The low thermal gradient CZ technique as a way of growing of dislocation-free germanium crystals

NASA Astrophysics Data System (ADS)

Moskovskih, V. A.; Kasimkin, P. V.; Shlegel, V. N.; Vasiliev, Y. V.; Gridchin, V. A.; Podkopaev, O. I.

2014-09-01

This paper considers the possibility of growth of dislocation-free germanium single crystals. This is achieved by reducing the temperature gradients at the level of 1 K/cm and lower. Single germanium crystals 45-48 mm in diameter with a dislocation density of 102 cm-2 were grown by a Low Thermal Gradient Czochralski technique (LTG CZ).

Single Crystal Membranes

NASA Technical Reports Server (NTRS)

Stormont, R. W.; Morrison, A.

1974-01-01

Single crystal a- and c-axis tubes and ribbons of sodium beta-alumina and sodium magnesium beta-alumina were grown from sodium oxide rich melts. Additional experiments grew ribbon crystals containing sodium magnesium beta, beta double prime, beta triple prime, and beta quadruple prime. A high pressure crystal growth chamber, sodium oxide rich melts, and iridium for all surfaces in contact with the melt were combined with the edge-defined, film-fed growth technique to grow the single crystal beta-alumina tubes and ribbons. The crystals were characterized using metallographic and X-ray diffraction techniques, and wet chemical analysis was used to determine the sodium, magnesium, and aluminum content of the grown crystals.

(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.

Microgravity

NASA Image and Video Library

1995-09-17

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.

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.

Macromolecular Crystallization in Microgravity

NASA Technical Reports Server (NTRS)

Snell, Edward H.; Helliwell, John R.

2004-01-01

The key concepts that attracted crystal growers, macromolecular or solid state, to microgravity research is that density difference fluid flows and sedimentation of the growing crystals are greatly reduced. Thus, defects and flaws in the crystals can be reduced, even eliminated, and crystal volume can be increased. Macromolecular crystallography differs from the field of crystalline semiconductors. For the latter, crystals are harnessed for their electrical behaviors. A crystal of a biological macromolecule is used instead for diffraction experiments (X-ray or neutron) to determine the three-dimensional structure of the macromolecule. The better the internal order of the crystal of a biological macromolecule then the more molecular structure detail that can be extracted. This structural information that enables an understanding of how the molecule functions. This knowledge is changing the biological and chemical sciences with major potential in understanding disease pathologies. Macromolecular structural crystallography in general is a remarkable field where physics, biology, chemistry, and mathematics meet to enable insight to the basic fundamentals of life. In this review, we examine the use of microgravity as an environment to grow macromolecular crystals. We describe the crystallization procedures used on the ground, how the resulting crystals are studied and the knowledge obtained from those crystals. We address the features desired in an ordered crystal and the techniques used to evaluate those features in detail. We then introduce the microgravity environment, the techniques to access that environment, and the theory and evidence behind the use of microgravity for crystallization experiments. We describe how ground-based laboratory techniques have been adapted to microgravity flights and look at some of the methods used to analyze the resulting data. Several case studies illustrate the physical crystal quality improvements and the macromolecular structural advances. Finally, limitations and alternatives to microgravity and future directions for this research are covered.

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.

Synthesis, growth and characterization of 3-nitroacetanilide—A new organic nonlinear optical crystal by Bridgman technique

NASA Astrophysics Data System (ADS)

Lenin, M.; Ramasamy, P.

2008-10-01

Single crystals of 3-nitroacetanilide, an organic nonlinear optical material has been grown by the Bridgman-Stockbarger method. The single crystal X-ray diffraction (XRD) data revealed the noncentrosymmetric crystal structure, which is an essential criterion for second harmonic generation. The crystalline nature of the grown crystals was confirmed using powder XRD techniques. The functional group of the compound is identified by FTIR spectrum. The thermal stability and its tendency to grow as single crystal in solution and in melt have been identified for the new title compound. The UV-vis spectrum of mNAA shows the lower optical cut off at 400 nm and was transparent in the visible region. The second harmonic generation efficiency was found using Kurtz powder technique. The dielectric constant and dielectric loss of the crystal were measured as a function of frequency and temperature, and the results are discussed.

Development of single crystal membranes

NASA Technical Reports Server (NTRS)

Stormont, R. W.; Cocks, F. H.

1972-01-01

The design and construction of a high pressure crystal growth chamber was accomplished which would allow the growth of crystals under inert gas pressures of 2 MN/sq m (300 psi). A novel crystal growth technique called EFG was used to grow tubes and rods of the hollandite compounds, BaMgTi7O16, K2MgTi7O16, and tubes of sodium beta-alumina, sodium magnesium-alumina, and potassium beta-alumina. Rods and tubes grown are characterized using metallographic and X-ray diffraction techniques. The hollandite compounds are found to be two or three-phase, composed of coarse grained orientated crystallites. Single crystal c-axis tubes of sodium beta-alumina were grown from melts containing excess sodium oxide. Additional experiments demonstrated that crystals of magnesia doped beta-alumina and potassium beta-alumina also can be achieved by this EFG technique.

