(PCG) Protein Crystal Growth Horse Serum Albumin

NASA Technical Reports Server (NTRS)

1995-01-01

Horse Serum Albumin crystals grown during the USML-1 (STS-50) mission's Protein Crystal Growth Glovebox Experiment. These crystals were grown using a vapor diffusion technique at 22 degrees C. The crystals were allowed to grow for nine days while in orbit. Crystals of 1.0 mm in length were produced. The most abundant blood serum protein, regulates blood pressure and transports ions, metabolites, and therapeutic drugs. Principal Investigator was Edward Meehan.

Crystal growth and crystallography

NASA Technical Reports Server (NTRS)

Chernov, A. A.

1998-01-01

Selected topics that may be of interest for both crystal-structure and crystal-growth communities are overviewed. The growth of protein crystals, along with that of some other compounds, is one of the topics, and recent insights into related phenomena are considered as examples of applications of general principles. The relationship between crystal growth shape and structure is reviewed and an attempt to introduce semiquantitative characterization of binding for proteins is made. The concept of kinks for complex structures is briefly discussed. Even at sufficiently low supersaturations, the fluctuation of steps may not be sufficient to implement the Gibbs-Thomson law if the kink density is low enough. Subsurface ordering of liquids and growth of rough interfaces from melts is discussed. Crystals growing in microgravity from solution should be more perfect if they preferentially trap stress-inducing impurities, thus creating an impurity-depleted zone around themselves. Evidently, such a zone is developed only around the crystals growing in the absence of convection. Under terrestrial conditions, the self-purified depleted zone is destroyed by convection, the crystal traps more impurity and grows stressed. The stress relief causes mosaicity. In systems containing stress-inducing but poorly trapped impurities, the crystals grown in the absence of convection should be worse than those of their terrestrial counterparts.

Protein crystal growth (5-IML-1)

NASA Technical Reports Server (NTRS)

Bugg, Charles E.

1992-01-01

Proteins (enzymes, hormones, immunoglobulins) account for 50 pct. or more of the dry weight of most living systems. A detailed understanding of the structural makeup of a protein is essential to any systematic research pertaining to it. Most macromolecules are extremely difficult to crystallize, and many otherwise exciting projects have terminated at the crystal growth stage. In principle, there are several aspects of microgravity that might be exploited to enhance protein crystal growth. The major factor is the elimination of density driven convective flow. Other factors that can be controlled in the absence of gravity is the sedimentation of growing crystals in a gravitational field, and the potential advantage of doing containerless crystal growth. As a result of these theories and facts, one can readily understand why the microgravity environment of an Earth orbiting vehicle seems to offer unique opportunities for the protein crystallographer. This perception has led to the establishment of the Protein Crystal Growth in a Microgravity Environment (PCG/ME) project. The results of experiments already performed during STS missions have in many cases resulted in large protein crystals which are structurally correct. Thus, the near term objective of the PCG/ME project is to continue to improve the techniques, procedures, and hardware systems used to grow protein crystals in Earth orbit.

Interface shape and crystallinity in LEC GaAs

NASA Astrophysics Data System (ADS)

Tower, J. P.; Tobin, R.; Pearah, P. J.; Ware, R. M.

1991-12-01

Growth striation mapping was used to relate the growth interface shape to crystallinity failure modes in LEC growth of undoped <100> GaAs. The onset of twinning and polycrystallinity were both found to depend on the interface shape near the crystal periphery. The origins of polycrystalline growth were investigated in 8 kg, 3-inch and 4-inch diameter crystals. Interface maps of these crystals show that polycrystalline growth begins when the growth interface periphery turns down, independent of the shape of the central portions. The cause of initial grain boundary formation was found to be included gallium droplets which originate on the surface and migrate through the crystal toward the growth interface. Twinning occurs on {111} facets, usually during shoulder growth. Growth striations show that the sequence of events leading to twin formation consists of deep facet growth, followed by meltback and rapid regrowth. We found it possible to avoid twinning by reducing melt instabilities or by reducing the extent of facet growth.

Modeling of Macroscopic/Microscopic Transport and Growth Phenomena in Zeolite Crystal Solutions Under Microgravity Conditions

NASA Technical Reports Server (NTRS)

Gatsonis, Nikos A.; Alexandrou, Andreas; Shi, Hui; Ongewe, Bernard; Sacco, Albert, Jr.

1999-01-01

Crystals grown from liquid solutions have important industrial applications. Zeolites, for instance, a class of crystalline aluminosilicate materials, form the backbone of the chemical process industry worldwide, as they are used as adsorbents and catalysts. Many of the phenomena associated with crystal growth processes are not well understood due to complex microscopic and macroscopic interactions. Microgravity could help elucidate these phenomena and allow the control of defect locations, concentration, as well as size of crystals. Microgravity in an orbiting spacecraft could help isolate the possible effects of natural convection (which affects defect formation) and minimize sedimentation. In addition, crystals will stay essentially suspended in the nutrient pool under a diffusion-limited growth condition. This is expected to promote larger crystals by allowing a longer residence time in a high-concentration nutrient field. Among other factors, the crystal size distribution depends on the nucleation rate and crystallization. These two are also related to the "gel" polymerization/depolymerization rate. Macroscopic bulk mass and flow transport and especially gravity, force the crystals down to the bottom of the reactor, thus forming a sedimentation layer. In this layer, the growth rate of the crystals slows down as crystals compete for a limited amount of nutrients. The macroscopic transport phenomena under certain conditions can, however, enhance the nutrient supply and therefore, accelerate crystal growth. Several zeolite experiments have been performed in space with mixed results. The results from our laboratory have indicated an enhancement in size of 30 to 70 percent compared to the best ground based controls, and a reduction of lattice defects in many of the space grown crystals. Such experiments are difficult to interpret, and cannot be easily used to derive empirical or other laws since many physical parameters are simultaneously involved in the process. At the same time, however, there is increased urgency to develop such an understanding in order to more accurately quantify the process. In order to better understand the results obtained from our prior space experiments, and design future experiments, a detailed fluid dynamic model simulating the crystal growth mechanism is required. This will not only add to the fundamental knowledge on the crystallization of zeolites, but also be useful in predicting the limits of size and growth of these important industrial materials. Our objective is to develop macro/microscopic theoretical and computational models to study the effect of transport phenomena in the growth of crystals grown in solutions. Our effort has concentrated so far in the development of separate macroscopic and microscopic models. The major highlights of our accomplishments are described.

Low-Temperature Growth of Two-Dimensional Layered Chalcogenide Crystals on Liquid.

PubMed

Zhou, Yubing; Deng, Bing; Zhou, Yu; Ren, Xibiao; Yin, Jianbo; Jin, Chuanhong; Liu, Zhongfan; Peng, Hailin

2016-03-09

The growth of high-quality two-dimensional (2D) layered chalcogenide crystals is highly important for practical applications in future electronics, optoelectronics, and photonics. Current route for the synthesis of 2D chalcogenide crystals by vapor deposition method mainly involves an energy intensive high-temperature growth process on solid substrates, often suffering from inhomogeneous nucleation density and grain size distribution. Here, we first demonstrate a facile vapor-phase synthesis of large-area high-quality 2D layered chalcogenide crystals on liquid metal surface with relatively low surface energy at a growth temperature as low as ∼100 °C. Uniform and large-domain-sized 2D crystals of GaSe and GaxIn1-xSe were grown on liquid metal surface even supported on a polyimide film. As-grown 2D GaSe crystals have been fabricated to flexible photodetectors, showing high photoresponse and excellent flexibility. Our strategy of energy-sustainable low-temperature growth on liquid metal surface may open a route to the synthesis of high-quality 2D crystals of Ga-, In-, Bi-, Hg-, Pb-, or Sn-based chalcogenides and halides.

Novel growth techniques of group-IV based semiconductors on insulator for next-generation electronics

NASA Astrophysics Data System (ADS)

Miyao, Masanobu; Sadoh, Taizoh

2017-05-01

Recent progress in the crystal growth of group-IV-based semiconductor-on-insulators is reviewed from physical and technological viewpoints. Liquid-phase growth based on SiGe-mixing-triggered rapid-melting growth enables formation of hybrid (100) (110) (111)-orientation Ge-on-insulator (GOI) structures, which show defect-free GOI with very high carrier mobility (˜1040 cm2 V-1 s-1). Additionally, SiGe mixed-crystals with laterally uniform composition were obtained by eliminating segregation phenomena during the melt-back process. Low-temperature solid-phase growth has been explored by combining this process with ion-beam irradiation, additional doping of group-IV elements, metal induced lateral crystallization with/without electric field, and metal-induced layer exchange crystallization. These efforts have enabled crystal growth on insulators below 400 °C, achieving high carrier mobility (160-320 cm2 V-1 s-1). Moreover, orientation-controlled SiGe and Ge films on insulators have been obtained below the softening temperatures of conventional plastic films (˜300 °C). Detailed characterization provides an understanding of physical phenomena behind these crystal growth techniques. Applying these methods when fabricating next-generation electronics is also discussed.

Formation of nanotwin networks during high-temperature crystallization of amorphous germanium

DOE PAGES

Sandoval, Luis; Reina, Celia; Marian, Jaime

2015-11-26

Germanium is an extremely important material used for numerous functional applications in many fields of nanotechnology. In this paper, we study the crystallization of amorphous Ge using atomistic simulations of critical nano-metric nuclei at high temperatures. We find that crystallization occurs by the recurrent transfer of atoms via a diffusive process from the amorphous phase into suitably-oriented crystalline layers. We accompany our simulations with a comprehensive thermodynamic and kinetic analysis of the growth process, which explains the energy balance and the interfacial growth velocities governing grain growth. For the <111> crystallographic orientation, we find a degenerate atomic rearrangement process, withmore » two zero-energy modes corresponding to a perfect crystalline structure and the formation of a Σ3 twin boundary. Continued growth in this direction results in the development a twin network, in contrast with all other growth orientations, where the crystal grows defect-free. This particular mechanism of crystallization from amorphous phases is also observed during solid-phase epitaxial growth of <111> semiconductor crystals, where growth is restrained to one dimension. Lastly, we calculate the equivalent X-ray diffraction pattern of the obtained nanotwin networks, providing grounds for experimental validation.« less

Formation of Nanotwin Networks during High-Temperature Crystallization of Amorphous Germanium

PubMed Central

Sandoval, Luis; Reina, Celia; Marian, Jaime

2015-01-01

Germanium is an extremely important material used for numerous functional applications in many fields of nanotechnology. In this paper, we study the crystallization of amorphous Ge using atomistic simulations of critical nano-metric nuclei at high temperatures. We find that crystallization occurs by the recurrent transfer of atoms via a diffusive process from the amorphous phase into suitably-oriented crystalline layers. We accompany our simulations with a comprehensive thermodynamic and kinetic analysis of the growth process, which explains the energy balance and the interfacial growth velocities governing grain growth. For the 〈111〉 crystallographic orientation, we find a degenerate atomic rearrangement process, with two zero-energy modes corresponding to a perfect crystalline structure and the formation of a Σ3 twin boundary. Continued growth in this direction results in the development a twin network, in contrast with all other growth orientations, where the crystal grows defect-free. This particular mechanism of crystallization from amorphous phases is also observed during solid-phase epitaxial growth of 〈111〉 semiconductor crystals, where growth is restrained to one dimension. We calculate the equivalent X-ray diffraction pattern of the obtained nanotwin networks, providing grounds for experimental validation. PMID:26607496

The release of trapped gases from amorphous solid water films. I. "Top-down" crystallization-induced crack propagation probed using the molecular volcano.

PubMed

May, R Alan; Smith, R Scott; Kay, Bruce D

2013-03-14

In this (Paper I) and the companion paper (Paper II; R. May, R. Smith, and B. Kay, J. Chem. Phys. 138, 104502 (2013)), we investigate the mechanisms for the release of trapped gases from underneath amorphous solid water (ASW) films. In prior work, we reported the episodic release of trapped gases in concert with the crystallization of ASW, a phenomenon that we termed the "molecular volcano." The observed abrupt desorption is due to the formation of cracks that span the film to form a connected pathway for release. In this paper, we utilize the "molecular volcano" desorption peak to characterize the formation of crystallization-induced cracks. We find that the crack length distribution is independent of the trapped gas (Ar, Kr, Xe, CH4, N2, O2, or CO). Selective placement of the inert gas layer is used to show that cracks form near the top of the film and propagate downward into the film. Isothermal experiments reveal that, after some induction time, cracks propagate linearly in time with an Arrhenius dependent velocity corresponding to an activation energy of 54 kJ∕mol. This value is consistent with the crystallization growth rates reported by others and establishes a direct connection between crystallization growth rate and the crack propagation rate. A two-step model in which nucleation and crystallization occurs in an induction zone near the top of the film followed by the propagation of a crystallization∕crack front into the film is in good agreement with the temperature programmed desorption results.

ICCG-10: Tenth International Conference on Crystal Growth. Poster presentation abstracts

NASA Technical Reports Server (NTRS)

1992-01-01

Poster presentation abstracts from the tenth International Conference on Crystal Growth (ICCG) (Aug. 16-21, 1992) are provided. Topics discussed at the conference include crystal growth mechanisms, superconductors, semiconductors, laser materials, optical materials, and biomaterials. Organizing committees, ICCG advisory board and officers, and sponsors of the conference are also included.

DHS Internship Summary-Crystal Assembly at Different Length Scales

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mishchenko, L

2009-08-06

I was part of a project in which in situ atomic force microscopy (AFM) was used to monitor growth and dissolution of atomic and colloidal crystals. At both length scales, the chemical environment of the system greatly altered crystal growth and dissolution. Calcium phosphate was used as a model system for atomic crystals. A dissolution-reprecipitation reaction was observed in this first system, involving the conversion of brushite (DCPD) to octacalcium phosphate (OCP). In the second system, polymeric colloidal crystals were dissolved in an ionic solvent, revealing the underlying structure of the crystal. The dissolved crystal was then regrown through anmore » evaporative step method. Recently, we have also found that colloids can be reversibly deposited in situ onto an ITO (indium tin oxide) substrate via an electrochemistry setup. The overall goal of this project was to develop an understanding of the mechanisms that control crystallization and order, so that these might be controlled during material synthesis. Controlled assembly of materials over a range of length scales from molecules to nanoparticles to colloids is critical for designing new materials. In particular, developing materials for sensor applications with tailorable properties and long range order is important. In this work, we examine two of these length scales: small molecule crystallization of calcium phosphate (whose crystal phases include DCPD, OCP, and HAP) and colloidal crystallization of Poly(methyl methacrylate) beads. Atomic Force Microscopy is ideal for this line of work because it allows for the possibility of observing non-conducting samples in fluid during growth with high resolution ({approx} 10 nm). In fact, during atomic crystal growth one can observe changes in atomic steps, and with colloidal crystals, one can monitor the individual building blocks of the crystal. Colloids and atoms crystallize under the influence of different forces acting at different length scales as seen in Table 1. In particular, molecular crystals, which are typically dominated by ionic and covalent bonding, are an order of magnitude more strongly bonded than colloidal crystals. In molecular crystals, ordering is driven by the interaction potentials between molecules. By contrast, colloidal assembly is a competition between the repulsive electrostatic forces that prevent aggregation in solution (due to surface charge), and short-range van der Waals and entropic forces that leads to ordering. Understanding atomic crystallization is fundamentally important for fabrication of tailorable crystalline materials, for example for biological or chemical sensors. The transformation of brushite to OCP not only serves as a model system for atomic crystal growth (applicable to many other crystal growth processes), but is also important in bone cements. Colloidal crystals have unique optical properties which respond to chemical and mechanical stimuli, making them very important for sensing applications. The mechanism of colloidal crystal assembly is thus fundamentally important. Our in situ dissolution and regrowth experiments are one good method of analyzing how these crystals pack under different conditions and how defect sites are formed and filled. In these experiments, a silica additive was used to strengthen the colloidal crystal during initial assembly (ex situ) and to increase domain size and long range order. Reversible electrodeposition of colloids onto a conductive substrate (ITO in our case) is another system which can further our knowledge of colloidal assembly. This experiment holds promise of allowing in situ observation of colloidal crystal growth and the influence of certain additives on crystal order. The ultimate goal would be to achieve long range order in these crystals by changing the surface charge or the growth environment.« less

Deducing growth mechanisms for minerals from the shapes of crystal size distributions

USGS Publications Warehouse

Eberl, D.D.; Drits, V.A.; Srodon, J.

1998-01-01

Crystal size distributions (CSDs) of natural and synthetic samples are observed to have several distinct and different shapes. We have simulated these CSDs using three simple equations: the Law of Proportionate Effect (LPE), a mass balance equation, and equations for Ostwald ripening. The following crystal growth mechanisms are simulated using these equations and their modifications: (1) continuous nucleation and growth in an open system, during which crystals nucleate at either a constant, decaying, or accelerating nucleation rate, and then grow according to the LPE; (2) surface-controlled growth in an open system, during which crystals grow with an essentially unlimited supply of nutrients according to the LPE; (3) supply-controlled growth in an open system, during which crystals grow with a specified, limited supply of nutrients according to the LPE; (4) supply- or surface-controlled Ostwald ripening in a closed system, during which the relative rate of crystal dissolution and growth is controlled by differences in specific surface area and by diffusion rate; and (5) supply-controlled random ripening in a closed system, during which the rate of crystal dissolution and growth is random with respect to specific surface area. Each of these mechanisms affects the shapes of CSDs. For example, mechanism (1) above with a constant nucleation rate yields asymptotically-shaped CSDs for which the variance of the natural logarithms of the crystal sizes (??2) increases exponentially with the mean of the natural logarithms of the sizes (??). Mechanism (2) yields lognormally-shaped CSDs, for which ??2 increases linearly with ??, whereas mechanisms (3) and (5) do not change the shapes of CSDs, with ??2 remaining constant with increasing ??. During supply-controlled Ostwald ripening (4), initial lognormally-shaped CSDs become more symmetric, with ??2 decreasing with increasing ??. Thus, crystal growth mechanisms often can be deduced by noting trends in ?? versus ??2 of CSDs for a series of related samples.