Metal-assisted and microwave accelerated-evaporative crystallization: Application to lysozyme protein

NASA Astrophysics Data System (ADS)

Mauge-Lewis, Kevin

In response to the growing need for new crystallization techniques that afford for rapid processing times along with control over crystal size and distribution, the Aslan Research Group has recently demonstrated the use of Metal-Assisted and Microwave-Accelerated Evaporative Crystallization MA-MAEC technique in conjunction with metal nanoparticles and nanostructures for the crystallization of amino acids and organic small molecules. In this study, we have employed the newly developed MA-MAEC technique to the accelerated crystallization of chicken egg-white lysozyme on circular crystallization platforms in order to demonstrate the proof-of-principle application of the method for protein crystallization. The circular crystallization platforms are constructed in-house from poly (methyl methacrylate) (PMMA) and silver nanoparticle films (SNFs), indium tin oxide (ITO) and iron nano-columns. In this study, we prove the MA-MAEC method to be a more effective technique in the rapid crystallization of macromolecules in comparison to other conventional methods. Furthermore, we demonstrate the use of the novel iCrystal system, which incorporates the use of continuous, low wattage heating to facilitate the rapid crystallization of the lysozyme while still retaining excellent crystal quality. With the incorporation of the iCrystal system, we observe crystallization times that are even shorter than those produced by the MA-MAEC technique using a conventional microwave oven in addition to significantly improved crystal quality.

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 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.

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

Femtosecond laser direct writing of monocrystalline hexagonal silver prisms

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

Vora, Kevin; Kang, SeungYeon; Moebius, Michael

Bottom-up growth methods and top-down patterning techniques are both used to fabricate metal nanostructures, each with a distinct advantage: One creates crystalline structures and the other offers precise positioning. Here, we present a technique that localizes the growth of metal crystals to the focal volume of a laser beam, combining advantages from both approaches. We report the fabrication of silver nanoprisms—hexagonal nanoscale silver crystals—through irradiation with focused femtosecond laser pulses. The growth of these nanoprisms is due to a nonlinear optical interaction between femtosecond laser pulses and a polyvinylpyrrolidone film doped with silver nitrate. The hexagonal nanoprisms have bases hundredsmore » of nanometers in size and the crystal growth occurs over exposure times of less than 1 ms (8 orders of magnitude faster than traditional chemical techniques). Electron backscatter diffraction analysis shows that the hexagonal nanoprisms are monocrystalline. The fabrication method combines advantages from both wet chemistry and femtosecond laser direct-writing to grow silver crystals in targeted locations. The results presented in this letter offer an approach to directly positioning and growing silver crystals on a substrate, which can be used for plasmonic devices.« less

Simultaneous in situ Optical Monitoring Techniques during Crystal Growth of ZnSe by Physical Vapor Transport

NASA Technical Reports Server (NTRS)

Su, C.- H.; Feth, S.; Lehoczky, S. L.

1998-01-01

ZnSe crystals grown in sealed ampoules by the physical vapor transport method were monitored in situ using three techniques, simultaneously. A Michelson interferometer was set-up to observe the growth rate and surface morphological evolution. An interference pattern (interferogram) is formed by the interaction between the reflection of a HeNe laser (632.8 nm wavelength) off the crystal-vapor interface and a reference beam from the same laser. Preliminary results indicate that the rate of growth/thermal-etching can be calculated using analog data acquisition and simple fringe counting techniques. Gross surface features may also be observed using a digital frame grabber and fringe analysis software. The second in situ technique uses optical absorption to determine the partial pressures of the vapor species. The Se2 and Zn vapor species present in the sealed ampoule absorb light at characteristic wavelengths. The optical absorption is determined by monitoring the light intensity difference between the sample and reference beams. The Se2 Partial pressure profile along the length of the ampoule was estimated from the vibronic absorption peaks at 340.5, 350.8, 361.3 and 379.2 nm using the Beer's law constants established in the calibration runs of pure Se. Finally, because the high temperature crystal growth furnace contains windows, in situ visual observation of the growing crystal is also possible. The use of these techniques not only permits in situ investigation of high temperature vapor growth of semiconductors, but also offers the potential for real time feed back on the growing crystal and allows the possibility of actively controlling the growth process.

Development of low-cost silicon crystal growth techniques for terrestrial photovoltaic solar energy conversion

NASA Technical Reports Server (NTRS)

Zoutendyk, J. A.

1976-01-01

Because of the growing need for new sources of electrical energy, photovoltaic solar energy conversion is being developed. Photovoltaic devices are now being produced mainly from silicon wafers obtained from the slicing and polishing of cylindrically shaped single crystal ingots. Inherently high-cost processes now being used must either be eliminated or modified to provide low-cost crystalline silicon. Basic to this pursuit is the development of new or modified methods of crystal growth and, if necessary, crystal cutting. If silicon could be grown in a form requiring no cutting, a significant cost saving would potentially be realized. Therefore, several techniques for growth in the form of ribbons or sheets are being explored. In addition, novel techniques for low-cost ingot growth and cutting are under investigation.

Systematic Improvement of Protein Crystals by Determining the Supersolubility Curves of Phase Diagrams

PubMed Central

Saridakis, Emmanuel; Chayen, Naomi E.