Study on growth techniques and macro defects of large-size Nd:YAG laser crystal

NASA Astrophysics Data System (ADS)

Quan, Jiliang; Yang, Xin; Yang, Mingming; Ma, Decai; Huang, Jinqiang; Zhu, Yunzhong; Wang, Biao

2018-02-01

Large-size neodymium-doped yttrium aluminum garnet (Nd:YAG) single crystals were grown by the Czochralski method. The extinction ratio and wavefront distortion of the crystal were tested to determine the optical homogeneity. Moreover, under different growth conditions, the macro defects of inclusion, striations, and cracking in the as-grown Nd:YAG crystals were analyzed. Specifically, the inclusion defects were characterized using scanning electron microscopy and energy dispersive spectroscopy. The stresses of growth striations and cracking were studied via a parallel plane polariscope. These results demonstrate that improper growth parameters and temperature fields can enhance defects significantly. Thus, by adjusting the growth parameters and optimizing the thermal environment, high-optical-quality Nd:YAG crystals with a diameter of 80 mm and a total length of 400 mm have been obtained successfully.

Nonclassical crystallization in vivo et in vitro (II): Nanogranular features in biomimetic minerals disclose a general colloid-mediated crystal growth mechanism.

PubMed

Rodríguez-Navarro, Carlos; Ruiz-Agudo, Encarnación; Harris, Joe; Wolf, Stephan E

2016-11-01

Recent research has shown that biominerals and their biomimetics (i) typically form via an amorphous precursor phase, and (ii) commonly display a nanogranular texture. Apparently, these two key features are closely related, underlining the fact that the formation of biominerals and their biomimetics does not necessarily follow classical crystallization routes, and leaves a characteristic nanotextural imprint which may help to disclose their origins and formation mechanisms. Here we present a general overview of the current theories and models of nonclassical crystallization and their applicability for the advance of our current understanding of biomineralization and biomimetic mineralization. We pay particular attention to the link between nonclassical crystallization routes and the resulting nanogranular textures of biomimetic CaCO 3 mineral structures. After a general introductory section, we present an overview of classical nucleation and crystal growth theories and their limitations. Then, we introduce the Ostwald's step rule as a general framework to explain nonclassical crystallization. Subsequently, we describe nonclassical crystallization routes involving stable prenucleation clusters, dense liquid and solid amorphous precursor phases, as well as current nonclassical crystal growth models. The latter include oriented attachment, mesocrystallization and the new model based on the colloidal growth of crystals via attachment of amorphous nanoparticles. Biomimetic examples of nanostructured CaCO 3 minerals formed via these nonclassical routes are presented which help us to show that colloid-mediated crystal growth can be regarded as a wide-spread growth mechanism. Implications of these observations for the advance in the current understanding on the formation of biomimetic materials and biominerals are finally outlined. Copyright © 2016 Elsevier Inc. All rights reserved.

Lab-on-a-Chip Based Protein Crystallization

NASA Technical Reports Server (NTRS)

vanderWoerd, Mark J.; Brasseur, Michael M.; Spearing, Scott F.; Whitaker, Ann F. (Technical Monitor)

2001-01-01

We are developing a novel technique with which we will grow protein crystals in very small volumes, utilizing chip-based, microfluidic ("LabChip") technology. This development, which is a collaborative effort between NASA's Marshall Space Flight Center and Caliper Technologies Corporation, promises a breakthrough in the field of protein crystal growth. Our initial results obtained from two model proteins, Lysozyme and Thaumatin, show that it is feasible to dispense and adequately mix protein and precipitant solutions on a nano-liter scale. The mixtures have shown crystal growth in volumes in the range of 10 nanoliters to 5 microliters. In addition, large diffraction quality crystals were obtained by this method. X-ray data from these crystals were shown to be of excellent quality. Our future efforts will include the further development of protein crystal growth with LabChip(trademark) technology for more complex systems. We will initially address the batch growth method, followed by the vapor diffusion method and the liquid-liquid diffusion method. The culmination of these chip developments is to lead to an on orbit protein crystallization facility on the International Space Station. Structural biologists will be invited to utilize the on orbit Iterative Biological Crystallization facility to grow high quality macromolecular crystals in microgravity.

Dynamically controlled crystal growth system

NASA Technical Reports Server (NTRS)

Bray, Terry L. (Inventor); Kim, Larry J. (Inventor); Harrington, Michael (Inventor); DeLucas, Lawrence J. (Inventor)

2002-01-01

Crystal growth can be initiated and controlled by dynamically controlled vapor diffusion or temperature change. In one aspect, the present invention uses a precisely controlled vapor diffusion approach to monitor and control protein crystal growth. The system utilizes a humidity sensor and various interfaces under computer control to effect virtually any evaporation rate from a number of different growth solutions simultaneously by means of an evaporative gas flow. A static laser light scattering sensor can be used to detect aggregation events and trigger a change in the evaporation rate for a growth solution. A control/follower configuration can be used to actively monitor one chamber and accurately control replicate chambers relative to the control chamber. In a second aspect, the invention exploits the varying solubility of proteins versus temperature to control the growth of protein crystals. This system contains miniature thermoelectric devices under microcomputer control that change temperature as needed to grow crystals of a given protein. Complex temperature ramps are possible using this approach. A static laser light scattering probe also can be used in this system as a non-invasive probe for detection of aggregation events. The automated dynamic control system provides systematic and predictable responses with regard to crystal size. These systems can be used for microgravity crystallization projects, for example in a space shuttle, and for crystallization work under terrestial conditions. The present invention is particularly useful for macromolecular crystallization, e.g. for proteins, polypeptides, nucleic acids, viruses and virus particles.

Bibliography of the space processing program. Volume 1: A compilation through June 1974, Parts 1 and 2. [space manufacturing/spacecraft construction materials - aerospace environments

NASA Technical Reports Server (NTRS)

Shoultz, M. B.; Mcclurken, E. W., Jr.

1975-01-01

A compilation of NASA research efforts in the area of space environmental effects on materials and processes is presented. Topics considered are: (1) fluid mechanics and heat transfer; (2) crystal growth and containerless melts; (3) acoustics; (4) glass and ceramics; (5) electrophoresis; (6) welding; and (7) exobiology.

SM50 Repeat-Polypeptides Self-Assemble into Discrete Matrix Subunits and Promote Appositional Calcium Carbonate Crystal Growth during Sea Urchin Tooth Biomineralization

PubMed Central

Mao, Yelin; Satchell, Paul G.; Luan, Xianghong; Diekwisch, Thomas G.H.

2015-01-01

The two major proteins involved in vertebrate enamel formation and echinoderm sea urchin tooth biomineralization, amelogenin and SM50, are both characterized by elongated polyproline repeat domains in the center of the macromolecule. To determine the role of polyproline repeat polypeptides in basal deuterostome biomineralization, we have mapped the localization of SM50 as it relates to crystal growth, conducted self-assembly studies of SM50 repeat polypeptides, and examined their effect on calcium carbonate and apatite crystal growth. Electron micrographs of the growth zone of Strongylocentrotus purpuratus sea urchin teeth documented a series of successive events from intravesicular mineral nucleation to mineral deposition at the interface between tooth surface and odontoblast syncytium. Using immunohistochemistry, SM50 was detected within the cytoplasm of cells associated with the developing tooth mineral, at the mineral secreting front, and adjacent to initial mineral deposits, but not in muscles and ligaments. Polypeptides derived from the SM50 polyproline alternating hexa- and hepta-peptide repeat region (SM50P6P7) formed highly discrete, donut-shaped self-assembly patterns. In calcium carbonate crystal growth studies, SM50P6P7 repeat peptides triggered the growth of expansive networks of fused calcium carbonate crystals while in apatite growth studies, SM50P6P7 peptides facilitated the growth of needle-shaped and parallel arranged crystals resembling those found in developing vertebrate enamel. In comparison, SM50P6P7 surpassed the PXX24 polypeptide repeat region derived from the vertebrate enamel protein amelogenin in its ability to promote crystal nucleation and appositional crystal growth. Together, these studies establish the SM50P6P7 polyproline repeat region as a potent regulator in the protein-guided appositional crystal growth that occurs during continuous tooth mineralization and eruption. In addition, our studies highlight the role of species-specific polyproline repeat motifs in the formation of discrete self-assembled matrices and the resulting control of mineral growth. PMID:26194158

SM50 repeat-polypeptides self-assemble into discrete matrix subunits and promote appositional calcium carbonate crystal growth during sea urchin tooth biomineralization.

PubMed

Mao, Yelin; Satchell, Paul G; Luan, Xianghong; Diekwisch, Thomas G H

2016-01-01

The two major proteins involved in vertebrate enamel formation and echinoderm sea urchin tooth biomineralization, amelogenin and SM50, are both characterized by elongated polyproline repeat domains in the center of the macromolecule. To determine the role of polyproline repeat polypeptides in basal deuterostome biomineralization, we have mapped the localization of SM50 as it relates to crystal growth, conducted self-assembly studies of SM50 repeat polypeptides, and examined their effect on calcium carbonate and apatite crystal growth. Electron micrographs of the growth zone of Strongylocentrotus purpuratus sea urchin teeth documented a series of successive events from intravesicular mineral nucleation to mineral deposition at the interface between tooth surface and odontoblast syncytium. Using immunohistochemistry, SM50 was detected within the cytoplasm of cells associated with the developing tooth mineral, at the mineral secreting front, and adjacent to initial mineral deposits, but not in muscles and ligaments. Polypeptides derived from the SM50 polyproline alternating hexa- and hepta-peptide repeat region (SM50P6P7) formed highly discrete, donut-shaped self-assembly patterns. In calcium carbonate crystal growth studies, SM50P6P7 repeat peptides triggered the growth of expansive networks of fused calcium carbonate crystals while in apatite growth studies, SM50P6P7 peptides facilitated the growth of needle-shaped and parallel arranged crystals resembling those found in developing vertebrate enamel. In comparison, SM50P6P7 surpassed the PXX24 polypeptide repeat region derived from the vertebrate enamel protein amelogenin in its ability to promote crystal nucleation and appositional crystal growth. Together, these studies establish the SM50P6P7 polyproline repeat region as a potent regulator in the protein-guided appositional crystal growth that occurs during continuous tooth mineralization and eruption. In addition, our studies highlight the role of species-specific polyproline repeat motifs in the formation of discrete self-assembled matrices and the resulting control of mineral growth. Copyright © 2015 Elsevier GmbH. All rights reserved.

Direct flow crystal growth system

DOEpatents

Montgomery, Kenneth E.; Milanovich, Fred P.

1992-01-01

A crystal is grown in a constantly filtered solution which is flowed directly into the growing face of a crystal. In a continuous flow system, solution at its saturation temperature is removed from a crystal growth tank, heated above its saturation temperature, filtered, cooled back to its saturation temperature, and returned to the tank.

Molecular insights into the heterogeneous crystal growth of si methane hydrate.

PubMed

Vatamanu, Jenel; Kusalik, Peter G

2006-08-17

In this paper we report a successful molecular simulation study exploring the heterogeneous crystal growth of sI methane hydrate along its [001] crystallographic face. The molecular modeling of the crystal growth of methane hydrate has proven in the past to be very challenging, and a reasonable framework to overcome the difficulties related to the simulation of such systems is presented. Both the microscopic mechanisms of heterogeneous crystal growth as well as interfacial properties of methane hydrate are probed. In the presence of the appropriate crystal template, a strong tendency for water molecules to organize into cages around methane at the growing interface is observed; the interface also demonstrates a strong affinity for methane molecules. The maximum growth rate measured for a hydrate crystal is about 4 times higher than the value previously determined for ice I in a similar framework (Gulam Razul, M. S.; Hendry, J. G.; Kusalik, P. G. J. Chem. Phys. 2005, 123, 204722).

Tetragonal Lysozyme Nucleation and Crystal Growth: The Role of the Solution Phase

NASA Technical Reports Server (NTRS)

Pusey, Marc L.; Forsythe, Elizabeth; Sumida, John; Maxwell, Daniel; Gorti, Sridhar

2002-01-01

Lysozyme, and most particularly the tetragonal form of the protein, has become the default standard protein for use in macromolecule crystal nucleation and growth studies. There is a substantial body of experimental evidence, from this and other laboratories, that strongly suggests this proteins crystal nucleation and growth is by addition of associated species that are preformed by standard reversible concentration-driven self association processes in the bulk solution. The evidence includes high resolution AFM studies of the surface packing and of growth unit size at incorporation, fluorescence resonance energy transfer measurements of intermolecular distances in dilute solution, dialysis kinetics, and modeling of the growth rate data. We have developed a selfassociation model for the proteins crystal nucleation and growth. The model accounts for the obtained crystal symmetry, explains the observed surface structures, and shows the importance of the symmetry obtained by self-association in solution to the process as a whole. Further, it indicates that nucleation and crystal growth are not distinct mechanistically, but identical, with the primary difference being the probability that the particle will continue to grow or dissolve. This model also offers a possible mechanism for fluid flow effects on the growth process and how microgravity may affect it. While a single lysozyme molecule is relatively small (M.W. = 14,400), a structured octamer in the 4(sub 3) helix configuration (the proposed average sized growth unit) would have a M.W. = 115,000 and dimensions of 5.6 x 5.6 x 7.6 nm. Direct AFM measurements of growth unit incorporation indicate that units as wide as 11.2 nm and as long as 11.4 nm commonly attach to the crystal. These measurements were made at approximately saturation conditions, and they reflect the sizes of species that both added or desorbed from the crystal surface. The larger and less isotropic the associated species the more likely that it will be oriented to some degree in a flowing boundary layer, even at the low flow velocities measured about macromolecule crystals. Flow-driven effects resulting in misorientation upon addition to and incorporation into the crystal need only be a small fraction of a percentage to significantly affect the resulting crystal. One Earth, concentration gradient driven flow will maintain a high interfacial concentration, i.e., a high level (essentially that of the bulk solution) of solute association at the interface and higher growth rate. Higher growth rates mean an increased probability that misaligned growth units are trapped by subsequent growth layers before they can be desorbed and try again, or that the desorbing species will be smaller than the adsorbing species. In microgravity the extended diffusive boundary layer will lower the interfacial concentration. This results in a net dissociation of aggregated species that diffuse in from the bulk solution, i.e., smaller associated species, which are more likely able to make multiple attempts to correctly bind, yielding higher quality crystals.

Study of single crystals of metal solid solutions

NASA Technical Reports Server (NTRS)

Doty, J. P.; Reising, J. A.

1973-01-01

The growth of single crystals of relatively high melting point metals such as silver, copper, gold, and their alloys was investigated. The purpose was to develop background information necessary to support a space flight experiment and to generate ground based data for comparison. The ground based data, when compared to the data from space grown crystals, are intended to identify any effects which zero-gravity might have on the basic process of single crystal growth of these metals. The ultimate purposes of the complete investigation are to: (1) determine specific metals and alloys to be investigated; (2) grow single metal crystals in a terrestrial laboratory; (3) determine crystal characteristics, properties, and growth parameters that will be effected by zero-gravity; (4) evaluate terrestrially grown crystals; (5) grow single metal crystals in a space laboratory such as Skylab; (6) evaluate the space grown crystals; (7) compare for zero-gravity effects of crystal characteristics, properties, and parameters; and (8) make a recommendation as to production of these crystals as a routine space manufacturing proceses.

Crystal growth, spectral, structural and optical studies of π-conjugated stilbazolium crystal: 4-bromobenzaldehyde-4'-N'-methylstilbazolium tosylate.

PubMed

Krishna Kumar, M; Sudhahar, S; Bhagavannarayana, G; Mohan Kumar, R

2014-05-05

Nonlinear optical (NLO) organic compound, 4-bromobenzaldehyde-4'-N'-methylstilbazolium tosylate was synthesized by reflux method. The formation of molecular complex was confirmed from (1)H NMR, FT-IR and FT-Raman spectral analyses. The single crystals were grown by slow evaporation solution growth method and the crystal structure and atomic packing of grown crystal was identified. The morphology and growth axis of grown crystal were determined. The crystal perfection was analyzed using high resolution X-ray diffraction study on (001) plane. Thermal stability, decomposition stages and melting point of the grown crystal were analyzed. The optical absorption coefficient (α) and energy band gap (E(g)) of the crystal were determined using UV-visible absorption studies. Second harmonic generation efficiency of the grown crystal was examined by Kurtz powder method with different particle size using 1064 nm laser. Laser induced damage threshold study was carried out for the grown crystal using Nd:YAG laser. Copyright © 2014 Elsevier B.V. All rights reserved.

Microgravity crystal growth

NASA Technical Reports Server (NTRS)

2001-01-01

Advanced finite element models are used to study three-dimensional, time-dependent flow and segregation in crystal growth systems. In this image of a prototypical model for melt and crystal growth, pathlines at one instant in time are shown for the flow of heated liquid silicon in a cylindrical container. The container is subjected to g-jitter disturbances along the vertical axis. A transverse magnetic field is applied to control them. Such computations are extremely powerful for understanding melt growth in microgravity where g-jitter drives buoyant flows. The simulation is part of the Theoretical Analysis of 3D, Transient Convection and Segregation in Microgravity Bridgman Crystal Growth investigation by Dr. Jeffrey J. Derby of the University of Mirnesota, Minneapolis.

Critical Supersaturation for Ice Crystal Growth: Laboratory Measurements and Atmospheric Modeling Implications

NASA Astrophysics Data System (ADS)

Magee, N.; Moyle, A.; Lamb, D.

2003-12-01

An improved understanding of ice crystal growth, particularly at low temperatures, is much in demand for the advancement of numerical modeling of atmospheric processes. Cirrus models must contend with the complexity of ice crystals growing in cold temperatures, low pressures, low supersaturations, and with multiple nucleation mechanisms. Recent observations have allowed increasingly realistic parameterizations of cirrus ice crystal microphysics, but these observations need to be supplemented by a fundamental understanding of growth processes affecting low-temperature crystals. Several experimental studies have demonstrated that certain ice crystals require a minimum "critical" supersaturation before exhibiting detectable growth. These crystals are presumed to be essentially defect-free, preventing vicinal hillock growth at the site of crystal dislocations. In the case of crystal growth by spiral dislocation, advancement of faces begins as soon as supersaturation is present. The finding of conditional critical supersaturations have analogies in other materials (metals, semiconductors, potassium dihydrogen phosphate) and are thermodynamically predicted given a two-dimensional nucleation growth mechanism. Previous measurements have determined the critical supersaturation for ice as a function of temperature and crystallographic face from 0 to --15° C with extrapolation to --30° C. For both basal and prism faces, critical supersaturation is seen to increase with decreasing temperature, suggesting that low-temperature, low-supersaturation processes are most likely to be affected by this critical contingency. We present laboratory results to verify and extend prior critical supersaturation measurements using a novel approach for supersaturation generation, control, and measurement. The crystals are grown on the tip of a fine glass fiber ( ˜10 microns in diameter) under varying conditions of temperature, pressure, and saturation. Supersaturation is generated when a pre-saturated airflow passes over a coil of ice warmed by electrical resistance upstream from the growing crystal. Supersaturation is determined by a system of differential thermocouples calibrated to sulfuric acid drop size measurements. Measurements follow those made in earlier studies, but also extend to temperatures of --45° C, mimicking conditions found in some high altitude clouds.