2003-01-01

A systematic approach for improving protein crystals by growing them in the metastable zone using the vapor diffusion technique is described. This is a simple technique for optimization of crystallization conditions. Screening around known conditions is performed to establish a working phase diagram for the crystallization of the protein. Dilutions of the crystallization drops across the supersolubility curve into the metastable zone are then carried out as follows: the coverslips holding the hanging drops are transferred, after being incubated for some time at conditions normally giving many small crystals, over reservoirs at concentrations which normally yield clear drops. Fewer, much larger crystals are obtained when the incubation times are optimized, compared with conventional crystallization at similar conditions. This systematic approach has led to the structure determination of the light-harvesting protein C-phycocyanin to the highest-ever resolution of 1.45 Å. PMID:12547801

Recent results and new hardware developments for protein crystal growth in microactivity

NASA Technical Reports Server (NTRS)

Delucas, L. J.; Long, M. M.; Moore, K. M.; Smith, C.; Carson, M.; Narayana, S. V. L.; Carter, D.; Clark, A. D., Jr.; Nanni, R. G.; Ding, J.

1993-01-01

Protein crystal growth experiments have been performed on 16 space shuttle missions since April, 1985. The initial experiments utilized vapor diffusion crystallization techniques similar to those used in laboratories for earth-based experiments. More recent experiments have utilized temperature induced crystallization as an alternative method for growing high quality protein crystals in microgravity. Results from both vapor diffusion and temperature induced crystallization experiments indicate that proteins grown in microgravity may be larger, display more uniform morphologies, and yield diffraction data to significantly higher resolutions than the best crystals of these proteins grown on earth.

Hydrothermal Growth of Polyscale Crystals

NASA Astrophysics Data System (ADS)

Byrappa, Kullaiah

In this chapter, the importance of the hydrothermal technique for growth of polyscale crystals is discussed with reference to its efficiency in synthesizing high-quality crystals of various sizes for modern technological applications. The historical development of the hydrothermal technique is briefly discussed, to show its evolution over time. Also some of the important types of apparatus used in routine hydrothermal research, including the continuous production of nanosize crystals, are discussed. The latest trends in the hydrothermal growth of crystals, such as thermodynamic modeling and understanding of the solution chemistry, are elucidated with appropriate examples. The growth of some selected bulk, fine, and nanosized crystals of current technological significance, such as quartz, aluminum and gallium berlinites, calcite, gemstones, rare-earth vanadates, electroceramic titanates, and carbon polymorphs, is discussed in detail. Future trends in the hydrothermal technique, required to meet the challenges of fast-growing demand for materials in various technological fields, are described. At the end of this chapter, an Appendix 18.A containing a more or less complete list of the characteristic families of crystals synthesized by the hydrothermal technique is given with the solvent and pressure-temperature (PT) conditions used in their synthesis.

The performance studies of DKDP crystals grown by a rapid horizontal growth method

NASA Astrophysics Data System (ADS)

Xie, Xiaoyi; Qi, Hongji; Wang, Bin; Wang, Hu; Chen, Duanyang; Shao, Jianda

2018-04-01

A deuterated potassium dihydrogen phosphate (DKDP) crystal with about 70% deuterium level was grown by a rapid horizontal growth method with independent design equipment, which includes a continuous filtration system. The cooling program during crystal growth was designed according to a self-developed software to catch the size of growing crystal in real time. The crystal structure, optical performance and laser induced damage threshold (LIDT) of this DKDP crystal were investigated in this paper. The deuterium concentration of the crystal was confirmed by the neutron diffraction technique, which was effective and available in determining a complete range of deuteration level. The dielectric property was measured to evaluate the perfection of the lattice. The transmittance and LIDT were carried out further to evaluate the optical and functional properties of this DKDP crystal grown in the rapid horizontal growth technique. All of the detailed characterization for DKDP figured out that the 70% deuterated KDP crystal grown in this way had relatively good qualities.

Biomimetic and Aggregation-Driven Crystallization Route for Room-Temperature Material Synthesis: Growth of β-Ga2O3 Nanoparticles Using Peptide Assemblies as Nanoreactors

PubMed Central

Lee, Sang-Yup; Gao, Xueyun; Matsui, Hiroshi

2008-01-01

The room temperature synthesis of β-Ga2O3 nanocrystal was examined by coupling two biomimetic crystallization techniques, the enzymatic peptide nano-assembly templating and the aggregation-driven crystallization. The catalytic template of peptide assembly nucleated and mineralized primary β-Ga2O3 crystals, and then fused them to grow single-crystalline and monodisperse nanoparticles in the cavity of the peptide assembly at room temperature. In this work, the peptide assembly was exploited as a nano-reactor with an enzymatic functionality catalyzing the hydrolysis of gallium precursors. In addition, the characteristic ring-structure of peptide assembly is expected to provide an efficient dehydration pathway and the crystallization control over the surface tension, which are advantageous for the β-Ga2O3 crystal growth. This multifunctional peptide assembly could be applied for syntheses of a variety of nanomaterials that are kinetically difficult to grow at room temperature. PMID:17302413

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.

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.

Subsurface Growth Of Silicide Structures In Silicon

NASA Technical Reports Server (NTRS)

Fathauer, Robert W.; George, Thomas; Pike, William T.; Schowalter, Leo

1993-01-01

Technique shows promise for fabrication of novel electronic, optoelectronic, and electro-optical devices. Experiments demonstrated feasibility of growing microscopic single-crystal CoSi2 structures beneath surfaces of Si substrates.

A study on inclusion formation mechanism in alpha-LiIO sub 3 crystals

NASA Technical Reports Server (NTRS)

Chen, W. C.; Yan, S. L.; Jia, S. Q.; Du, S. Y.

1985-01-01

The spatial distribution of inclusions in alpha-LiIO3 crystals by means of an argon laser beam scanning technique is studied. The effects of crystal dimensions and solution fluid flow on the inclusion formation in the alpha-LiIO3 crystals were observed. It was further shown that the fluid flow plays an important role in the formation of inclusions. The results obtained were further applied and verified by growing a perfect alpha-LiIO3 single crystal. An experimental foundation for further theoretical studies on the causes of inclusions may be provided.

The Protein Crystallization Facility STS-95

NASA Technical Reports Server (NTRS)

2004-01-01

The Protein Crystallization Facility will be used to grow crystals of human insulin. Insulin is the primary treatment for diabetes, the fourth leading cause of death by disease. Research on STS-95 is aimed at producing crystals of even higher quality, which when combined with new analysis techniques will permit a better understanding of the interaction between insulin and its receptor. This has the potential to aid in the development of a new commercially available insulin product with unique time release properties that could reduce fluctuations in a patient's blood sugar level. The Protein Crystallization Facility supports large-scale commercial investigations.

Crystal growth, structural, thermal and mechanical behavior of l-arginine 4-nitrophenolate 4-nitrophenol dihydrate (LAPP) single crystals.

PubMed

Mahadevan, M; Ramachandran, K; Anandan, P; Arivanandhan, M; Bhagavannarayana, G; Hayakawa, Y

2014-12-10

Single crystals of l-arginine 4-nitrophenolate 4-nitrophenol dihydrate (LAPP) have been grown successfully from the solution of l-arginine and 4-nitrophenol. Slow evaporation of solvent technique was adopted to grow the bulk single crystals. Single crystal X-ray diffraction analysis confirms the grown crystal has monoclinic crystal system with space group of P21. Powder X-ray diffraction analysis shows the good crystalline nature. The crystalline perfection of the grown single crystals was analyzed by HRXRD by employing a multicrystal X-ray diffractometer. The functional groups were identified from proton NMR spectroscopic analysis. Linear and nonlinear optical properties were determined by UV-Vis spectrophotometer and Kurtz powder technique respectively. It is found that the grown crystal has no absorption in the green wavelength region and the SHG efficiency was found to be 2.66 times that of the standard KDP. The Thermal stability of the crystal was found by obtaining TG/DTA curve. The mechanical behavior of the grown crystal has been studied by Vicker's microhardness method. Copyright © 2014 Elsevier B.V. All rights reserved.

Modeling of axial vibrational control technique for CdTe VGF crystal growth under controlled cadmium partial pressure

NASA Astrophysics Data System (ADS)

Avetissov, I.; Kostikov, V.; Meshkov, V.; Sukhanova, E.; Grishechkin, M.; Belov, S.; Sadovskiy, A.

2014-01-01

A VGF growth setup assisted by axial vibrations of baffle submerged into CdTe melt with controlled Cd partial pressure was designed. An influence of baffle shape on flow velocity map, temperature distribution in CdTe melt and interface shape of growing crystal was analyzed by numerical simulation and physical modeling. To produce the desirable shape of crystal melt interface we slant under different angles vertical generatrix in a cylindrical disk and made chasing on faceplates of a disk. It was ascertained that a disk with conical generatrix formed more intensive convective flows from a faceplate with larger diameter. It was shown that at CdTe VGF crystal growth rate about 10 mm/h application of AVC technique made it possible to produce convex interface for 2 in. crystal diameter.

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.

Compact Apparatus Grows Protein Crystals

NASA Technical Reports Server (NTRS)

Bugg, Charles E.; Delucas, Lawrence J.; Suddath, Fred L.; Snyder, Robert S.; Herren, Blair J.; Carter, Daniel C.; Yost, Vaughn H.

1989-01-01

Laboratory apparatus provides delicately balanced combination of materials and chemical conditions for growth of protein crystals. Apparatus and technique for growth based on hanging-drop method for crystallization of macromolecules. Includes pair of syringes with ganged plungers. One syringe contains protein solution; other contains precipitating-agent solution. Syringes intrude into cavity lined with porous reservoir material saturated with 1 mL or more of similar precipitating-agent solution. Prior to activation, ends of syringes plugged to prevent transport of water vapor among three solutions.

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.

Multiphysical simulation analysis of the dislocation structure in germanium single crystals

NASA Astrophysics Data System (ADS)

Podkopaev, O. I.; Artemyev, V. V.; Smirnov, A. D.; Mamedov, V. M.; Sid'ko, A. P.; Kalaev, V. V.; Kravtsova, E. D.; Shimanskii, A. F.