Experimental determination of growth rate effect on U 6+ and Mg 2+ partitioning between aragonite and fluid at elevated U 6+ concentration

NASA Astrophysics Data System (ADS)

Gabitov, R. I.; Gaetani, G. A.; Watson, E. B.; Cohen, A. L.; Ehrlich, H. L.

2008-08-01

Results are reported from an experimental study in which the partitioning of U and Mg between aragonite and an aqueous solution were determined as a function of crystal growth rate. Crystals, identified as aragonite by X-ray diffractometry and micro-Raman spectroscopy, were grown by diffusion of CO 2 from an ammonium carbonate source into a calcium-bearing solution at temperatures of 22 and 53 °C. Hemispherical bundles (spherulites) of aragonite crystals were produced, the growth rates of which decreased monotonically from the spherulite interiors to the edges and thus provide the opportunity to examine the influence of growth rate on crystal composition. Element concentration ratios were measured using electron microprobe (EMP) and fluid composition was determined by inductively coupled plasma-mass spectrometry (ICP-MS) and atomic absorption (AA). Growth rates were determined directly by addition of a Dy spike to the fluid during the experiment that was subsequently located in an experimentally precipitated spherulite using secondary ion mass spectrometry (SIMS). At 22 °C both U/Ca and Mg/Ca partition coefficients exhibited a strong growth rate dependence when crystal growth rates were low, and became independent of growth rate when crystal growth rates were high. The U/Ca ratios in aragonite increase between 22 and 53 °C; in contrast Mg/Ca ratios show inverse dependence on temperature.

Modeling Tetragonal Lysozyme Crystal Growth Rates

NASA Technical Reports Server (NTRS)

Gorti, Sridhar; Forsythe, Elizabeth L.; Pusey, Marc L.

2003-01-01

Tetragonal lysozyme 110 face crystal growth rates, measured over 5 orders of magnitude in range, can be described using a model where growth occurs by 2D nucleation on the crystal surface for solution supersaturations of c/c(sub eq) less than or equal to 7 +/- 2. Based upon the model, the step energy per unit length, beta was estimated to be approx. 5.3 +/- 0.4 x 10(exp -7) erg/mol-cm, which for a step height of 56 A corresponds to barrier of approx. 7 +/- 1 k(sub B)T at 300 K. For supersaturations of c/c(sub eq) > 8, the model emphasizing crystal growth by 2D nucleation not only could not predict, but also consistently overestimated, the highest observable crystal growth rates. Kinetic roughening is hypothesized to occur at a cross-over supersaturation of c/c(sub eq) > 8, where crystal growth is postulated to occur by a different process such as adsorption. Under this assumption, all growth rate data indicated that a kinetic roughening transition and subsequent crystal growth by adsorption for all solution conditions, varying in buffer pH, temperature and precipitant concentration, occurs for c/c(sub eq)(T, pH, NaCl) in the range between 5 and 10, with an energy barrier for adsorption estimated to be approx. 20 k(sub B)T at 300 K. Based upon these and other estimates, we determined the size of the critical surface nucleate, at the crossover supersaturation and higher concentrations, to range from 4 to 10 molecules.

Growth mechanism changes in pseudo-dewetted monolayer poly(ethylene oxide) crystallization

NASA Astrophysics Data System (ADS)

Zhu, Dun-Shen; Chen, Er-Qiang; Shi, An-Chang; Cheng, Stephen

2006-03-01

Crystal growth mechanism changes have been observed in pseudo-dewetted monolayers of low molecular weight (LMW) (PEO) on freshly cleaved hydrophilic mica surfaces [HPEO(4250) which have -OH groups at both ends and MHPEO(4700) which has one -OH and one -OCH3 as end groups]. X-ray scattering reflectivity measurements show a wetted monolayer of molten PEO with a thickness of ˜ 4.5 nm on the mica surface. Non-adsorbed PEO droplets sit on top of the wetted monolayer. A two-step process for PEO single crystal growth under isothermal conditions was identified utilizing in-situ atomic force microscopy at different crystallization temperatures (Tx). In the first step, the crystal grows within the droplet which supplies the molten PEO that participates in the crystal formation. In this second-step, the wetted monolayer at the growth front is depleted by about 1.5 - 2.5 nm. The growing crystal lateral sizes obey a power law of t^α (t: time). At a high Tx of 63 C for MHPEO(4700), the growth behavior obeys r t (α = 1). While in the case of HPEO(4250), its growth behavior follows r t^0.5 (α = 0.5) in the whole Tx range. With decreasing Tx, the growth of MHPEO(4700) falls into a scaling law of r t^α (0.5 < α < 1).

Crystal Growth of ZnSe and Related Ternary Compound Semiconductors by Vapor Transport

NASA Technical Reports Server (NTRS)

2003-01-01

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 buoyancy-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. Significant effects of gravity vector orientation on the growth crystal morphology and point defect distribution were observed.

Development of a model for on-line control of crystal growth by the AHP method

NASA Astrophysics Data System (ADS)

Gonik, M. A.; Lomokhova, A. V.; Gonik, M. M.; Kuliev, A. T.; Smirnov, A. D.

2007-05-01

The possibility to apply a simplified 2D model for heat transfer calculations in crystal growth by the axial heat close to phase interface (AHP) method is discussed in this paper. A comparison with global heat transfer calculations with the CGSim software was performed to confirm the accuracy of this model. The simplified model was shown to provide adequate results for the shape of the melt-crystal interface and temperature field in an opaque (Ge) and a transparent crystal (CsI:Tl). The model proposed is used for identification of the growth setup as a control object, for synthesis of a digital controller (PID controller at the present stage) and, finally, in on-line simulations of crystal growth control.

Morphology design of porous coordination polymer crystals by coordination modulation.

PubMed

Umemura, Ayako; Diring, Stéphane; Furukawa, Shuhei; Uehara, Hiromitsu; Tsuruoka, Takaaki; Kitagawa, Susumu

2011-10-05

The design of crystal morphology, or exposed crystal facets, has enabled the development (e.g., catalytic activities, material attributes, and oriented film formation) of porous coordination polymers (PCPs) without changing material compositions. However, because crystal growth mechanisms are not fully understood, control of crystal morphology still remains challenging. Herein, we report the morphology design of [Cu(3)(btc)(2)](n) (btc = benzene-1,3,5-tricarboxylate) by the coordination modulation method (modulator = n-dodecanoic acid or lauric acid). A morphological transition (octahedron-cuboctahedron-cube) in the [Cu(3)(btc)(2)](n) crystal was observed with an increase in concentration of the modulator. By suitably defining a coarse-grained standard unit of [Cu(3)(btc)(2)](n) as its cuboctahedron main pore and determining its attachment energy on crystal surfaces, Monte Carlo coarse-grain modeling revealed the population and orientation of carboxylates and elucidated an important role of the modulator in determining the <100>- and <111>-growth throughout the crystal growth process. This comprehension, in fact, successfully led to designed crystal morphologies with oriented growth on bare substrates. Because selective crystal orientations on the bare substrates were governed by crystal morphology, this contribution also casts a new light on the unexplored issue of the significance of morphology design of PCPs.

Analytical studies on the crystal melt interface shape in the Czochralski process for oxide single crystals

NASA Astrophysics Data System (ADS)

Jeong, Ja Hoon; Kang, In Seok

2000-09-01

Effects of the operating conditions on the crystal-melt interface shape are analytically investigated for the Czochralski process of the oxide single crystals. The ideas, which were used for the silicon single-crystal growth by Jeong et al. (J. Crystal Growth 177 (1997) 157), are extended to the oxide single-crystal growth problem by considering the internal radiation in the crystal phase and the melt phase heat transfer with the high Prandtl number. The interface shape is approximated in the simplest form as a quadratic function of radial position and an expression for the deviation from the flat interface shape is derived as a function of operating conditions. The radiative heat transfer rate between the interface and the ambient is computed by calculating the view factors for the curved interface shape with the assumption that the crystal phase is completely transparent. For the melt phase, the well-known results from the thermal boundary layer analysis are applied for the asymptotic case of high Prandtl number based on the idea that the flow field near the crystal-melt interface can be modeled as either a uniaxial or a biaxial flow. Through this work, essential information on the interface shape deformation and the effects of operating conditions are brought out for the oxide single-crystal growth.

The Growth and Characterization of the Bismuth Strontium-Calcium 2212 Superconductor

NASA Astrophysics Data System (ADS)

Moulton, Linda Vidale

A miniaturized float zone technique, sometimes referred to as the Laser-heated Pedestal Growth (LHPG) method, was used to produce high quality crystals of the incongruently melting rm Bi_2Sr_2CaCu _2O_{8+delta} (2212) superconductor. The main focus of this research was to (1) produce superconducting samples having different compositions, (2) identify the melt compositions and growth temperatures which produced these samples, and (3) determine the variation of their superconducting transition temperature (T _{rm C}) with composition and processing conditions. The rm Bi_2(Sr,Ca) _3Cu_2O_{8+delta} crystallization experiments were supplemented by a series of similar experiments on the incongruently melting compound rm Ca_3Al_2O_6. The phase equilibria in the CaO-rm Al_2O _3 system has been thoroughly studied, and by analyzing the float-zone growth of this simpler and better-characterized material, it was verified that phase equilibria information and solidification behavior could be extracted from and explained by these solidification experiments. Two different types of nonplanar, crystal/melt interface morphologies were observed in the rm Ca_3Al_2O_6 experiments. Each reflected the influence of the phase equilibria in the CaO-rm Al_2O_3 system and component segregation in the melt. The molten zone compositions were found to approach those predicted by the CaO-rm Al_2O_3 phase diagram as the growth rate decreased, in accordance with the Burton-Prim Slichter relationship. Excellent agreement was obtained between actual phases found to coexist at the rm Ca_3Al_2O_6 /melt interface and the predictions of classical crystal growth theory. Based on the results of the rm Ca _3Al_2O_6 crystallization study, the crystal/melt equilibria in the far more complex rm Bi_2O_3-SrO-CaO-CuO system was evaluated by determining the phases formed during the superconductor growth experiments. The melt compositions were found to be rm Bi_2O_3 -rich and SrO-poor relative to the compositions of the 2212 crystals grown from them. The CaO and CuO segregation coefficients, on the other hand, were observed to be near unity. As one would expect for an incongruently -melting compound, segregation at the solidification front generally decreased with increasing crystallization temperature, but all the segregation coefficients were not observed to simultaneously approach unity. The superconducting transition temperatures (T _{rm C}'s) of six as-crystallized samples having homogeneous crystal compositions were also measured. Sample T_{rm C} was observed to increase with increasing growth temperature and, therefore, change with crystal composition. The results of this study suggested that it is desirable to grow crystals at the highest possible crystallization temperature since they will: (1) have the highest as-grown T_{rm C} 's, and (2) solidify with the least component segregation at the growth interface. In addition, the analysis presented here suggests that such growth is not recommended at higher growth rates, since crystals with mid-range solidus compositions (and consequently, moderate growth temperatures) should crystallize most reliably as single-phase samples at higher growth rates.

Identification and Control of Gravity Related Defect Formation During Melt Growth of Electro-Optic Single Crystals Bismuth Silicate(Bi12SiO20)

NASA Technical Reports Server (NTRS)

Becia, Piotr; Wiegel, Michaela E. K.

2004-01-01

A research carried out under Award Number NAG8-1487 was aimed at to the design, conduct and analysis of experiments directed at the identification and control of gravitational effects on crystal growth, segregation and defect formation in the Sillenite system: bismuth silicate (Bi(12)SiO(20)). Correlation analyses was conducted in order to establish the influence of gravity related defects introduced during crystal growth on critical, application specific properties. Achievement of the states objective was conducted during the period from Feb. 01, 1998 to Dec. 31, 2003 with the following anticipated milestones: 1. Establishment of capabilities for (a) reproducible Czochralski and Bridgman-type growth of BSO single crystals and (b) for comprehensive analysis of crystalline and chemical defects as well as for selective property characterization of grown crystals (year 1). 2. Design and execution of critical space growth experiment(s) based on analyses of prefatory space results (experiments aimed at establishing the viability of planned approaches and procedures) and on unresolved issues related to growth, segregation and defect formation associated with conventional growth in Bridgman geometries. Comparative analysis of growth under conventional and under mu-g conditions; identification of gravity related defect formation during conventional Bridgman growth and formulation of approaches for their control (years 2 and 3). Development of charge confinement system which permits growth interface demarcation (in a mu-g environment) as well as minimization of confinement related stress and contamination during growth; design of complementary mu-g growth experiments aimed at quantitative mu-g growth and segregation analyses (year 4). 3. Conduct of quantitative mu-g growth experiments directed at: (a) identification and control of gravity related crystalline and chemical defect formation during single crystal growth of Bi(12)SiO(20) and at (b) defect engineering -the development of approaches to the controlled generation during crystal growth of specified point defects in homogeneous distribution (year 5). The proposed research places focus on a class of materials which have outstanding electrical and optical properties but have so far failed to reach their potential, primarily because of our inability to control adequately their stoichiometry and crystal defect formation as well as confinement related contamination and lattice stress.

Flight Experiments of Physical Vapor Transport of ZnSe: Growth of Crystals in Various Convective Conditions

NASA Technical Reports Server (NTRS)

Su, Ching-Hua

2015-01-01

A low gravity material experiment will be performed in the Material Science Research Rack (MSRR) on International Space Station (ISS). The flight experiment will conduct crystal growths of ZnSe and related ternary compounds, such as ZnSeS and ZnSeTe, by physical vapor transport (PVT). The main 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 grown crystals as results of buoyancy-driven convection and growth interface fluctuations caused by irregular fluid-flows on Earth. The investigation consists of extensive ground-based experimental and theoretical research efforts and concurrent flight experimentation. The objectives of the ground-based studies are (1) obtain the experimental data and conduct the analyses required to define the optimum growth parameters for the flight experiments, (2) perfect various characterization techniques to establish the standard procedure for material characterization, (3) quantitatively establish the characteristics of the crystals grown on Earth as a basis for subsequent comparative evaluations of the crystals grown in a low-gravity environment and (4) develop theoretical and analytical methods required for such evaluations. ZnSe and related ternary compounds have been grown by vapor transport technique with real time in-situ non-invasive monitoring techniques. The grown crystals have been characterized extensively by various techniques to correlate the grown crystal properties with the growth conditions. This talk will focus on the ground-based studies on the PVT crystal growth of ZnSe and related ternary compounds, especially the effects of different growth orientations related to gravity direction on the grown crystals.

On thermal conditions and properties of thallium bromide single crystals grown by the Electro Dynamic Gradient method

NASA Astrophysics Data System (ADS)

Zheng, Zhiping; Yu, Yongtao; Gong, Shuping; Fu, Qiuyun; Zhou, Dongxiang

2013-05-01

The Electro Dynamic Gradient (EDG) method has been proved to be a feasible way to grow TlBr crystals in our previous work. In this research, the influence of thermal conditions such as cooling rate during growth process on the crystal performance was investigated. Crystals of approximately 12 mm diameter were obtained by the EDG method at different cooling rates during the growth process, and the quality of the crystals was routinely evaluated by X-ray diffraction (XRD), infrared (IR) and ultraviolet (UV) transmission, I-V measurement and energy response spectrum. The results proved that thermal conditions during growth had a profound influence on the characteristics of the crystals.

A Review of In Situ Observations of Crystallization and Growth in High Temperature Oxide Melts

NASA Astrophysics Data System (ADS)

Wang, Zhanjun; Sohn, Il

2018-05-01

This review summarizes the significant results of high-temperature confocal laser scanning microscopy (CLSM) and single hot thermocouple technology (SHTT) and its application in observing the crystallization and growth in high-temperature oxide melts from iron- and steel-making slags to continuous casting mold fluxes. Using in situ observations of CLSM and SHTT images of high-temperature molten oxides with time, temperature, and composition, the crystallization behavior, including crystal morphology, crystallization temperature, initial nucleation and growth rate, could be obtained. The broad range of applications using in situ observations during crystallization have provided a wealth of opportunities in pyrometallurgy and is provided in this review.

Potassium-cobalt sulphate crystal growth assisted by low frequency vibrations

NASA Astrophysics Data System (ADS)

Sadovsky, A.; Ermochenkov, I.; Dubovenko, E.; Sukhanova, E.; Bebyakin, M.; Dubov, V.; Avetissov, I.

2018-02-01

Single crystals of K2Co(SO4)2·6H2O were grown from solution using the temperature reduction method enhanced by the axial low frequency vibration control technique (AVC-technique). Physical modeling of heat-mass transfer in solution under the AVC action was performed. The growth rate of the AVC grown crystal was found to be twice that of the crystal grown under natural convection conditions. Analysis of spectral characteristics (absorption and Raman spectra) as well as structural properties (dislocation density and microhardness) of the grown crystals showed the significant superiority of the AVC technique for the growth of K2Co(SO4)2·6H2O crystals.