2016-09-01

To grow high-quality germanium crystals is one of the most important problems of growth industry. The dislocation density is an important parameter of the quality of single crystals. The dislocation densities in germanium crystals 100 mm in diameter, which have various shapes of the side surface and are grown by the Czochralski technique, are experimentally measured. The crystal growth is numerically simulated using heat-transfer and hydrodynamics models and the Alexander-Haasen dislocation model in terms of the CGSim software package. A comparison of the experimental and calculated dislocation densities shows that the dislocation model can be applied to study lattice defects in germanium crystals and to improve their quality.

Solid state neutron detector and method for use

DOEpatents

Doty, F. Patrick; Zwieback, Ilya; Ruderman, Warren

2002-01-01

Crystals of lithium tetraborate or alpha-barium borate had been found to be neutron detecting materials. The crystals are prepared using known crystal growing techniques, wherein the process does not include the common practice of using a fluxing agent, such as sodium oxide or sodium fluoride, to reduce the melting temperature of the crystalline compound. Crystals prepared by this method can be sliced into thin single or polycrystalline wafers, or ground to a powder and prepared as a sintered compact or a print paste, and then configured with appropriate electronic hardware, in order to function as neutron detectors.

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.

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.

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.

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.

Recent Advances in the Understanding of the Influence of Electric and Magnetic Fields on Protein Crystal Growth

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

Pareja-Rivera, Carina; Cuéllar-Cruz, Mayra; Esturau-Escofet, Nuria

Here, in this contribution we use nonconventional methods that help to increase the success rate of a protein crystal growth, and consequently of structural projects using X-ray diffraction techniques. In order to achieve this purpose, this contribution presents new approaches involving more sophisticated techniques of protein crystallization, not just for growing protein crystals of different sizes by using electric fields, but also for controlling crystal size and orientation. Also, this latter was possible through the use of magnetic fields that allow to obtain protein crystals suitable for both high-resolution X-ray and neutron diffraction crystallography where big crystals are required. Thismore » contribution discusses some pros, cons and realities of the role of electromagnetic fields in protein crystallization research, and their effect on protein crystal contacts. Additionally, we discuss the importance of room and low temperatures during data collection. Finally, we also discuss the effect of applying a rather strong magnetic field of 16.5 T, for shorts and long periods of time, on protein crystal growth, and on the 3D structure of two model proteins.« less

Recent Advances in the Understanding of the Influence of Electric and Magnetic Fields on Protein Crystal Growth

DOE PAGES

Pareja-Rivera, Carina; Cuéllar-Cruz, Mayra; Esturau-Escofet, Nuria; ...

2016-12-05

Here, in this contribution we use nonconventional methods that help to increase the success rate of a protein crystal growth, and consequently of structural projects using X-ray diffraction techniques. In order to achieve this purpose, this contribution presents new approaches involving more sophisticated techniques of protein crystallization, not just for growing protein crystals of different sizes by using electric fields, but also for controlling crystal size and orientation. Also, this latter was possible through the use of magnetic fields that allow to obtain protein crystals suitable for both high-resolution X-ray and neutron diffraction crystallography where big crystals are required. Thismore » contribution discusses some pros, cons and realities of the role of electromagnetic fields in protein crystallization research, and their effect on protein crystal contacts. Additionally, we discuss the importance of room and low temperatures during data collection. Finally, we also discuss the effect of applying a rather strong magnetic field of 16.5 T, for shorts and long periods of time, on protein crystal growth, and on the 3D structure of two model proteins.« less

X-ray diffraction, spectroscopic and mechanical studies on potential organic NLO materials of metaNitroaniline and N-3-Nitrophenyl Acetamide single crystals

NASA Astrophysics Data System (ADS)

Senthil, S.; Madhavan, J.

2015-02-01

In the present paper, attempts were made to grow good quality metaNitroaniline (mNA) and N-3-Nitrophenyl (3-NAA) single crystals. The lattice parameter values from the Powder X-ray diffraction pattern confirms that mNA belongs to orthorhombic crystal system with the unit cell parameter values of a = 6.501 Å, b = 19.330 Å and c = 5.082 Å with space group Pbc21. Similarly the powder XRD data indicates that 3-NAA crystal retained its monoclinic structure with lattice parameter values a = 9.762 Å, b =13.287 Å, c =13.226 Å, and β = 102.99°. Investigation has been carried out to assign the vibrational frequencies of the grown crystals by Fourier Transform infrared spectroscopy technique. The SHG efficiency of mNA and 3NAA was determined by Kurtz and Perry powder technique. The Optical absorption study confirms the suitability of the crystals for device applications. The mechanical properties of the grown crystals have been studied using Vickers microhardness tester.