Growth of CdZnTe Crystals for Radiation Detector Applications by Directional Solidification

NASA Technical Reports Server (NTRS)

Su, Ching-Hua

2014-01-01

Advances in Cadmium Zinc Telluride (Cd(sub 1-x)Zn(sub x)Te) growth techniques are needed for the production of large-scale arrays of gamma and x-ray astronomy. The research objective is to develop crystal growth recipes and techniques to obtain large, high quality CdZnTe single crystal with reduced defects, such as charge trapping, twinning, and tellurium precipitates, which degrade the performance of CdZnTe and, at the same time, to increase the yield of usable material from the CdZnTe ingot. A low gravity material experiment, "Crystal Growth of Ternary Compound Semiconductors in Low Gravity Environment", will be performed in the Material Science Research Rack (MSRR) on International Space Station (ISS). One section of the flight experiment is the melt growth of CdZnTe ternary compounds. This talk will focus on the ground-based studies on the growth of Cd(sub 0.80)Zn(sub 0.20)Te crystals for radiation detector applications by directional solidification. In this investigation, we have improved the properties that are most critical for the detector applications (electrical properties and crystalline quality): a) Electrical resistivity: use high purity starting materials (with reproducible impurity levels) and controlled Cd over pressure during growth to reproducibly balance the impurity levels and Cd vacancy concentration b) Crystalline quality: use ultra-clean growth ampoule (no wetting after growth), optimized thermal profile and ampoule design, as well as a technique for supercool reduction to growth large single crystal with high crystalline quality

Lattice Boltzmann Simulation of Water Isotope Fractionation During Growth of Ice Crystals in Clouds

NASA Astrophysics Data System (ADS)

Lu, G.; Depaolo, D.; Kang, Q.; Zhang, D.

2006-12-01

The isotopic composition of precipitation, especially that of snow, plays a special role in the global hydrological cycle and in reconstruction of past climates using polar ice cores. The fractionation of the major water isotope species (HHO, HDO, HHO-18) during ice crystal formation is critical to understanding the global distribution of isotopes in precipitation. Ice crystal growth in clouds is traditionally treated with a spherically- symmetric steady state diffusion model, with semi-empirical modifications added to account for ventilation and for complex crystal morphology. Although it is known that crystal growth rate, which depends largely on the degree of vapor over-saturation, determines crystal morphology, there are no existing quantitative models that directly relate morphology to the vapor saturation factor. Since kinetic (vapor phase diffusion-controlled) isotopic fractionation also depends on growth rate, there should be a direct relationship between vapor saturation, crystal morphology, and crystal isotopic composition. We use a 2D Lattice-Boltzmann model to simulate diffusion-controlled ice crystal growth from vapor- oversaturated air. In the model, crystals grow solely according to the diffusive fluxes just above the crystal surfaces, and hence crystal morphology arises from the initial and boundary conditions in the model and does not need to be specified a priori. The input parameters needed are the isotope-dependent vapor deposition rate constant (k) and the water vapor diffusivity in air (D). The values of both k and D can be computed from kinetic theory, and there are also experimentally determined values of D. The deduced values of k are uncertain to the extent that the sticking coefficient (or accommodation coefficient) for ice is uncertain. The ratio D/k is a length that determines the minimum scale of dendritic growth features and allows us to scale the numerical calculations to atmospheric conditions using a dimensionless Damkohler number: Da = kh/D, where h is the width of the 2D calculation domain. Varying the nondimensional Da in the model is equivalent to varying the scale (h) in the model. Our calculations confirm that the crystal/vapor isotopic fractionation approaches the equilibrium value, and the crystals are compact (circular in 2D) as the saturation factor approaches unity (S= 1.0). At higher oversaturation (e.g. S = 1.2), dendritic crystals of millimeter size develop on timescales appropriate to cloud processes, the isotopic fractionations are dominated by kinetic effects, and similar to those predicted by the spherical diffusion model. Dendritic crystals are constrained to be relatively large, with dimension much greater than D/k. The most difficult aspect of the modeling is to account for the large density difference between air and ice, which requires us to use a fictitious higher density for the vapor-oversaturated air and scale the crystal growth time accordingly. A different approach, using a larger scale simulation to derive boundary conditions for a nested smaller scale calculation is in progress. The results to date clarify the controls on dendritic crystal growth, the relationships between saturation state, growth rate, crystal morphology and isotopic fractionation, and provide limits on the value of the accommodation coefficient.

Controllable Growth of Monolayer MoS2 and MoSe2 Crystals Using Three-temperature-zone Furnace

NASA Astrophysics Data System (ADS)

Zheng, Binjie; Chen, Yuanfu

2017-12-01

Monolayer molybdenum disulfide (MoS2) and molybdenum diselenide (MoSe2) have attracted a great attention for their exceptional electronic and optoelectronic properties among the two dimensional family. However, controllable synthesis of monolayer crystals with high quality needs to be improved urgently. Here we demonstrate a chemical vapor deposition (CVD) growth of monolayer MoS2 and MoSe2 crystals using three-temperature-zone furnace. Systematical study of the effects of growth pressure, temperature and time on the thickness, morphology and grain size of crystals shows the good controllability. The photoluminescence (PL) characterizations indicate that the as-grown monolayer MoS2 and MoSe2 crystals possess excellent optical qualities with very small full-width-half-maximum (FWHM) of 96 me V and 57 me V, respectively. It is comparable to that of exfoliated monolayers and reveals their high crystal quality. It is promising that our strategy should be applicable for the growth of other transition metal dichalcogenides (TMDs) monolayer crystals.

Growth of NH4Cl Single Crystal from Vapor Phase in Vertical Furnace

NASA Astrophysics Data System (ADS)

Nigara, Yutaka; Yoshizawa, Masahito; Fujimura, Tadao

1983-02-01

A pure and internally stress-free single crystal of NH4Cl was grown successfully from the vapor phase. The crystal measured 1.6 cmφ× 2 cm and had the disordered CsCl structure, which was stable below 184°C. The crystal was grown in an ampoule in a vertical furnace, in which the vapor was efficiently transported both by diffusion and convection. In line with the growth mechanism of a single crystal, the temperature fluctuation (°C/min) on the growth interface was kept smaller than the product of the temperature gradient (°C/cm) and the growth rate (cm/min). The specific heat of the crystal was measured around -31°C (242 K) during cooling and heating cycles by AC calorimetry. The thermal hysteresis (0.4 K) obtained here was smaller than that (0.89 K) of an NH4Cl crystal grown from its aqueous solution with urea added as a habit modifier.

Two-Dimensional Raman Correlation Spectroscopy Study of Poly[(R)-3-hydroxybutyrate- co-(R)-3-hydroxyhexanoate] Copolymers.

PubMed

Noda, Isao; Roy, Anjan; Carriere, James; Sobieski, Brian J; Chase, D Bruce; Rabolt, John F

2017-07-01

Two-dimensional correlation analysis was applied to the time-dependent evolution of Raman spectra during the isothermal crystallization of bioplastic, poly[(R)-3-hydroxybutyrate- co-(R)-3-hydroxyhexanoate] or PHBHx copolymer. Simultaneous Raman measurement of both carbonyl stretching and low-frequency crystalline lattice mode regions made it possible to carry out the highly informative hetero-mode correlation analysis. The crystallization process of PHBHx involves: (1) the early nucleation stage; (2) the primary growth of well-ordered crystals of PHBHx; and (3) the secondary crystal growth phase. The latter stage probably occurs in the inter-lamellar region, with an accompanying reduction of the amorphous component, which occurs most dominantly during the primary crystal growth. The development of a fully formed lamellar structure comprising the 2 1 helices occurs after the primary growth of crystals. In the later stage, secondary inter lamellar space crystallization occurs after the full formation of packed helices comprising the lamellae.

Investigation on the growth and characterization of 4-aminobenzophenone single crystal by the vertical dynamic gradient freeze technique

NASA Astrophysics Data System (ADS)

Prabhakaran, SP.; Ramesh Babu, R.; Sukumar, M.; Bhagavannarayana, G.; Ramamurthi, K.

2014-03-01

Growth of bulk single crystal of 4-Aminobenzophenone (4-ABP) from the vertical dynamic gradient freeze (VDGF) setup designed with eight zone furnace was investigated. The experimental parameters for the growth of 4-ABP single crystal with respect to the design of VDGF setup are discussed. The eight zones were used to generate multiple temperature gradients over the furnace, and video imaging system helped to capture the real time growth and solid-liquid interface. 4-ABP single crystal with the size of 18 mm diameter and 40 mm length was grown from this investigation. Structural and optical quality of grown crystal was examined by high resolution X-ray diffraction and UV-visible spectral analysis, respectively and the blue emission was also confirmed from the photoluminescence spectrum. Microhardness number of the crystal was estimated at different loads using Vicker's microhardness tester. The size and quality of single crystal grown from the present investigation are compared with the vertical Bridgman grown 4-ABP.

Characterizing the effect of growth conditions and crystal habit on the distribution of imperfections amongst populations of crystals

NASA Astrophysics Data System (ADS)

Price, C. J.

1993-03-01

The distribution of gross imperfections amongst populations of copper sulphate pentahydrate crystals grown under different conditions of purity and temperature are examined. The frequency of imperfection increases with decreasing crystal size. The nature of the imperfections vary with growth temperature and impurities present.

International Conference on Crystal Growth (10th) Held in San Diego, California, on 16-21 August 1992

DTIC Science & Technology

1993-07-14

precipitation. This additive appeared to retard growth be different for the nuclei formed on additive molecules and and to stimulate nucleation of BaSO4...dispersion is described by some of different crystals of the same material grow at different rates. the mentioned distributions. Aiming at that, the...of crystals that grow with different a from the histo- grams of distributions of crystal growth rates [2,3], and it is 1. U.K. Burton et al., Phil

Secondary Crystal Growth on a Cracked Hydrotalcite-Based Film Synthesized by the Sol-Gel Method.

PubMed

Lee, Wooyoung; Lee, Chan Hyun; Lee, Ki Bong

2016-05-02

The sol-gel synthesis method is an attractive technology for the fabrication of ceramic films due to its preparation simplicity and ease of varying the metal composition. However, this technique presents some limitations in relation to the film thickness. Notably, when the film thickness exceeds the critical limit, large tensile stresses occur, resulting in a cracked morphology. In this study, a secondary crystal growth method was introduced as a post-treatment process for Mg/Al hydrotalcite-based films synthesized by the sol-gel method, which typically present a cracked morphology. The cracked hydrotalcite-based film was hydrothermally treated for the secondary growth of hydrotalcite crystals. In the resulting film, hydrotalcite grew with a vertical orientation, and the gaps formed during the sol-gel synthesis were filled with hydrotalcite after the crystal growth. The secondary crystal growth method provides a new solution for cracked ceramic films synthesized by the sol-gel method.

Illusory spirals and loops in crystal growth

PubMed Central

Shtukenberg, Alexander G.; Zhu, Zina; Bhandari, Misha; Song, Pengcheng; Kahr, Bart; Ward, Michael D.

2013-01-01

The theory of dislocation-controlled crystal growth identifies a continuous spiral step with an emergent lattice displacement on a crystal surface; a mechanistic corollary is that closely spaced, oppositely winding spirals merge to form concentric loops. In situ atomic force microscopy of step propagation on pathological l-cystine crystals did indeed show spirals and islands with step heights of one lattice displacement. We show by analysis of the rates of growth of smaller steps only one molecule high that the major morphological spirals and loops are actually consequences of the bunching of the smaller steps. The morphology of the bunched steps actually inverts the predictions of the theory: Spirals arise from pairs of dislocations, loops from single dislocations. Only through numerical simulation of the growth is it revealed how normal growth of anisotropic layers of molecules within the highly symmetrical crystals can conspire to create features in apparent violation of the classic theory. PMID:24101507

A Rationale for System-Dependent Advantages and Disadvantages of Solution Crystal Growth at Low Gravity

NASA Technical Reports Server (NTRS)

Rosenberger, Franz; Vekilov, Peter G.; Lin, Hong; Alexander, J. Iwan D.

1997-01-01

Protein crystallization experiments at reduced gravity have yielded crystals that, depending on the specific material, are either superior or inferior in their structural perfection compared to counterparts grown at normal gravity. A reduction of the crystals' quality due to their growth at low gravity cannot be understood from existing models. Our experimental investigations of the ground-based crystallization of the protein lysozyme have revealed pronounced unsteady growth layer dynamics and associated defect formation under steady external conditions. Through scaling analysis and numerical simulations we show that the observed fluctuations originate from the coupling of bulk transport with non-linear interface kinetics under mixed kinetics-transport control of the growth rate. The amplitude of the fluctuations is smallest when either transport or interfacial kinetics dominate the control of the crystallization process. Thus, depending on the specific system, crystal quality may be improved by either enhancing or suppressing the transport in the solution. These considerations provide, for the first time, a material-dependent rationale for the advantages, as well as the disadvantages, of reduced gravity for (protein) crystallization.

Vapor Growth and Characterization of Cr-Doped ZnSe Crystals

NASA Technical Reports Server (NTRS)

Su, Ching-Hua; Feth, Shari; Volz, M. P.; Matyi, R.; George, M. A.; Chattopadhyay, K.; Burger, A.; Lehoczky, S. L.

1999-01-01

Cr-doped ZnSe single crystals were grown by a self-seeded physical vapor transport technique in both vertical (stabilized) and horizontal configurations. The source materials were mixtures of ZnSe and CrSe. Growth temperatures were in the range of 1140-1150 C and the furnace translation rates were 1.9-2.2 mm/day. The surface morphology of the as-grown crystals was examined by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Different features of the as-grown surface of the vertically and horizontally grown crystals suggest that different growth mechanisms were involved in the two growth configurations. The [Cr] doping levels were determined to be in the range of 1.8-8.3 x 10 (exp 19) cm (exp -3) from optical absorption measurements. The crystalline quality of the grown crystals were examined by high-resolution triple-crystal X-ray diffraction (HRTXD) analysis.

Carbon agent chemical vapor transport growth of Ga2O3 crystal

NASA Astrophysics Data System (ADS)

Jie, Su; Tong, Liu; Jingming, Liu; Jun, Yang; Guiying, Shen; Yongbiao, Bai; Zhiyuan, Dong; Youwen, Zhao

2016-10-01

Beta-type gallium oxide (β-Ga2O3) is a new attractive material for optoelectronic devices. Different methods had been tried to grow high quality β-Ga2O3 crystals. In this work, crystal growth of Ga2O3 has been carried out by chemical vapor transport (CVT) method in a closed quartz tube using C as transport agent and sapphire wafer as seed. The CVT mass flux has been analyzed by theoretical calculations based on equilibrium thermodynamics and 1D diffusional mass transport. The crystal growth experimental results are in agreement with the theoretical predictions. Influence factors of Ga2O3 crystal growth, such as temperature distribution, amount of C as transport agent used, have also been discussed. Structural (XRD) and optical (Raman spectroscopy, photoluminescence spectrum) properties of the CVT-Ga2O3 crystal are presented. Project supported by the National Natural Science Foundation of China (Nos. 61474104, 61504131).

Growth and studies of cyclohexylammonium 4-methoxy benzoate single crystal for nonlinear optical applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sathya, P.; Gopalakrishnan, R., E-mail: krgkrishnan@annauniv.edu

2015-06-24

Cyclohexylammonium 4-Methoxy Benzoate (C4MB) was synthesised and the functional groups were confirmed by FTIR analysis. The purified C4MB (by repeated recrystallisation) was used for single crystal growth. Single crystal of cyclohexylammonium 4-methoxy benzoate was successfully grown by slow evaporation solution growth method at ambient temperature. Structural orientations were determined from single crystal X-ray diffractometer. Optical absorption and cut off wavelength were identified by UV-Visible spectroscopy. Thermal stability of the crystal was studied from thermogravimetric and differential thermal analyses curves. Mechanical stability of the grown crystal was analysed by Vicker’s microhardness tester. The Second Harmonic Generation (SHG) study revealed that themore » C4MB compound exhibits the SHG efficiency 3.3 times greater than KDP crystal.« less

Transport phenomena in the crystallization of lysozyme by osmotic dewatering and liquid-liquid diffusion in low gravity

NASA Technical Reports Server (NTRS)

Todd, Paul; Sportiello, Michael G.; Gregory, Derek; Cassanto, John M.; Alvarado, Ulises A.; Ostroff, Robert; Korszun, Z. R.

1993-01-01

Two methods of protein crystallization, osmotic dewatering and liquid-liquid diffusion, like the vapor diffusion (hanging-drop and sessile-drop) methods allow a gradual approach to supersaturation conditions. The crystallization of hen egg-white lysozyme, an extensively characterized protein crystal, in the presence of sodium chloride was used as an experimental model with which to compare these two methods in low gravity and in the laboratory. Comparisons of crystal growth rates by the two methods under the two conditions have, to date, indicated that the rate of crystal growth by osmotic dewatering is nearly the same in low gravity and on the ground, while much faster crystal growth rates can be achieved by the liquid-liquid diffusion method in low gravity.

Large-volume protein crystal growth for neutron macromolecular crystallography.

PubMed

Ng, Joseph D; Baird, James K; Coates, Leighton; Garcia-Ruiz, Juan M; Hodge, Teresa A; Huang, Sijay

2015-04-01

Neutron macromolecular crystallography (NMC) is the prevailing method for the accurate determination of the positions of H atoms in macromolecules. As neutron sources are becoming more available to general users, finding means to optimize the growth of protein crystals to sizes suitable for NMC is extremely important. Historically, much has been learned about growing crystals for X-ray diffraction. However, owing to new-generation synchrotron X-ray facilities and sensitive detectors, protein crystal sizes as small as in the nano-range have become adequate for structure determination, lessening the necessity to grow large crystals. Here, some of the approaches, techniques and considerations for the growth of crystals to significant dimensions that are now relevant to NMC are revisited. These include experimental strategies utilizing solubility diagrams, ripening effects, classical crystallization techniques, microgravity and theoretical considerations.

Magnetic field controlled single crystal growth and surface modification of titanium alloys exposed for biocompatibility

NASA Astrophysics Data System (ADS)

Hermann, Regina; Uhlemann, Margitta; Wendrock, Horst; Gerbeth, Gunter; Büchner, Bernd

2011-03-01

The aim of this work is growth and characterisation of Ti55Nb45 (wt%) single crystals by floating-zone single crystal growth of intermetallic compounds using two-phase radio-frequency (RF) electromagnetic heating. Thereby, the process and, in particular, the flow field in the molten zone is influenced by additional magnetic fields. The growth of massive intermetallic single crystals is very often unsuccessful due to an unfavourable solid-liquid interface geometry enclosing concave fringes. It is generally known that the crystallization process stability is enhanced if the crystallization interface is convex. For this, a tailored magnetic two-phase stirrer system has been developed, which enables a controlled influence on the melt ranging from intensive inwards to outwards flows. Since Ti is favourably light, strong and biocompatible, it is one of the few materials that naturally match the requirements for implantation in the human body. Therefore, the magnetic system was applied to crystal growth of Ti alloys. The grown crystals were oriented and cut to cubes with the desired crystallographic orientations [1 0 0] and [1 0 1] normally on a plane. The electron backscatter diffraction (EBSD) technique was applied to clearly determine crystal orientation and to localize grain boundaries. The formation of oxidic nanotubes on Ti surfaces in dependence of the grain orientation was investigated, performed electrochemically by anodic oxidation from fluoride containing electrolyte.