Li2MoO4 crystal growth from solution activated by low-frequency vibrations

NASA Astrophysics Data System (ADS)

Barinova, Olga; Sadovskiy, Andrey; Ermochenkov, Ivan; Kirsanova, Svetlana; Sukhanova, Ekaterina; Kostikov, Vladimir; Belov, Stanislav; Mozhevitina, Elena; Khomyakov, Andrew; Kuchuk, Zhanna; Zharikov, Eugeny; Avetissov, Igor

2017-01-01

The possibility of Li2MoO4 crystal growth from aqueous solutions activated by axial vibrational control (AVC) technique was investigated. It was found out that a low-frequency mechanical activation of the solution led to an increase of Li2MoO4 equilibrium solubility in aqueous solution for 11 rel% in the 25-29 °C temperature range. The changes in solution structure were analyzed in situ by Raman study of the solution. The AVC activation of solution resulted in a re-faceting of growing crystals, a smoothing of a face surface morphology and reduction of water content in the crystal.

Growth of new borate crystals with fiber shape by the micro-pulling down technique

NASA Astrophysics Data System (ADS)

Assi, Farah; Ferriol, Michel; Aillerie, Michel; Cochez, Marianne

2017-07-01

Borate-based materials are of high interest to generate an UV laser light from a crystal. Fiber-shaped crystals combining the advantages of fiber lasers and crystalline lasers, we have investigated the growing conditions required to obtain usable fibers of Bi2ZnB2O7 (BZBO) and LaBGeO5 (LBGO). For BZBO, the major drawback was the pronounced color of the fibers and for LBGO, it was the high viscosity of its melt leading to use a flux. This paper presents our state of the art to obtain good quality BZBO and LBGO crystal fibers.

Transmission electron microscopy study of the formation of epitaxial CoSi2/Si (111) by a room-temperature codeposition technique

NASA Technical Reports Server (NTRS)

D'Anterroches, Cecile; Yakupoglu, H. Nejat; Lin, T. L.; Fathauer, R. W.; Grunthaner, P. J.

1988-01-01

Co and Si have been codeposited on Si (111) substrates near room temperature in a stoichiometric 1:2 ratio in a molecular beam epitaxy system. Annealing of these deposits yields high-quality single-crystal CoSi2 layers. Transmission electron microscopy has been used to examine as-deposited layers and layers annealed at 300, 500, and 600 C. Single-crystal epitaxial grains of CoSi2 embedded in a matrix of amorphous Co/Si are observed in as-deposited samples, while the layer is predominantly single-crystal, inhomogeneously strained CoSi2 at 300 C. At 600 C, a homogeneously strained single-crystal layer with a high density of pinholes is observed. In contrast to other solid phase epitaxy techniques used to grow CoSi2 on Si (111), no intermediate silicide phases are observed prior to the formation of CoSi2.

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

Sparse and incomplete factorial matrices to screen membrane protein 2D crystallization

PubMed Central

Lasala, R.; Coudray, N.; Abdine, A.; Zhang, Z.; Lopez-Redondo, M.; Kirshenbaum, R.; Alexopoulos, J.; Zolnai, Z.; Stokes, D.L.; Ubarretxena-Belandia, I.

2014-01-01

Electron crystallography is well suited for studying the structure of membrane proteins in their native lipid bilayer environment. This technique relies on electron cryomicroscopy of two-dimensional (2D) crystals, grown generally by reconstitution of purified membrane proteins into proteoliposomes under conditions favoring the formation of well-ordered lattices. Growing these crystals presents one of the major hurdles in the application of this technique. To identify conditions favoring crystallization a wide range of factors that can lead to a vast matrix of possible reagent combinations must be screened. However, in 2D crystallization these factors have traditionally been surveyed in a relatively limited fashion. To address this problem we carried out a detailed analysis of published 2D crystallization conditions for 12 β-barrel and 138 α-helical membrane proteins. From this analysis we identified the most successful conditions and applied them in the design of new sparse and incomplete factorial matrices to screen membrane protein 2D crystallization. Using these matrices we have run 19 crystallization screens for 16 different membrane proteins totaling over 1,300 individual crystallization conditions. Six membrane proteins have yielded diffracting 2D crystals suitable for structure determination, indicating that these new matrices show promise to accelerate the success rate of membrane protein 2D crystallization. PMID:25478971

KSC-97PC1382

NASA Image and Video Library

1997-09-08

United States Microgravity Payload-4 (USMP-4) experiments are prepared to be flown on Space Shuttle mission STS-87 in the Space Station Processing Facility at Kennedy Space Center (KSC). This horizontal tube is known as MEPHISTO, the French acronym for a cooperative American-French investigation of the fundamentals of crystal growth. This experiment, designed for the study of solidification (or freezing) during the growth cycle of liquid materials used for semiconductor crystals, aims to aid in the development of techniques for growing higher quality crystals on Earth. All STS-87 experiments are scheduled for launch on Nov. 19 from KSC

Crystallization of isoelectrically homogeneous cholera toxin

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

Spangler, B.D.; Westbrook, E.M.

1989-02-07

Past difficulty in growing good crystals of cholera toxin has prevented the study of the crystal structure of this important protein. The authors have determined that failure of cholera toxin to crystallize well has been due to its heterogeneity. They have now succeeded in overcoming the problem by isolating a single isoelectric variant of this oligomeric protein (one A subunit and five B subunits). Cholera toxin purified by their procedure readily forms large single crystals. The crystal form has been described previously. They have recorded data from native crystals of cholera toxin to 3.0-{angstrom} resolution with our electronic area detectors.more » With these data, they have found the orientation of a 5-fold symmetry axis within these crystals, perpendicular to the screw dyad of the crystal. They are now determining the crystal structure of cholera toxin by a combination of multiple heavy-atom isomorphous replacement and density modification techniques, making use of rotational 5-fold averaging of the B subunits.« less

Advanced Methods of Protein Crystallization.