Investigating calcite growth rates using a quartz crystal microbalance with dissipation (QCM-D)

NASA Astrophysics Data System (ADS)

Cao, Bo; Stack, Andrew G.; Steefel, Carl I.; DePaolo, Donald J.; Lammers, Laura N.; Hu, Yandi

2018-02-01

Calcite precipitation plays a significant role in processes such as geological carbon sequestration and toxic metal sequestration and, yet, the rates and mechanisms of calcite growth under close to equilibrium conditions are far from well understood. In this study, a quartz crystal microbalance with dissipation (QCM-D) was used for the first time to measure macroscopic calcite growth rates. Calcite seed crystals were first nucleated and grown on sensors, then growth rates of calcite seed crystals were measured in real-time under close to equilibrium conditions (saturation index, SI = log ({Ca2+}/{CO32-}/Ksp) = 0.01-0.7, where {i} represent ion activities and Ksp = 10-8.48 is the calcite thermodynamic solubility constant). At the end of the experiments, total masses of calcite crystals on sensors measured by QCM-D and inductively coupled plasma mass spectrometry (ICP-MS) were consistent, validating the QCM-D measurements. Calcite growth rates measured by QCM-D were compared with reported macroscopic growth rates measured with auto-titration, ICP-MS, and microbalance. Calcite growth rates measured by QCM-D were also compared with microscopic growth rates measured by atomic force microscopy (AFM) and with rates predicted by two process-based crystal growth models. The discrepancies in growth rates among AFM measurements and model predictions appear to mainly arise from differences in step densities, and the step velocities were consistent among the AFM measurements as well as with both model predictions. Using the predicted steady-state step velocity and the measured step densities, both models predict well the growth rates measured using QCM-D and AFM. This study provides valuable insights into the effects of reactive site densities on calcite growth rate, which may help design future growth models to predict transient-state step densities.

Calcite growth-rate inhibition by fulvic acids isolated from Big Soda Lake, Nevada, USA, The Suwannee River, Georgia, USA and by polycarboxylic acids

USGS Publications Warehouse

Reddy, Michael M.; Leenheer, Jerry

2011-01-01

Calcite crystallization rates are characterized using a constant solution composition at 25°C, pH=8.5, and calcite supersaturation (Ω) of 4.5 in the absence and presence of fulvic acids isolated from Big Soda Lake, Nevada (BSLFA), and a fulvic acid from the Suwannee River, Georgia (SRFA). Rates are also measured in the presence and absence of low-molar mass, aliphatic-alicyclic polycarboxylic acids (PCA). BSLFA inhibits calcite crystal-growth rates with increasing BSLFA concentration, suggesting that BSLFA adsorbs at growth sites on the calcite crystal surface. Calcite growth morphology in the presence of BSLFA differed from growth in its absence, supporting an adsorption mechanism of calcite-growth inhibition by BSLFA. Calcite growth-rate inhibition by BSLFA is consistent with a model indicating that polycarboxylic acid molecules present in BSLFA adsorb at growth sites on the calcite crystal surface. In contrast to published results for an unfractionated SRFA, there is dramatic calcite growth inhibition (at a concentration of 1 mg/L) by a SRFA fraction eluted by pH 5 solution from XAD-8 resin, indicating that calcite growth-rate inhibition is related to specific SRFA component fractions. A cyclic PCA, 1, 2, 3, 4, 5, 6-cyclohexane hexacarboxylic acid (CHXHCA) is a strong calcite growth-rate inhibitor at concentrations less than 0.1 mg/L. Two other cyclic PCAs, 1, 1 cyclopentanedicarboxylic acid (CPDCA) and 1, 1 cyclobutanedicarboxylic acid (CBDCA) with the carboxylic acid groups attached to the same ring carbon atom, have no effect on calcite growth rates up to concentrations of 10 mg/L. Organic matter ad-sorbed from the air onto the seed crystals has no effect on the measured calcite crystal-growth rates.

Growing Larger Crystals for Neutron Diffraction

NASA Technical Reports Server (NTRS)

Pusey, Marc

2003-01-01

Obtaining crystals of suitable size and high quality has been a major bottleneck in macromolecular crystallography. With the advent of advanced X-ray sources and methods the question of size has rapidly dwindled, almost to the point where if one can see the crystal then it was big enough. Quality is another issue, and major national and commercial efforts were established to take advantage of the microgravity environment in an effort to obtain higher quality crystals. Studies of the macromolecule crystallization process were carried out in many labs in an effort to understand what affected the resultant crystal quality on Earth, and how microgravity improved the process. While technological improvements are resulting in a diminishing of the minimum crystal size required, neutron diffraction structural studies still require considerably larger crystals, by several orders of magnitude, than X-ray studies. From a crystal growth physics perspective there is no reason why these 'large' crystals cannot be obtained: the question is generally more one of supply than limitations mechanism. This talk will discuss our laboratory s current model for macromolecule crystal growth, with highlights pertaining to the growth of crystals suitable for neutron diffraction studies.

The Si ribbon crystal for the solar battery using the horizontal pull method

NASA Technical Reports Server (NTRS)

Norifuji, H.; Matsuo, M.; Maki, T.

1979-01-01

A method utilizing a device to spray noble gases to cool the site of silicon crystal growth is described. The salient points are: (1) soft and uniform cooling was possible, (2) the length of the boundary surface of growth along the growth direction was made long over a wide width compared to the thickness, and (3) this made it possible to effectively remove the heat produced from solification. By using forced gas spraying on the solution surface in contact with the points of crystal growth, growth at the points of growth is enhanced and the rate of growth is speeded up.

Electromagnetic induction heating for single crystal graphene growth: morphology control by rapid heating and quenching

NASA Astrophysics Data System (ADS)

Wu, Chaoxing; Li, Fushan; Chen, Wei; Veeramalai, Chandrasekar Perumal; Ooi, Poh Choon; Guo, Tailiang

2015-03-01

The direct observation of single crystal graphene growth and its shape evolution is of fundamental importance to the understanding of graphene growth physicochemical mechanisms and the achievement of wafer-scale single crystalline graphene. Here we demonstrate the controlled formation of single crystal graphene with varying shapes, and directly observe the shape evolution of single crystal graphene by developing a localized-heating and rapid-quenching chemical vapor deposition (CVD) system based on electromagnetic induction heating. Importantly, rational control of circular, hexagonal, and dendritic single crystalline graphene domains can be readily obtained for the first time by changing the growth condition. Systematic studies suggest that the graphene nucleation only occurs during the initial stage, while the domain density is independent of the growth temperatures due to the surface-limiting effect. In addition, the direct observation of graphene domain shape evolution is employed for the identification of competing growth mechanisms including diffusion-limited, attachment-limited, and detachment-limited processes. Our study not only provides a novel method for morphology-controlled graphene synthesis, but also offers fundamental insights into the kinetics of single crystal graphene growth.

Interaction between Convection and Heat Transfer in Crystal Growth

NASA Technical Reports Server (NTRS)

1998-01-01

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.

High resolution electron microscopy study of crystal growth mechanisms in chicken bone composites

NASA Astrophysics Data System (ADS)

Cuisinier, F. J. G.; Steuer, P.; Brisson, A.; Voegel, J. C.

1995-12-01

The present study describes the early stages of chicken bone crystal growth, followed by high resolution electron microscopy (HREM). We have developed an original analysis procedure to determine the crystal structure. Images were first digitalized and selected areas were fast Fourier transformed. Numerical masks were selected around the most intense spots and the filtered signal was retransformed back to real space. The filtered images were then compared to computer calculated images to identify the inorganic mineral phase. Nanometer-sized particles were observed on amorphous areas. These particles have a structure loosely related to hydroxyapatite (HA) and a specific orientation. In a more advanced situation, the nanoparticles appeared to grow in two dimensions and to form plate-like crystals. These crystals seem, in a last growth step, to fuse by their (100) faces. These experimental observations allowed us to propose a four-step model for the development and growth of chicken bone crystals. The two initial stages are the ionic adsorption onto the organic substrate followed by the nucleation of nanometer-sized particles. The two following steps, i.e. two-dimensional growth of the nanoparticles leading to the formation of needle-like crystals, and the lateral fusion of these crystals by their (100) faces, are controlled only by spatial constraints inside the extracellular organic matrix.

Laboratory studies of crystal growth in magma

NASA Astrophysics Data System (ADS)

Hammer, J. E.; Welsch, B. T.; First, E.; Shea, T.

2012-12-01

The proportions, compositions, and interrelationships among crystalline phases and glasses in volcanic rocks cryptically record pre-eruptive intensive conditions, the timing of changes in crystallization environment, and the devolatilization history of eruptive ascent. These parameters are recognized as important monitoring tools at active volcanoes and interpreting geologic events at prehistoric and remote eruptions, thus motivating our attempts to understand the information preserved in crystals through an experimental appoach. We are performing laboratory experiments in mafic, felsic, and intermediate composition magmas to study the mechanisms of crystal growth in thermochemical environments relevant to volcanic environments. We target features common to natural crystals in igneous rocks for our experimental studies of rapid crystal growth phenomena: (1) Surface curvature. Do curved interfaces and spongy cores represent evidence of dissolution (i.e., are they corrosion features), or do they record the transition from dendritic to polyhedral morphology? (2) Trapped melt inclusions. Do trapped liquids represent bulk (i.e., far-field) liquids, boundary layer liquids, or something intermediate, depending on individual species diffusivity? What sequence of crystal growth rates leads to preservation of sealed melt inclusions? (3) Subgrain boundaries. Natural phenocrysts commonly exhibit tabular subgrain regions distinguished by small angle lattice misorientations or "dislocation lamellae" and undulatory extinction. Might these crystal defects be produced as dendrites undergo ripening? (4) Clusters. Contacting clusters of polymineralic crystals are the building blocks of cumulates, and are ubiquitous features of mafic volcanic rocks. Are plagioclase and clinopyroxene aligned crystallographically, suggesting an epitaxial (surface energy) relationship? (5) Log-normal size distribution. What synthetic cooling histories produce "natural" distributions of crystal sizes, and are phenocrystic textures uniquely attributed to staged cooling? In addition, we seek to explore the limitations of the experimental approach. Which aspects of natural crystallization sequences are adequately reproduced in experimental charges, and which are compromised by the obligatory reduced temporal and spatial scales of crystal growth experiments? What are the implications of synthetic starting materials and thermal pre-treatments for nucleation, growth, heterophase equilibria, and textural maturation?

Apparatus for single ice crystal growth from the melt.

PubMed

Zepeda, Salvador; Nakatsubo, Shunichi; Furukawa, Yoshinori

2009-11-01

A crystal growth apparatus was designed and built to study the effect of growth modifiers, antifreeze proteins and antifreeze glycoproteins (AFGPs), on ice crystal growth kinetics and morphology. We used a capillary growth technique to obtain a single ice crystal with well-defined crystallographic orientation grown in AFGP solution. The basal plane was readily observed by rotation of the capillary. The main growth chamber is approximately a 0.8 ml cylindrical volume. A triple window arrangement was used to minimize temperature gradients and allow for up to 10 mm working distance objective lens. Temperature could be established to within +/-10 mK in as little as 3.5 min and controlled to within +/-2 mK after 15 min for at least 10 h. The small volume growth chamber and fast equilibration times were necessary for parabolic flight microgravity experiments. The apparatus was designed for use with inverted and side mount configurations.

Multiple seeding for the growth of bulk GdBCO-Ag superconductors with single grain behaviour

NASA Astrophysics Data System (ADS)

Shi, Y.; Durrell, J. H.; Dennis, A. R.; Huang, K.; Namburi, D. K.; Zhou, D.; Cardwell, D. A.

2017-01-01

Rare earth-barium-copper oxide bulk superconductors fabricated in large or complicated geometries are required for a variety of engineering applications. Initiating crystal growth from multiple seeds reduces the time taken to melt-process individual samples and can reduce the problem of poor crystal texture away from the seed. Grain boundaries between regions of independent crystal growth can reduce significantly the flow of current due to crystallographic misalignment and the agglomeration of impurity phases. Enhanced supercurrent flow at such boundaries has been achieved by minimising the depth of the boundary between A growth sectors generated during the melt growth process by reducing second phase agglomerations and by a new technique for initiating crystal growth that minimises the misalignment between different growth regions. The trapped magnetic fields measured for the resulting samples exhibit a single trapped field peak indicating they are equivalent to conventional single grains.

Numerical investigation on the batch characteristics of liquid encapsulated vertical Bridgman crystal growth

NASA Astrophysics Data System (ADS)

Lan, C. W.; Ting, C. C.

1995-04-01

Since the liquid encapsulated vertical Bridgman (LEVB) crystal growth is a batch process, it is time dependent in nature. A numerical simulation is conducted to study the unsteady features of the process, including the dynamic evolution of heat flow, growth rate, and interface morphology during crystal growth. The numerical model, which is governed by time-dependent equations for momentum and energy transport, and the conditions for evolution of melt/crystal and melt/encapsulant interfaces, is approximated by a body-fitted coordinate finite-volume method. The resulting differential/algebraic equations are then solved by the ILU (0) preconditioned DASPK code. Sample calculations are mainly conducted for GaAs. Dynamic effects of some process parameters, such as the growth speed, the ambient temperature profile, and ampoule design, are illustrated through calculated results. Due to the heat of fusion release and time-dependent end effects, in some cases a near steady-state operation is not possible. The control of growth front by modifying the ambient temperature profile is also demonstrated. Calculations are also performed for a 4.8 cm diameter InP crystal. The calculated melt/seed interface shape is compared with the measured one from Matsumoto et al. [J. Crystal Growth 132 (1993) 348] and they are in good agreement.

Basic ammonothermal GaN growth in molybdenum capsules

NASA Astrophysics Data System (ADS)

Pimputkar, S.; Speck, J. S.; Nakamura, S.

2016-12-01

Single crystal, bulk gallium nitride (GaN) crystals were grown using the basic ammonothermal method in a high purity growth environment created using a non-hermetically sealed molybdenum (Mo) capsule and compared to growths performed in a similarly designed silver (Ag) capsule and capsule-free René 41 autoclave. Secondary ion mass spectrometry (SIMS) analysis revealed transition metal free (<1×1017 cm-3) GaN crystals. Anomalously low oxygen concentrations ((2-6)×1018 cm-3) were measured in a {0001} seeded crystal boule grown using a Mo capsule, despite higher source material oxygen concentrations ((1-5)×1019 cm-3) suggesting that molybdenum (or molybdenum nitrides) may act to getter oxygen under certain conditions. Total system pressure profiles from growth runs in a Mo capsule system were comparable to those without a capsule, with pressures peaking within 2 days and slowly decaying due to hydrogen diffusional losses. Measured Mo capsule GaN growth rates were comparable to un-optimized growth rates in capsule-free systems and appreciably slower than in Ag-capsule systems. Crystal quality replicated that of the GaN seed crystals for all capsule conditions, with high quality growth occurring on the (0001) Ga-face. Optical absorption and impurity concentration characterization suggests reduced concentrations of hydrogenated gallium vacancies (VGa-Hx).

Ice Crystal Growth Rates Under Upper Troposphere Conditions

NASA Technical Reports Server (NTRS)

Peterson, Harold S.; Bailey, Matthew; Hallett, John

2010-01-01

Atmospheric conditions for growth of ice crystals (temperature and ice supersaturation) are often not well constrained and it is necessary to simulate such conditions in the laboratory to investigate such growth under well controlled conditions over many hours. The growth of ice crystals from the vapour in both prism and basal planes was observed at temperatures of -60 C and -70 C under ice supersaturation up to 100% (200% relative humidity) at pressures derived from the standard atmosphere in a static diffusion chamber. Crystals grew outward from a vertical glass filament, thickening in the basal plane by addition of macroscopic layers greater than 2 m, leading to growth in the prism plane by passing of successive layers conveniently viewed by time lapse video.

Direct observation of crystal growth from solution using optical investigation of a growing crystal face

NASA Technical Reports Server (NTRS)

Lal, Ravindra

1994-01-01

The first technical report for the period 1 Jan. 1993 till 31 Dec. 1993 for the research entitled, 'Direct observation of crystal growth from solution using Optical Investigation of a growing crystal Face' is presented. The work on the project did not start till 1 June 1993 due to the non-availability of the required personnel. The progress of the work during the period 1 June 1993 till the end of 1993 is described. Significant progress was made for testing various optical diagnostic techniques for monitoring crystal solution. Some of the techniques that are being tested are: heterodyne detection technique, in which changes in phase are measured as a interferometric function of time/crystal growth; a conventional technique, in which a fringe brightness is measured as a function of crystal growth/time; and a Mach-Zehnder interferometric technique in which a fringe brightness is measured as a function of time to obtain information on concentration changes. During the second year it will be decided to incorporate the best interferometric technique along with the ellipsometric technique, to obtain real time in-situ growth rate measurements. A laboratory mock-up of the first two techniques were made and tested.

Semiconductor crystal growth and segregation problems on earth and in space

NASA Technical Reports Server (NTRS)

Gatos, H. C.

1982-01-01

Semiconductor crystal growth and segregation problems are examined in the context of their relationship to material properties, and some of the problems are illustrated with specific experimental results. The compositional and structural defects encountered in semiconductors are largely associated with gravity-induced convective currents in the melt; additional problems are introduced by variations in stoichiometry. It is demonstrated that in near-zero gravity environment, crystal growth and segregation takes place under ideal steady-state conditions with minimum convective interference. A discussion of the advantages of zero-gravity crystal growth is followed by a summary of problems arising from the absence of gravitational forces.