PubMed

Moreno, Abel

2017-01-01

This chapter provides a review of different advanced methods that help to increase the success rate of a crystallization project, by producing larger and higher quality single crystals for determination of macromolecular structures by crystallographic methods. For this purpose, the chapter is divided into three parts. The first part deals with the fundamentals for understanding the crystallization process through different strategies based on physical and chemical approaches. The second part presents new approaches involved in more sophisticated methods not only for growing protein crystals but also for controlling the size and orientation of crystals through utilization of electromagnetic fields and other advanced techniques. The last section deals with three different aspects: the importance of microgravity, the use of ligands to stabilize proteins, and the use of microfluidics to obtain protein crystals. All these advanced methods will allow the readers to obtain suitable crystalline samples for high-resolution X-ray and neutron crystallography.

Interactions that know no boundaries

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

Wall, Michael E.

Deviations from an ideal crystal lead to diffuse scattering (DS) intensity, both between and beneath the Bragg peaks in diffraction patterns (Guinier, 1963). First characterized using simple ionic crystals in early studies of X-ray diffraction (Lonsdale, 1942), DS has a rich history (Welberry & Weber, 2016) and is a well established technique in smallmolecule crystallography (Welberry, 2004). DS studies in macromolecular crystallography began more recently (Phillips et al., 1980) and now the potential for obtaining information about protein motions is fueling the growing interest in DS (Meisburger et al., 2017).

Interactions that know no boundaries

DOE PAGES

Wall, Michael E.

2018-03-01

Deviations from an ideal crystal lead to diffuse scattering (DS) intensity, both between and beneath the Bragg peaks in diffraction patterns (Guinier, 1963). First characterized using simple ionic crystals in early studies of X-ray diffraction (Lonsdale, 1942), DS has a rich history (Welberry & Weber, 2016) and is a well established technique in smallmolecule crystallography (Welberry, 2004). DS studies in macromolecular crystallography began more recently (Phillips et al., 1980) and now the potential for obtaining information about protein motions is fueling the growing interest in DS (Meisburger et al., 2017).

Growing Organic Crystals By The Czochralski Method

NASA Technical Reports Server (NTRS)

Shields, Angela; Frazier, Donald O.; Penn, Benjamin G.; Aggarwal, M. D.; Wang, W. S.

1994-01-01

Apparatus grows high-quality single crystals of organic compounds by Czochralski method. In Czochralski process, growing crystal lifted from middle of molten material without touching walls. Because of low melting temperatures of organic crystals, glass vessels usable. Traditional method for inorganic semiconductors adapted to optically nonlinear organic materials.

Single crystal growth from separated educts and its application to lithium transition-metal oxides

PubMed Central

Freund, F.; Williams, S. C.; Johnson, R. D.; Coldea, R.; Gegenwart, P.; Jesche, A.

2016-01-01

Thorough mixing of the starting materials is the first step of a crystal growth procedure. This holds true for almost any standard technique, whereas the intentional separation of educts is considered to be restricted to a very limited number of cases. Here we show that single crystals of α-Li2IrO3 can be grown from separated educts in an open crucible in air. Elemental lithium and iridium are oxidized and transported over a distance of typically one centimeter. In contrast to classical vapor transport, the process is essentially isothermal and a temperature gradient of minor importance. Single crystals grow from an exposed condensation point placed in between the educts. The method has also been applied to the growth of Li2RuO3, Li2PtO3 and β-Li2IrO3. A successful use of this simple and low cost technique for various other materials is anticipated. PMID:27748402

Impact of impurities on the α-LiIO{sub 3} crystal growth: Technique for measuring the “dead zone”

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

Noskova, A. N., E-mail: anna-13.08@mail.ru; Rubakha, V. I.; Prokhorov, A. P.

Lithium iodate (α-LiIO{sub 3}) single crystal is a promising nonlinear optical material, which used for efficient laser radiation conversion in the visible and near-IR regions. A technique for measuring the “dead zone” (ΔТ{sub dz}) of LiIO{sub 3} solutions has been developed; data on the impact of Fe(IO{sub 3}){sub 2}, AgIO{sub 3}, CsOH, H{sub 3}PO{sub 4}, and methyl methacrylate on the growth of the (100) face of α-LiIO{sub 3} crystals have been presented; and the dependences of the nucleation and motion of single steps on the degree of supersaturation have been measured. It is shown that the ΔТ{sub dz} value makesmore » it possible to estimate the validity of solutions for growing α-LiIO{sub 3} crystals. The results of measuring the face growth rates and step velocities for KDP and α-LiIO{sub 3} crystals are compared.« less

Dosimetry with diamond detectors

NASA Astrophysics Data System (ADS)

Gervino, G.; Marino, C.; Silvestri, F.; Lavagno, A.; Truc, F.