A low temperature furnace for solution crystal growth on the International Space Station

NASA Astrophysics Data System (ADS)

Baç, Nurcan; Harpster, Joseph; Maston, Robert A.; Sacco, Albert

2000-01-01

The Zeolite Crystal Growth Furnace Unit (ZCG-FU) is the first module in an integrated payload designed for low temperature crystal growth in solutions on the International Space Station (ISS). This payload is scheduled to fly on the ISS flight 7A.1 in an EXPRESS rack. Its name originated from early shuttle flight experiments limited to the growth of zeolite crystals but has since grown to include other materials of significant commercial interest using the solution method of crystal growth. Zeolites, ferroelectrics, piezeoelectrics and silver halides are some of the materials considered. The ZCG-FU experiment consists of a furnace unit and its electronic control system, and mechanically complex, crystal growth autoclaves suitable for use with a particular furnace and solution. The ZCG facility is being designed to grow into four independent furnaces controlled by IZECS (Improved Zeolite Electronic Control System). IZECS provides monitoring of critical parameters, data logging, safety monitoring, air-to-ground control and operator interfacing. It is suitable for controlling the four furnaces either individually or all at one time. It also contains the power management solid-state drivers and switches for the ZCG-FU furnace. The furnace contains 19 tubes operating at three different temperature zones. .

Crystal growth, structure analysis and characterisation of 2 - (1, 3 - dioxoisoindolin - 2 - yl) acetic acid single crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sankari, R. Siva, E-mail: sivasankari.sh@act.edu.in; Perumal, Rajesh Narayana

2014-04-24

Single crystal of dielectric material 2 - (1, 3 - dioxoisoindolin - 2 - yl) acetic acid has been grown by slow evaporation solution growth method. The grown crystal was harvested in 25 days. The crystal structure was analyzed by Single crystal X - ray diffraction. UV-vis-NIR analysis was performed to examine the optical property of the grown crystal. The thermal property of the grown crystal was studied by thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The dielectric measurements were carried out and the dielectric constant was calculated and plotted at all frequencies.

Czochralski crystal growth: Modeling study

NASA Technical Reports Server (NTRS)

Dudukovic, M. P.; Ramachandran, P. A.; Srivastava, R. K.; Dorsey, D.

1986-01-01

The modeling study of Czochralski (Cz) crystal growth is reported. The approach was to relate in a quantitative manner, using models based on first priniciples, crystal quality to operating conditions and geometric variables. The finite element method is used for all calculations.

Effect of amino acid doping on the growth and ferroelectric properties of triglycine sulphate single crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Raghavan, C.M.; Sankar, R.; Mohan Kumar, R.

2008-02-05

Effect of amino acids (L-leucine and isoleucine) doping on the growth aspects and ferroelectric properties of triglycine sulphate crystals has been studied. Pure and doped crystals were grown from aqueous solution by low temperature solution growth technique. The cell parameter values were found to significantly vary for doped crystals. Fourier transform infrared analysis confirmed the presence of functional groups in the grown crystal. Morphology study reveals that amino acid doping induces faster growth rate along b-direction leading to a wide b-plane and hence suitable for pyroelectric detector applications. Ferroelectric domain structure has been studied by atomic force microscopy and hysteresismore » measurements reveal an increase of coercive field due to the formation of single domain pattern.« less

Temperature Dependence of Morphology and Growth Mechanism of Vapor-Grown Cd crystals as Affected by Bi Impurities

NASA Astrophysics Data System (ADS)

Yumoto, Hisami; Hasiguti, Ryukiti R.

1984-07-01

Hexagonal prismatic Cd crystals having {10\\bar{1}0} prismatic planes, or occasionally having {11\\bar{2}0} prismatic planes, were grown as high-temperature-type Cd crystals by the thin layer VLS mechanism at Ts (growth temperature) ≥ Tt (transition temperature range: 250-260°C). Pencil-shaped Cd crystals (low-temperature-type Cd crystals) were grown, having {10\\bar{1}0} and {11\\bar{2}0} prismatic planes and {10\\bar{1}1} pyramidal planes by the mixed-type VLS mechanism at Ts≤Tt. When the growth temperature was decreased below Tt, the shape of the solid-liquid interface changed from rounded to faceted. Three processes for the termination of the mixed-type VLS growth are proposed.

Crystallization of Silicon Ribbons

NASA Technical Reports Server (NTRS)

Leipold, M. H.

1984-01-01

Purity constraints for reasonable solar-cell efficiency require that silicon-ribbon growth for photovoltaics occur in a regime in which constitutional supercooling or other compositional effects on the crystallization front are not important. A major consideration in the fundamentals of crystallization is the removal of the latent heat of fusion. The direction of removal, compared with the growth direction, has a major influence on the crystallization rate and the development of localized stresses. The detailed shape of the crystallization front appears to have two forms: that required for dendritic-web growth, and that occurring in all others. After the removal of the latent heat of fusion, the thermal-mechanical behavior of all ribbons appears similar within the constraints of the exothermal gradient. The technological constraints in achieving the required thermal and mechanical conditions vary widely among the growth processes.

Crystallization of the collagen-like polypeptide (PPG)10 aboard the International Space Station. 1. Video observation.

PubMed

Vergara, Alessandro; Corvino, Ermanno; Sorrentino, Giosué; Piccolo, Chiara; Tortora, Alessandra; Carotenuto, Luigi; Mazzarella, Lelio; Zagari, Adriana

2002-10-01

Single chains of the collagen model polypeptide with sequence (Pro-Pro-Gly)(10), hereafter referred to as (PPG)(10), aggregate to form rod-shaped triple helices. Crystals of (PPG)(10) were grown in the Advanced Protein Crystallization Facility (APCF) both onboard the International Space Station (ISS) and on Earth. The experiments allow the direct comparison of four different crystallization environments for the first time: solution in microgravity ((g), agarose gel in (g, solution on earth, and gel on earth. Both on board and on ground, the crystal growth was monitored by a CCD video camera. The image analysis provided information on the spatial distribution of the crystals, their movement and their growth rate. The analysis of the distribution of crystals reveals that the crystallization process occurs as it does in batch conditions. Slow motions have been observed onboard the ISS. Different to Space-Shuttle experiment, the crystals onboard the ISS moved coherently and followed parallel trajectories. Growth rate and induction time are very similar both in gel and in solution, suggesting that the crystal growth rate is controlled by the kinetics at the interface under the used experimental conditions. These results provide the first data in the crystallogenesis of (PPG)(10), which is a representative member of non-globular, rod-like proteins.

The mechanism of deceleration of nucleation and crystal growth by the small addition of transition metals to lithium disilicate glasses

PubMed Central

Thieme, Katrin; Avramov, Isak; Rüssel, Christian

2016-01-01

The addition of small amounts of niobium or tantalum oxide to lithium disilicate glass provokes a drastic decrease of the steady-state nucleation rates and the crystal growth velocities. The viscosity of the residual glassy matrix is considered as a function of the crystallization degree in the course of a non-isothermal crystallization. For simplification, a homogeneous distribution of the added oxides in the glass matrix is assumed. While the viscosity initially decreases, it significantly increases again for higher crystallization degrees hindering crystal growth. However, it was shown that the additives are enriched at the crystal interface. Several possible reasons for the inhibition of nucleation and growth kinetics such as viscosity, interfacial energy crystal/glassy phase, thermodynamic driving force or impingement rate are discussed. Since the crystallization front is blocked by the additives the impingement rate is decreased with increasing additive concentration. Since small concentrations of Nb2O5 and Ta2O5 have a drastic effect on the nucleation, these components should be enriched at the interface crystal/glass. This will only take place, if it leads to a decrease in the interfacial energy. Since this effect alone should result in an increase of the nucleation rate, it must be overcompensated by kinetic effects. PMID:27150844

Growth and characterization of high-purity SiC single crystals

NASA Astrophysics Data System (ADS)

Augustine, G.; Balakrishna, V.; Brandt, C. D.

2000-04-01

High-purity SiC single crystals with diameter up to 50 mm have been grown by the physical vapor transport method. Finite element analysis was used for thermal modeling of the crystal growth cavity in order to reduce stress in the grown crystal. Crystals are grown in high-purity growth ambient using purified graphite furniture and high-purity SiC sublimation sources. Undoped crystals up to 50 mm in diameter with micropipe density less than 100 cm -2 have been grown using this method. These undoped crystals exhibit resistivities in the 10 3 Ω cm range and are p-type due to the presence of residual acceptor impurities, mainly boron. Semi-insulating SiC material is obtained by doping the crystal with vanadium. Vanadium has a deep donor level located near the middle of the band gap, which compensates the residual acceptor resulting in semi-insulating behavior.

Protein-crystal growth experiment (planned)

NASA Technical Reports Server (NTRS)

Fujita, S.; Asano, K.; Hashitani, T.; Kitakohji, T.; Nemoto, H.; Kitamura, S.

1988-01-01

To evaluate the effectiveness of a microgravity environment on protein crystal growth, a system was developed using 5 cubic feet Get Away Special payload canister. In the experiment, protein (myoglobin) will be simultaneously crystallized from an aqueous solution in 16 crystallization units using three types of crystallization methods, i.e., batch, vapor diffusion, and free interface diffusion. Each unit has two compartments: one for the protein solution and the other for the ammonium sulfate solution. Compartments are separated by thick acrylic or thin stainless steel plates. Crystallization will be started by sliding out the plates, then will be periodically recorded up to 120 hours by a still camera. The temperature will be passively controlled by a phase transition thermal storage component and recorded in IC memory throughout the experiment. Microgravity environment can then be evaluated for protein crystal growth by comparing crystallization in space with that on Earth.

Crystal Growth Inhibitors for the Prevention of L-Cystine Kidney Stones Through Molecular Design

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rimer, Jeffrey D.; An, Zhihua; Zhu, Zina

2010-11-12

Crystallization of L-cystine is a critical step in the pathogenesis of cystine kidney stones. Treatments for this disease are somewhat effective but often lead to adverse side effects. Real-time in situ atomic force microscopy (AFM) reveals that L-cystine dimethylester (L-CDME) and L-cystine methylester (L-CME) dramatically reduce the growth velocity of the six symmetry-equivalent {l_brace}100{r_brace} steps because of specific binding at the crystal surface, which frustrates the attachment of L-cystine molecules. L-CDME and L-CME produce L-cystine crystals with different habits that reveal distinct binding modes at the crystal surfaces. The AFM observations are mirrored by reduced crystal yield and crystal sizemore » in the presence of L-CDME and L-CME, collectively suggesting a new pathway to the prevention of L-cystine stones by rational design of crystal growth inhibitors.« less

[Microcosmic mechanisms of amorphous indomethacin crystallization and the influence of nano-coating on crystallization].

PubMed

Hui, Ou-Yang; Yi, Tao; Zheng, Qin; Liu, Feng

2011-06-01

Amorphous drugs have higher solubility, better oral bioavailability and are easier to be absorbed than their crystalline counterparts. However, the amorphous drugs, with weak stability, are so easy to crystallize that they will lose the original advantages. Polarization microscope, scanning electron microscope, differential scanning calorimetry, X-ray diffractomer and Raman spectroscopy were used to study the microcosmic crystallization mechanisms of amorphous indometacin and the performance of the drug crystals. The results showed that the growth rate of amorphous indometacin crystals at the free surface was markedly faster than that through the bulk, and that the crystal growth rate decreased observably after spraying an ultrathin melting gold (10 nm) at the free surface of the drug. These results indicated that the high growth rates of amorphous drugs crystals at the free surface were the key to their stability and that an ultrathin coating could be applied to enhance the stability of amorphous drugs.

A Novel Method of Fabricating a Well-Faceted Large-Crystal Diamond Through MPCVD

NASA Astrophysics Data System (ADS)

Man, Weidong; Weng, Jun; Wu, Yuqiong; Chen, Peng; Yu, Xuechao; Wang, Jianhua

2009-12-01

A novel method was developed to deposit a large crystal diamond with good facets up to 1000 μm on a tungsten substrate using a microwave plasma enhanced chemical vapor deposition (MPCVD). This method consists of two steps, namely single-crystal nucleation and growth. Prior to the fabrication of the well-faceted, large crystal diamond, an investigation was made into the nucleation and growth of the diamond which were affected by the O2 concentration and substrate temperature. Deposited diamond crystals were characterized by scanning electron microscopy and micro-Raman spectroscopy. The results showed that the conditions of single-crystal nucleation were appropriate when the ratio of H2/CH4/O2 was about 200/7.0/2.0, while the substrate temperature Ts of 1000°C to 1050°C was the appropriate range for single-crystal diamond growth. Under the optimum parameters, a well-faceted large crystal diamond was obtained.

Bulk Group-III Nitride Crystal Growth in Supercritical Ammonia-Sodium Solutions

NASA Astrophysics Data System (ADS)

Griffiths, Steven Herbert

Gallium nitride (GaN) and its alloys with indium nitride (InGaN) and aluminum nitride (AlGaN), collectively referred to as Group-III Nitride semiconductors, have enabled white solid-state lighting (SSL) sources and power electronic devices. While these technologies have already made a lasting, positive impact on society, improvements in design and efficiency are anticipated by shifting from heteroepitaxial growth on foreign substrates (such as sapphire, Si, SiC, etc.) to homoepitaxial growth on native, bulk GaN substrates. Bulk GaN has not supplanted foreign substrate materials due to the extreme conditions required to achieve a stoichiometric GaN melt (temperatures and pressures in excess of 2200°C and 6 GPa, respectively). The only method used to produce bulk GaN on an industrial scale is hydride vapor phase epitaxy (HVPE), but the high cost of gaseous precursors and relatively poor crystal quality have limited the adoption of this technology. A solution growth technique known as the ammonothermal method has attracted interest from academia and industry alike for its ability to produce bulk GaN boules of exceedingly high crystal quality. The ammonothermal method employs supercritical ammonia (NH3) solutions to dissolve, transport, and crystallize GaN. However, ammonothermal growth pressures are still relatively high (˜200 MPa), which has thus far prevented the acquisition of fundamental crystal growth knowledge needed to efficiently (i.e. through data-driven approaches) advance the field. This dissertation focused on addressing the gaps in the literature through two studies employing in situ fluid temperature analysis. The first study focused on identifying the solubility of GaN in supercritical NH3-Na solutions. The design and utilization of in situ and ex situ monitoring equipment enabled the first reports of the two-phase nature of supercritical NH3-Na solutions, and of Ga-alloying of Ni-containing autoclave components. The effects of these error sources on the gravimetric determination of GaN solubility were explored in detail. The second study was aimed at correlating autoclave dissolution and growth zone fluid temperatures with bulk GaN crystal growth kinetics, crystal quality, and impurity incorporation. The insights resulting from this analysis include the identification of the barrier between mass transport and surface integration-limited GaN growth regimes, GaN crystal shape evolution with fluid temperature, the sensitivity of (0001)-orientation crystal quality with fluid temperature, and impurity-specific incorporation activated from the dissolution and growth zones of the autoclave. The results of the aforementioned studies motivated a paradigm-shift in ammonothermal growth. To address this need, a fundamentally different crystal growth approach involving isothermal solutions and tailor-made Group-III alloy source materials was developed/demonstrated. This growth method enabled impurity incorporation reduction compared to traditional ammonothermal GaN growth, and the realization of bulk, ternary Group-III Nitride crystals.

Kinetics of liquid-mediated crystallization of amorphous Ge from multi-frame dynamic transmission electron microscopy

DOE PAGES

Santala, M. K.; Raoux, S.; Campbell, G. H.

2015-12-24

The kinetics of laser-induced, liquid-mediated crystallization of amorphous Ge thin films were studied using multi-frame dynamic transmission electron microscopy (DTEM), a nanosecond-scale photo-emission transmission electron microscopy technique. In these experiments, high temperature gradients are established in thin amorphous Ge films with a 12-ns laser pulse with a Gaussian spatial profile. The hottest region at the center of the laser spot crystallizes in ~100 ns and becomes nano-crystalline. Over the next several hundred nanoseconds crystallization continues radially outward from the nano-crystalline region forming elongated grains, some many microns long. The growth rate during the formation of these radial grains is measuredmore » with time-resolved imaging experiments. Crystal growth rates exceed 10 m/s, which are consistent with crystallization mediated by a very thin, undercooled transient liquid layer, rather than a purely solid-state transformation mechanism. The kinetics of this growth mode have been studied in detail under steady-state conditions, but here we provide a detailed study of liquid-mediated growth in high temperature gradients. Unexpectedly, the propagation rate of the crystallization front was observed to remain constant during this growth mode even when passing through large local temperature gradients, in stark contrast to other similar studies that suggested the growth rate changed dramatically. As a result, the high throughput of multi-frame DTEM provides gives a more complete picture of the role of temperature and temperature gradient on laser crystallization than previous DTEM experiments.« less

Kinetics of liquid-mediated crystallization of amorphous Ge from multi-frame dynamic transmission electron microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Santala, M. K., E-mail: melissa.santala@oregonstate.edu; Campbell, G. H.; Raoux, S.

2015-12-21

The kinetics of laser-induced, liquid-mediated crystallization of amorphous Ge thin films were studied using multi-frame dynamic transmission electron microscopy (DTEM), a nanosecond-scale photo-emission transmission electron microscopy technique. In these experiments, high temperature gradients are established in thin amorphous Ge films with a 12-ns laser pulse with a Gaussian spatial profile. The hottest region at the center of the laser spot crystallizes in ∼100 ns and becomes nano-crystalline. Over the next several hundred nanoseconds crystallization continues radially outward from the nano-crystalline region forming elongated grains, some many microns long. The growth rate during the formation of these radial grains is measured withmore » time-resolved imaging experiments. Crystal growth rates exceed 10 m/s, which are consistent with crystallization mediated by a very thin, undercooled transient liquid layer, rather than a purely solid-state transformation mechanism. The kinetics of this growth mode have been studied in detail under steady-state conditions, but here we provide a detailed study of liquid-mediated growth in high temperature gradients. Unexpectedly, the propagation rate of the crystallization front was observed to remain constant during this growth mode even when passing through large local temperature gradients, in stark contrast to other similar studies that suggested the growth rate changed dramatically. The high throughput of multi-frame DTEM provides gives a more complete picture of the role of temperature and temperature gradient on laser crystallization than previous DTEM experiments.« less

Materials processing in space program tasks

NASA Technical Reports Server (NTRS)

Pentecost, E. (Compiler)

1982-01-01

Active research areas as of the end of the fiscal year 1982 of the Materials Processing in Space Program, NASA-Office of Space and Terrestrial Applications, involving several NASA centers and other organizations are highlighted to provide an overview of the program scope for managers and scientists in industry, university, and government communities. The program is described as well as its history, strategy and overall goal; the organizational structures and people involved are identified and each research task is described together with a list of recent publications. The tasks are grouped into four categories: crystal growth; solidification of metals, alloys, and composites; fluids, transports, and chemical processes; and ultrahigh vacuum and containerless processing technologies.

Phase transitions of amorphous solid acetone in confined geometry investigated by reflection absorption infrared spectroscopy.

PubMed

Shin, Sunghwan; Kang, Hani; Kim, Jun Soo; Kang, Heon

2014-11-26

We investigated the phase transformations of amorphous solid acetone under confined geometry by preparing acetone films trapped in amorphous solid water (ASW) or CCl4. Reflection absorption infrared spectroscopy (RAIRS) and temperature-programmed desorption (TPD) were used to monitor the phase changes of the acetone sample with increasing temperature. An acetone film trapped in ASW shows an abrupt change in the RAIRS features of the acetone vibrational bands during heating from 80 to 100 K, which indicates the transformation of amorphous solid acetone to a molecularly aligned crystalline phase. Further heating of the sample to 140 K produces an isotropic solid phase, and eventually a fluid phase near 157 K, at which the acetone sample is probably trapped in a pressurized, superheated condition inside the ASW matrix. Inside a CCl4 matrix, amorphous solid acetone crystallizes into a different, isotropic structure at ca. 90 K. We propose that the molecularly aligned crystalline phase formed in ASW is created by heterogeneous nucleation at the acetone-water interface, with resultant crystal growth, whereas the isotropic crystalline phase in CCl4 is formed by homogeneous crystal growth starting from the bulk region of the acetone sample.

Fluid mechanics in crystal growth - The 1982 Freeman scholar lecture

NASA Technical Reports Server (NTRS)

Ostrach, S.

1983-01-01

An attempt is made to unify the current state of knowledge in crystal growth techniques and fluid mechanics. After identifying important fluid dynamic problems for such representative crystal growth processes as closed tube vapor transport, open reactor vapor deposition, and the Czochralski and floating zone melt growth techniques, research results obtained to date are presented. It is noted that the major effort to date has been directed to the description of the nature and extent of bulk transport under realistic conditions, where bulk flow determines the heat and solute transport which strongly influence the temperature and concentration fields in the vicinity of the growth interface. Proper treatment of near field, or interface, problems cannot be given until the far field, or global flow, involved in a given crystal growth technique has been adequately described.

Small-Angle Neutron Scattering Investigation of Growth Modifiers on Hydrate Crystal Surfaces

NASA Astrophysics Data System (ADS)

Sun, Thomas; Hutter, Jeffrey L.; Lin, M.; King, H. E., Jr.

1998-03-01

Hydrates are crystals consisting of small molecules enclathrated within an ice-like water cage. Suppression of their growth is important in the oil industry. The presence of small quantities of specific polymers during hydrate crystallization can induce a transition from an octahedral to planar growth habit. This symmetry breaking is surprising because of the suppression of two 111 planes relative to the other six crystallographically equivalent faces. To better understand the surface effects leading to this behavior, we have studied the surface adsorption of these growth-modifing polymers onto the hydrate crytals using SANS. The total hydrate surface area, as measured by Porod scattering, increases in the presence of the growth modifier, but, no significant increase in polymer concentration on the crystal surfaces is found. Implications for possible growth mechanisms will be discussed.

Protein Crystallization by Combining Laser Irradiation and Solution-Stirring Techniques

NASA Astrophysics Data System (ADS)

Adachi, Hiroaki; Niino, Ai; Murakami, Satoshi; Takano, Kazufumi; Matsumura, Hiroyoshi; Kinoshita, Takayoshi; Warizaya, Masaichi; Inoue, Tsuyoshi; Mori, Yusuke; Sasaki, Takatomo

2005-03-01

Bovine adenosine deaminase in the absence of an inhibitor (free-ADA) does not form crystals when using conventional crystallization methods. Using a solution-stirring technique, we recently succeeded in generating a small number of free-ADA crystals. In this paper, we demonstrate the combination of laser-irradiated growth and stirring (COLAS). This technique was found to be useful for controlling crystal nucleation and growth, which led to the production of a much larger number of high-quality free-ADA crystals.

Microgravity

NASA Image and Video Library

1992-02-21

Vapor Crystal Growth System developed in IML-1, Mercuric Iodide Crystal grown in microgravity FES/VCGS (Fluids Experiment System/Vapor Crystal Growth Facility). During the mission, mercury iodide source material was heated, vaporized, and transported to a seed crystal where the vapor condensed. Mercury iodide crystals have practical uses as sensitive X-ray and gamma-ray detectors. In addition to their excellent optical properties, these crystals can operate at room temperature, which makes them useful for portable detector devices for nuclear power plant monitoring, natural resource prospecting, biomedical applications, and astronomical observing.

Effects of Convective Solute and Impurity Transport in Protein Crystal Growth

NASA Technical Reports Server (NTRS)

Vekilov, Peter G.; Thomas, Bill R.; Rosenberger, Franz

1998-01-01

High-resolution optical interferometry was used to investigate the effects of forced solution convection on the crystal growth kinetics of the model protein lysozyme. Most experiments were conducted with 99.99% pure protein solutions. To study impurity effects, approx. 1% of lysozyme dimer (covalently bound) was added in some cases. We show that the unsteady kinetics, corresponding to bunching of growth steps, can be characterized by the Fourier components of time traces of the growth rate. Specific Fourier spectra are uniquely determined by the solution conditions (composition, temperature, and flow rate) and the growth layer source activity. We found that the average step velocity and growth rate increase by approx. I0% with increasing flow rate, as a result of the enhanced solute supply to the interface. More importantly, faster convective transport results in lower fluctuation amplitudes. This observation supports our rationale for system-dependent effects of transport on the structural perfection of protein crystals. We also found that solution flow rates greater than 500 microns/s result in stronger fluctuations while the average growth rate is decreased. This can lead to growth cessation at low supersaturations. With the intentionally contaminated solutions, these undesirable phenomena occurred at about half the flow rates required in pure solutions. Thus, we conclude that they are due to enhanced convective supply of impurities that are incorporated into the crystal during growth. Furthermore, we found that the impurity effects are reduced at higher crystal growth rates. Since the exposure time of terraces is inversely proportional to the growth rate, this observation suggests that the increased kinetics instability results from impurity adsorption on the interface. Finally, we provide evidence relating earlier observations of "slow protein crystal growth kinetics" to step bunch formation in response to nonsteady step generation.

Experimental and quantum chemical studies of a new organic proton transfer compound, 1H-imidazole-3-ium-3-hydroxy-2,4,6-trinitrophenolate

NASA Astrophysics Data System (ADS)

Dhamodharan, P.; Sathya, K.; Dhandapani, M.

2018-02-01

A new proton transfer compound, 1H-imidazole-3-ium-3-hydroxy-2,4,6-trinitrophenolate (IMHTP), was crystallized by slow evaporation-solution growth technique. 1H and 13C NMR spectral studies confirm the molecular structure of the grown crystal. Single crystal X-ray diffraction study confirms that IMHTP crystallizes in monoclinic system with space group P21/c. Thermal curves (TG/DTA) show that the material is thermally stable up to 198 °C. The crystal emits fluorescence at 510 nm, proving its utility in making green light emitting materials in optical applications. The stable molecular structure was optimized by Gaussian 09 program with B3LYP/6-311++G(d,p) level of basis set. The frontier molecular orbital study shows that the charge transfer interaction occurs within the complex. The calculated first-order hyperpolarizability value of IMHTP is 44 times higher than that the reference material, urea. The electrostatic potential map was used to probe into electrophilic and nucleophilic reactive sites present in the molecule.

Economic analysis of crystal growth in space

NASA Technical Reports Server (NTRS)

Ulrich, D. R.; Chung, A. M.; Yan, C. S.; Mccreight, L. R.

1972-01-01

Many advanced electronic technologies and devices for the 1980's are based on sophisticated compound single crystals, i.e. ceramic oxides and compound semiconductors. Space processing of these electronic crystals with maximum perfection, purity, and size is suggested. No ecomonic or technical justification was found for the growth of silicon single crystals for solid state electronic devices in space.

Devitrification and delayed crazing of SiO2 on single-crystal silicon and chemically vapor-deposited silicon nitride

NASA Technical Reports Server (NTRS)

Choi, Doo Jin; Scott, William D.

1987-01-01

The linear growth rate of cristobalite was measured in thin SiO2 films on silicon and chemically vapor-deposited silicon nitride. The presence of trace impurities from alumina furnace tubes greatly increased the crystal growth rate. Under clean conditions, the growth rate was still 1 order-of-magnitude greater than that for internally nucleated crystals in bulk silica. Crystallized films cracked and lifted from the surface after exposure to atmospheric water vapor. The crystallization and subsequent crazing and lifting of protective SiO2 films on silicon nitride should be considered in long-term applications.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Junjie; Zheng, Hong; Ren, Yang

We report the first single crystal growth of the correlated metal LaNiO 3 using a high-pressure optical-image floating zone furnace. The crystals were studied using single crystal/powder X-ray diffraction, resistivity, specific heat, and magnetic susceptibility. The availability of bulk LaNiO 3 crystals will (i) promote deep understanding in this correlated material, including the mechanism of enhanced paramagnetic susceptibility, and (ii) provide rich opportunities as a substrate for thin film growth such as important ferroelectric and/or multiferroic materials. As a result, this study demonstrates the power of high pO 2 single crystal growth of nickelate perovskites and correlated electron oxides moremore » generally.« less

Rotating lattice single crystal architecture on the surface of glass

DOE PAGES

Savytskii, D.; Jain, H.; Tamura, N.; ...

2016-11-03

Defying the requirements of translational periodicity in 3D, rotation of the lattice orientation within an otherwise single crystal provides a new form of solid. Such rotating lattice single (RLS) crystals are found, but only as spherulitic grains too small for systematic characterization or practical application. Here we report a novel approach to fabricate RLS crystal lines and 2D layers of unlimited dimensions via a recently discovered solid-to-solid conversion process using a laser to heat a glass to its crystallization temperature but keeping it below the melting temperature. The proof-of-concept including key characteristics of RLS crystals is demonstrated using the examplemore » of Sb 2S 3 crystals within the Sb-S-I model glass system for which the rotation rate depends on the direction of laser scanning relative to the orientation of initially formed seed. Lattice rotation in this new mode of crystal growth occurs upon crystallization through a well-organized dislocation/disclination structure introduced at the glass/ crystal interface. Implications of RLS growth on biomineralization and spherulitic crystal growth are noted.« less

Top-seeded solution growth and morphology change of RbTiOPO4:Ta single crystal

NASA Astrophysics Data System (ADS)

Li, Ziqing; Chen, Yang; Zhu, Pengfei; Ji, Nianjing; Duan, Xiulan; Jiang, Huaidong

2018-04-01

The RbTiOPO4:Ta single crystal with dimensions of 4 mm × 31 mm × 18 mm was successfully grown by Top Seeded Solution Growth Technique. It is concluded that the doping Ta element can strongly influence the growth and morphology of the RbTiOPO4 crystal. The evident morphology change of RbTiOPO4:Ta crystal with respect to RbTiOPO4 crystal has been observed and the (1 0 0) crystal face was more developed than any other crystal faces. The possible reasons of the morphology change were analyzed through experimental and theoretical methods. Several methods were tried to increase crystallographic a direction dimension of RbTiOPO4:Ta crystals. Finally, the RbTiOPO4:Ta single crystal with crystallographic a direction dimension up to 6 mm was obtained by using thicker seed crystal. This way makes it possible to get isometric RbTiOPO4:Ta crystals, which is beneficial for nonlinear optical applications due to larger area in x-y plane.

Single crystal growth of spin-ladder compound La8Cu7O19 by the travelling-solvent floating zone method

NASA Astrophysics Data System (ADS)

Mohan, A.; Singh, S.; Partzsch, S.; Zwiebler, M.; Geck, J.; Wurmehl, S.; Büchner, B.; Hess, C.

2016-08-01

Large single crystals of La8Cu7O19 have been grown using the travelling-solvent floating zone method. A rather high oxygen pressure of 9 bar in the growth chamber and a slow growth speed of 0.5 mm/h were among the most important parameters in stabilizing the growth of this incongruently melting compound. Interestingly, a novel growth scenario has been witnessed. The crystal structure of the grown La8Cu7O19 crystal has been analyzed using single crystal diffractometry to extract important structural parameters of this compound. We find that La8Cu7O19 crystallizes in a monoclinic structure with space group C 2 / c and has the lattice parameters a ≈ 13.83 Å, b ≈ 3.75 Å, c ≈ 34.59 Å, and β ≈ 99.33 °, in good agreement with the data obtained on polycrystalline samples in the literature. The magnetization shows a highly anisotropic behavior, and an anomaly at T ≈103 K.

Characterization and inhibitive study of gel-grown hydroxyapatite crystals at physiological temperature

NASA Astrophysics Data System (ADS)

Parekh, Bharat; Joshi, Mihir; Vaidya, Ashok

2008-04-01

Hydroxyapatite is very useful for various biomedical applications, due to its chemical similarity with mineralized bone of human. Hydroxyapatite is also responsible for arthropathy (joint disease). In the present study, the growth of hydroxyapatite crystals was carried out by using single-diffusion gel growth technique in silica hydro gel media, at physiological temperature. The growth of hydroxyapatite crystals under slow and controlled environment in gel medium can be simulated in a simple manner to the growth in human body. The crystals, formed in the Liesegang rings, were characterized by powder XRD, FTIR and dielectric study. The diffusion study is also carried out for the hydroxyapatite crystals using the moving boundary model. The inhibitive influence of various Ayurvedic medicinal plant extracts such as Boswellia serrata gum resin , Tribulus terrestris fruits, Rotula aquatica roots, Boerhaavia diffusa roots and Commiphora wightii, on the growth of hydroxyapatite was studied. Roots of R. aquatica and B. diffusa show some inhibition of the hydroxyapatite crystals in vitro. This preclinical study will be helpful to design the therapy for prevention of hydroxyapatite-based ailments.

Simulation of Gravity Effects on Bulk Crystal Growth with Effects on undercooling

NASA Astrophysics Data System (ADS)

Chuang, S.-H.; Lu, M.-F.

For the production of a perfect single crystal by Bridgman, it is important to acquire the correct information about the heat transfer mechanism and to control the heat transfer in the Bridgman furnace. Because the quality of the crystal is closely related to its thermal history and the transport phenomena in the furnace. Ma et al. (2004) presented that faceting simulation of bulk crystal growth with undercooling method. Lan et al. (2003) developed a new model to study heat flow and facet formation in Bridgman growth with the undercooling satisfied the given growth mechanism. Considering the gravity effects added kinetic undercooling is thus developed. Heat conduction, convection and radiation are considered and coupled with the two-dimensional transient undercooling simulation. The solidification interface temperature is related to the undercooling along the interface and the melting temperature. In this investigation, we are going to apply the developed model to simulate interface in vertical Bridgman crystal growth process for yttrium aluminum garnet subjected to the normal gravity to microgravity. Also, it discusses the effect upon the shape and the propagation of the solidification crystal front.

Solvent effects and polymorphic transformation of organic nonlinear optical crystal L-pyroglutamic acid in solution growth processes . I. Solvent effects and growth morphology

NASA Astrophysics Data System (ADS)

Wang, W. S.; Aggarwal, M. D.; Choi, J.; Gebre, T.; Shields, Angela D.; Penn, Benjamin G.; Frazier, Donald O.

1999-03-01

Single crystals of a new promising nonlinear optical material for the tunable UV harmonic generation, L-pyroglutamic acid 60×20×20 mm 3 in size were obtained from aqueous solution by using the temperature-lowering method. Solubility of L-pyroglutamic acid in different solvents was measured. The single crystals showed different morphological characteristics and growth rate in different solvents with different crystallographic orientations. Methanol or ethanol solutions yielded needle-like crystals. In mixed solution such as methanol/H 2O or ethanol/ H 2O plate-like crystals with a thickness in the direction [0 1 0] were observed. The water as a good solvent, however, produced long prism-like crystals. The two polymorphs of L-pyroglutamic acid (α and β phases) were found for the first time. The growth shapes of α-phase is mainly a prism and β phases is a rhombic plate.The growth rate of α and β phases is mainly a function of the supersaturation of the L-pyroglutamic acid in solution.

Supercritical fluid crystallization of griseofulvin: crystal habit modification with a selective growth inhibitor.

PubMed

Jarmer, Daniel J; Lengsfeld, Corinne S; Anseth, Kristi S; Randolph, Theodore W

2005-12-01

Poly (sebacic anhydride) (PSA) was used as a growth inhibitor to selectively modify habit of griseofulvin crystals formed via the Precipitation with a compressed-fluid antisolvent (PCA) process. PSA and griseofulvin were coprecipitated within a PCA injector, which provided efficient mixing between the solution and compressed antisolvent process streams. Griseofulvin crystal habit was modified from acicular to bipyramidal when the mass ratio of PSA/griseofulvin in the solution feed stream was

Containerless protein crystal growth technology: Electrostatic multidrop positioner

NASA Technical Reports Server (NTRS)

Rhim, Won-Kyu

1990-01-01

A brief discussion of containerless protein crystal growth in space and a diagram of the electrostatic multidrop positioner are presented. A picture of lysome crystals growing in a drop and a graph of levitation voltage versus time (minutes) are also presented.

A 4-D dataset for validation of crystal growth in a complex three-phase material, ice cream

NASA Astrophysics Data System (ADS)

Rockett, P.; Karagadde, S.; Guo, E.; Bent, J.; Hazekamp, J.; Kingsley, M.; Vila-Comamala, J.; Lee, P. D.

2015-06-01

Four dimensional (4D, or 3D plus time) X-ray tomographic imaging of phase changes in materials is quickly becoming an accepted tool for quantifying the development of microstructures to both inform and validate models. However, most of the systems studied have been relatively simple binary compositions with only two phases. In this study we present a quantitative dataset of the phase evolution in a complex three-phase material, ice cream. The microstructure of ice cream is an important parameter in terms of sensorial perception, and therefore quantification and modelling of the evolution of the microstructure with time and temperature is key to understanding its fabrication and storage. The microstructure consists of three phases, air cells, ice crystals, and unfrozen matrix. We perform in situ synchrotron X-ray imaging of ice cream samples using in-line phase contrast tomography, housed within a purpose built cold-stage (-40 to +20oC) with finely controlled variation in specimen temperature. The size and distribution of ice crystals and air cells during programmed temperature cycling are determined using 3D quantification. The microstructural evolution of three-phase materials has many other important applications ranging from biological to structural and functional material, hence this dataset can act as a validation case for numerical investigations on faceted and non-faceted crystal growth in a range of materials.

Face-by-face growth of sucrose crystals from aqueous solutions in the presence of raffinose—II: Growth morphology and segregation

NASA Astrophysics Data System (ADS)

Sgualdino, G.; Aquilano, D.; Pastero, L.; Vaccari, G.

2007-10-01

Raffinose segregation into sucrose crystals is experimentally determined along with the modifications of the quantitative sucrose growth morphology, which are in turn related to the different growth conditions. ( Craff, σ) morphodromes nicely represent the conflict between the supersaturation and the raffinose concentration in the solution on the growth morphology, while the overall segregation rate is nearly proportional to the linear overall crystal growth rate. Chernov and Burton-Prim-Slichter models, checked to fit our keff and ln(keff-1-1) coefficients as a function of the supersaturation and of the mean linear overall growth rate, do not allow to know whether the segregation occurs either by a process dominated by surface integration, or by additive transfer dominated by volume diffusion within the boundary layer. The distribution of segregated raffinose strictly depends on the { h k l} growth sectors and doped crystals contain deformed lattice zones, as it comes out from X-ray powder diagrams.

Structural Characterization of Lateral-grown 6H-SiC am-plane Seed Crystals by Hot Wall CVD Epitaxy

NASA Technical Reports Server (NTRS)

Goue, Ouloide Yannick; Raghothamachar, Balaji; Dudley, Michael; Trunek, Andrew J.; Neudeck, Philip G.; Woodworth, Andrew A.; Spry, David J.

2014-01-01

The performance of commercially available silicon carbide (SiC) power devices is limited due to inherently high density of screw dislocations (SD), which are necessary for maintaining polytype during boule growth and commercially viable growth rates. The NASA Glenn Research Center (GRC) has recently proposed a new bulk growth process based on axial fiber growth (parallel to the c-axis) followed by lateral expansion (perpendicular to the c-axis) for producing multi-faceted m-plane SiC boules that can potentially produce wafers with as few as one SD per wafer. In order to implement this novel growth technique, the lateral homoepitaxial growth expansion of a SiC fiber without introducing a significant number of additional defects is critical. Lateral expansion is being investigated by hot wall chemical vapor deposition (HWCVD) growth of 6H-SiC am-plane seed crystals (0.8mm x 0.5mm x 15mm) designed to replicate axially grown SiC single crystal fibers. The post-growth crystals exhibit hexagonal morphology with approximately 1500 m (1.5 mm) of total lateral expansion. Preliminary analysis by synchrotron white beam x-ray topography (SWBXT) confirms that the growth was homoepitaxial, matching the polytype of the respective underlying region of the seed crystal. Axial and transverse sections from the as grown crystal samples were characterized in detail by a combination of SWBXT, transmission electron microscopy (TEM) and Raman spectroscopy to map defect types and distribution. X-ray diffraction analysis indicates the seed crystal contained stacking disorders and this appears to have been reproduced in the lateral growth sections. Analysis of the relative intensity for folded transverse acoustic (FTA) and optical (FTO) modes on the Raman spectra indicate the existence of stacking faults. Further, the density of stacking faults is higher in the seed than in the grown crystal. Bundles of dislocations are observed propagating from the seed in m-axis lateral directions. Contrast extinction analysis of these dislocation lines reveals they are edge type basal plane dislocations that track the growth direction. Polytype phase transition and stacking faults were observed by high-resolution TEM (HRTEM), in agreement with SWBXT and Raman scattering.

A parametric study of segregation effects during vertical Bridgman crystal growth with an axial magnetic field

NASA Astrophysics Data System (ADS)

Ma, N.; Walker, J. S.

2000-01-01

This paper presents a model for the unsteady transport of a dopant during the vertical Bridgman crystal growth process with a planar crystal-melt interface and with an axial magnetic field, and investigates the effects of varying different process variables on the crystal composition. The convective mass transport due to the buoyant convection in the melt produces nonuniformities in the concentration in both the melt and the crystal. The convective mass transport plays an important role for all magnetic field strengths considered. Diffusive mass transport begins to dominate for a magnetic flux density of 4 T and a fast growth rate, producing crystals which have an axial variation of the radially averaged crystal composition approaching that of the diffusion-controlled limit. Dopant distributions for several different combinations of process parameters are presented.

Large-volume protein crystal growth for neutron macromolecular crystallography

DOE PAGES

Ng, Joseph D.; Baird, James K.; Coates, Leighton; ...

2015-03-30

Neutron macromolecular crystallography (NMC) is the prevailing method for the accurate determination of the positions of H atoms in macromolecules. As neutron sources are becoming more available to general users, finding means to optimize the growth of protein crystals to sizes suitable for NMC is extremely important. Historically, much has been learned about growing crystals for X-ray diffraction. However, owing to new-generation synchrotron X-ray facilities and sensitive detectors, protein crystal sizes as small as in the nano-range have become adequate for structure determination, lessening the necessity to grow large crystals. Here, some of the approaches, techniques and considerations for themore » growth of crystals to significant dimensions that are now relevant to NMC are revisited. We report that these include experimental strategies utilizing solubility diagrams, ripening effects, classical crystallization techniques, microgravity and theoretical considerations.« less

Large-volume protein crystal growth for neutron macromolecular crystallography

PubMed Central

Ng, Joseph D.; Baird, James K.; Coates, Leighton; Garcia-Ruiz, Juan M.; Hodge, Teresa A.; Huang, Sijay

2015-01-01

Neutron macromolecular crystallography (NMC) is the prevailing method for the accurate determination of the positions of H atoms in macromolecules. As neutron sources are becoming more available to general users, finding means to optimize the growth of protein crystals to sizes suitable for NMC is extremely important. Historically, much has been learned about growing crystals for X-ray diffraction. However, owing to new-generation synchrotron X-ray facilities and sensitive detectors, protein crystal sizes as small as in the nano-range have become adequate for structure determination, lessening the necessity to grow large crystals. Here, some of the approaches, techniques and considerations for the growth of crystals to significant dimensions that are now relevant to NMC are revisited. These include experimental strategies utilizing solubility diagrams, ripening effects, classical crystallization techniques, microgravity and theoretical considerations. PMID:25849493

Large-volume protein crystal growth for neutron macromolecular crystallography

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ng, Joseph D.; Baird, James K.; Coates, Leighton

Neutron macromolecular crystallography (NMC) is the prevailing method for the accurate determination of the positions of H atoms in macromolecules. As neutron sources are becoming more available to general users, finding means to optimize the growth of protein crystals to sizes suitable for NMC is extremely important. Historically, much has been learned about growing crystals for X-ray diffraction. However, owing to new-generation synchrotron X-ray facilities and sensitive detectors, protein crystal sizes as small as in the nano-range have become adequate for structure determination, lessening the necessity to grow large crystals. Here, some of the approaches, techniques and considerations for themore » growth of crystals to significant dimensions that are now relevant to NMC are revisited. We report that these include experimental strategies utilizing solubility diagrams, ripening effects, classical crystallization techniques, microgravity and theoretical considerations.« less

Growth of sodium chlorate crystals in the presence of potassium sulphate

NASA Astrophysics Data System (ADS)

Kim, E. L.; Tsyganova, A. A.; Vorontsov, D. A.; Ovsetsina, T. I.; Katkova, M. R.; Lykov, V. A.; Portnov, V. N.

2015-09-01

In this work, we investigated the morphology and growth rates of NaClO3 crystals in solutions with K2SO4 additives. NaClO3 crystals were grown using the temperature gradient technique under concentration convection. We found that the crystal habitus changed from cubic to tetrahedral, and the growth of the cubic {100}, tetrahedral {111} and rhomb-dodecahedral {110} faces decelerated with an increase in the concentration of SO42- ions. The {110} face was the most and the {100} face was the least inhibited by sulphate ions. The mechanism of SO42- ions action is their adsorption on the crystal surface, which impedes attachment of the crystal's building units. We conclude that different atomic structure and charge state of various crystal faces determine their sensitivity to the action of the SO42- ions.

Crystal Growth of ZnSe and Related Ternary Compound Semiconductors by Physical Vapor Transport

NASA Technical Reports Server (NTRS)

Cushman, Paula P.

1997-01-01

Preliminary definition of all of the necessary materials, labor, services, and facilities necessary to provide science requirement definition, initiate hardware development activities, and provide an update flight program proposal consistent with the NRA selection letter. The major tasks identified in this SOW are in the general category of science requirements determination, instrument definition, and updated flight program proposal. The Contractor shall define preliminary management, technical and integration requirements for the program, including improved cost/schedule estimates. The Contractor shall identify new technology requirements, define experiment accommodations and operational requirements and negotiate procurement of any long lead items, if required, with the government.

Crystal Growth of ZnSe and Related Ternary Compound Semiconductors by Physical Vapor Transport

NASA Technical Reports Server (NTRS)

Su, Ching-Hua

1997-01-01

Preliminary definition of all of the necessary materials, labor, services, and facilities necessary to provide science requirement definition, initiate hardware development activities, and provide an updated flight program proposal consistent with the NRA selection letter. The major tasks identified in this SOW are in the general category of science requirements determination, instrument definition, and updated flight program proposal. The Contractor shall define preliminary management, technical and integration requirements for the program, including improved cost/schedule estimates. The Contractor shall identify new technology requirements, define experiment accommodations and operational requirements and negotiate procurement of any long lead items, if required, with the government.

The Growth of Berlinite (AlPO4) Single Crystals.

DTIC Science & Technology

1980-03-01

Solubility of AlPO 4 18 6. Solubility Data of Jahn and Kordes on AlPO4 19 7. AlPO 4 Seed Crystal 23 8. Tem-Pres Hydrothermal Research Unit 25 9...Since the vapor pressure of water rises rapidly with temperature, a closed hydrothermal system was used. In a seeded hydrothermal growth process, the...to investigate the hydrothermal growth of Berlinite (AlPO4 ) to determine the optimum growth conditions for large high quality crystals. Over thirty

Growth of LiNbO{sub 3}:Er Crystals and concentration dependences of their properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Palatnikov, M. N., E-mail: palat-mn@chemy.kolasc.net.ru; Biryukova, I. V.; Shcherbina, O. B.

2016-11-15

A series of lithium niobate (LiNbO{sub 3}) crystals of congruent and stoichiometric compositions, doped with erbium, have been grown under non-steady-state thermal conditions. A series of LiNbO{sub 3}:Zn crystals, nominally pure LiNbO{sub 3} crystals of congruent and stoichiometric compositions, and a LiNbO{sub 3}:B crystal have also been grown. Both growth conditions and concentration dependences of physicochemical, ferroelectric, and structural characteristics of LiNbO{sub 3}:Er crystals are investigated. The growth regular domain microstructures and periodic nanostructures in LiNbO{sub 3}:Er crystals are analyzed by optical microscopy and atomic force microscopy (AFM). A comparative study of the optical homogeneity and photorefractive properties of LiNbO{submore » 3}:Er crystals of congruent and stoichiometric compositions and the Raman spectra of LiNbO{sub 3} crystals of different compositions is performed.« less

Preparation and Analysis of RNA Crystals

NASA Technical Reports Server (NTRS)

Todd, Paul

2000-01-01

The crystallization of RiboNucleic Acids (RNA) was studied from the standpoint of mechanisms of crystal growth in three tasks: (1) preparation of high-quality crystals of oligonuclotides for X-ray diffraction, (2) finding pathways to the growth of high-quality crystals for X-ray diffraction and (3) investigation of mechanisms of action of inertial acceleration on crystal growth. In these tasks: (1) RNA crystals were prepared and studied by X-ray diffraction; (2) a pathway to high-quality crystals was discovered and characterized; a combination of kinetic and equilibrium factors could be optimized as described below; and (3) an interplay between purity and gravity was found in a combination of space and ground experiments with nucleic acids and proteins. Most significantly, the rate of concentration of precipitant and RNA can be controlled by membrane-based methods of water removal or by diffusion of multivalent cations across an interface stabilized by a membrane. Oligonucleotide solutions are electrokinetically stabilized colloids, and crystals can form by the controlled addition of multivalent cations.

Rotating Vessels for Growing Protein Crystals

NASA Technical Reports Server (NTRS)

Cottingham, Paul

2005-01-01

Rotating vessels have been proposed as means of growing larger, more nearly uniform protein crystals than would otherwise be possible in the presence of normal Earth gravitation. Heretofore, nonrotating vessels have been used. It is difficult to grow high-quality protein crystals in the terrestrial gravitational field because of convection plumes created by the interaction between gravitation and density gradients in protein-solution depletion layers around growing crystals. The density gradients and the associated convection plumes cause the surfaces of growing crystals to be exposed to nonuniform solution densities, thereby causing the crystals to form in irregular shapes. The microgravitational environment of outer space has been utilized to eliminate gravitation-induced convection, but this approach is generally not favorable because of the high cost and limited availability of space flight. The use of a rotating vessel according to the proposal is intended to ameliorate the effects of gravitation and the resultant convection, relative to the corresponding effects in a non-rotating vessel. The rotation would exert an averaging effect over time, distributing the convective force on the depletion layer. Therefore, the depletion layer would be more nearly uniform and, as a result, the growing crystal would be more nearly perfect. The proposal admits of variations (see figure), including the following: The growing crystal could be rotated about its own central axis or an external axis. The crystal-growth vessel could be of any of various shapes, including cylindrical, hemispherical, conical, and combinations thereof. The crystal-growth vessel could be suspended in a viscous fluid in an outer vessel to isolate the growing crystal from both ambient vibrations and vibrations induced by a mechanism that drives the rotation. The rotation could be coupled to the crystal-growth vessel by viscous or magnetic means. The crystal-growth vessel could be supported within the outer vessel by use of a magnetic field. The crystal-growth vessel and the outer vessel could be configured in a variety of ways to facilitate heat transfer, instrumentation, and rotation.

Elemental and cooperative diffusion in a liquid, supercooled liquid and glass resolved

NASA Astrophysics Data System (ADS)

Cassar, Daniel R.; Lancelotti, Ricardo F.; Nuernberg, Rafael; Nascimento, Marcio L. F.; Rodrigues, Alisson M.; Diz, Luiza T.; Zanotto, Edgar D.

2017-07-01

The diffusion mechanisms controlling viscous flow, structural relaxation, liquid-liquid phase separation, crystal nucleation, and crystal growth in multicomponent glass-forming liquids are of great interest and relevance in physics, chemistry, materials, and glass science. However, the diffusing entities that control each of these important dynamic processes are still unknown. The main objective of this work is to shed some light on this mystery, advancing the knowledge on this phenomenon. For that matter, we measured the crystal growth rates, the viscosity, and lead diffusivities in PbSiO3 liquid and glass in a wide temperature range. We compared our measured values with published data covering 16 orders of magnitude. We suggest that above a certain temperature range Td (1.2Tg-1.3Tg), crystal growth and viscous flow are controlled by the diffusion of silicon and lead. Below this temperature, crystal growth and viscous flow are more sluggish than the diffusion of silicon and lead. Therefore, Td marks the temperature where decoupling between the (measured) cationic diffusivity and the effective diffusivities calculated from viscosity and crystal growth rates occurs. We reasonably propose that the nature or size of the diffusional entities controlling viscous flow and crystal growth below Td is quite different; the slowest is the one controlling viscous flow, but both processes require cooperative movements of some larger structural units rather than jumps of only one or a few isolated atoms.

Containerless crystallization of silicon

NASA Astrophysics Data System (ADS)

Kuribayashi, K.; Aoyama, T.

2002-04-01

Crystallization from undercooled melt of silicon was carried out by means of electro-magnetic levitation method under controlled undercooling. The measured growth rate vs. undercooling was categorized into three regions, I, II and III, respectively, from the point of the interface morphology. Thin plate crystals whose interface consisted of both faceted (1 1 1) plane and wavy edge plane like saw-tooth were observed in the region I where the undercooling is less than 100 K. The growth rate of the wavy edge plane was well described by the dendrite growth model. The morphology of growing crystals was abruptly changed to faceted dendrite in the region II, though there was no abrupt change in the growth rate. Seeding at temperatures in the region I changes the drop to a mono-crystalline sphere, if the growth rate along the normal direction of the thin plate crystal is controlled by step-wise growth on the faceted plane. Actually, the sample of 5 mm in diameter seeded at undercooling of 26 K was a quasi-single crystal with large grain, except for a small area where twinning and cracking are observed. The result suggests that the single crystal could be grown, if a smaller sample, 1 or 2 mm in diameter, that is difficult to be levitated by electro-magnetic force were processed with other methods such as free fall in a drop tube.

Magnetic field controlled floating-zone single crystal growth of intermetallic compounds

NASA Astrophysics Data System (ADS)

Hermann, R.; Gerbeth, G.; Priede, J.

2013-03-01

Radio-frequency (RF) floating zone single crystal growth is an important technique for the preparation of single bulk crystals. The advantage of the floating-zone method is the crucible-free growth of single crystals of reactive materials with high melting points. The strong heat diffusion on the surface, as well as the melt convection in the molten zone due to induction heating, often leads to an undesired solid-liquid interface geometry with a concave (towards the solid phase) outer rim. These concave parts aggravate the single crystal growth over the full cross-section. A two-phase stirrer was developed at IFW Dresden in order to avoid the problems connected with these concave parts. It acts as a magnetic field pump and changes the typical double vortex structure to a single roll structure, thus pushing hot melt into the regions where the concave parts may arise. The current in the secondary coil is induced by the primary coil, and the capacitor and the resistance of the secondary circuit are adjusted to get a stable 90 degree phase-shift between the coil currents. Single crystal growth of industrial relevant RuAl and TiAl intermetallic compounds was performed based on the material parameters and using the adjusted two-phase stirrer. Very recently, the magnetic system was applied to the crystal growth of biocompatible TiNb alloys and antiferromagnetic Heusler MnSi compounds.