2010-05-01

In this paper we present the dosimetry analysis in terms of stability and repeatability of the signal and dose rate dependence of a synthetic single crystal diamond grown by Chemical Vapor Deposition (CVD) technique. The measurements carried out by 5 MeV X-ray photons beam show very promising results, even if the dose rate detector response points out that the charge trapping centers distribution is not uniform inside the crystal volume. This handicap that affects the detectors performances, must be ascribed to the growing process. Synthetic single crystal diamonds could be a valuable alternative to air ionization chambers for quality beam control and for intensity modulated radiation therapy beams dosimetry.

Laser scattering in a hanging drop vapor diffusion apparatus for protein crystal growth in a microgravity environment

NASA Technical Reports Server (NTRS)

Casay, G. A.; Wilson, W. W.

1992-01-01

One type of hardware used to grow protein crystals in the microgravity environment aboard the U.S. Space Shuttle is a hanging drop vapor diffusion apparatus (HDVDA). In order to optimize crystal growth conditions, dynamic control of the HDVDA is desirable. A critical component in the dynamically controlled system is a detector for protein nucleation. We have constructed a laser scattering detector for the HDVDA capable of detecting the nucleation stage. The detector was successfully tested for several scatterers differing in size using dynamic light scattering techniques. In addition, the ability to detect protein nucleation using the HDVDA was demonstrated for lysozyme.

Room temperature aluminum antimonide radiation detector and methods thereof

DOEpatents

Lordi, Vincenzo; Wu, Kuang Jen J.; Aberg, Daniel; Erhart, Paul; Coombs, III, Arthur W; Sturm, Benjamin W

2015-03-03

In one embodiment, a method for producing a high-purity single crystal of aluminum antimonide (AlSb) includes providing a growing environment with which to grow a crystal, growing a single crystal of AlSb in the growing environment which comprises hydrogen (H.sub.2) gas to reduce oxide formation and subsequent incorporation of oxygen impurities in the crystal, and adding a controlled amount of at least one impurity to the growing environment to effectively incorporate at least one dopant into the crystal. In another embodiment, a high energy radiation detector includes a single high-purity crystal of AlSb, a supporting structure for the crystal, and logic for interpreting signals obtained from the crystal which is operable as a radiation detector at a temperature of about 25.degree. C. In one embodiment, a high-purity single crystal of AlSb includes AlSb and at least one dopant selected from a group consisting of selenium (Se), tellurium (Te), and tin (Sn).

A NASA Recipe for Protein Crystallography. Educational Brief.

ERIC Educational Resources Information Center

National Aeronautics and Space Administration, Washington, DC.

This brief discusses growing protein crystals. Protein crystals can be very difficult to grow. This activity for grades 9-12 provides a simple recipe for growing protein crystals from Brazil nuts. Included are a history of protein crystals, a discussion of microgravity effects on growth, connections to academic standards, and lab sheets. (MVL)

Ice Particle Charge Transfer Studies.

DTIC Science & Technology

1987-09-30

sufficient time for the rime feathers to grow . The rimed target was then exposed to the salt droplet cloud produced by a small Unicorn nebuliser. This...limited in extent, and it was possible only to grow crystals of 100 pm diameter; whereas, in nature, crystals have time to grow several hundred microns...updraft which countered ti~e terminal fall velocity of the growing crystals. The droplet supply was main- tained and the crystals grew to about 150-200

Determination of monomer concentrations in crystallizing lysozyme solutions

NASA Technical Reports Server (NTRS)

Wilson, L. J.; Pusey, Marc L.

1992-01-01

We have developed a non-optical technique for the study of aggregation in lysozyme and other protein solutions. By monitoring the rate at which lysozyme traverses a semipermeable membrane it was possible to quantitate the degree of aggregation in supersaturated solutions. Using this technique, we have measured the concentration of monomers and larger aggregates in under- and oversaturated lysozyme solutions, and in the presence of crystals, at pH 4.0 and 3 percent NaCl (0.1M NaAc). Comparison of these concentration profiles with (110) face growth rate data supports the theory that tetragonal lysozyme crystals grow by addition of preformed aggregates and not by monomer addition. The data suggest that a considerable population of aggregates larger than dimers are present at lysozyme concentrations above 22 mg/ml. Determination of dimer concentrations, and equilibrium constants for subsequent aggregation levels, are currently underway.

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.

Growth and characterization of an organic single crystal: 2-[2-(4-Diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide

NASA Astrophysics Data System (ADS)

Senthil, K.; Kalainathan, S.; Ruban Kumar, A.

Optically transparent crystal of the organic salt DEASI (2-[2-(4-Diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide) has been synthesized by using knoevenagel condensation reaction method. The synthesized material has been purified by successfully recrystallization process. Single crystals of DEASI have been grown by slow evaporation technique at room temperature. The solubility of the title material has been determined at different temperature in acetonitrile/methanol mixture. The cell parameters and crystallinity of the title crystal were determined by single crystal XRD. The powder diffraction was carried out to study the reflection plane of the grown crystal and diffraction peaks were indexed. The presence of different functional groups in the crystal was confirmed by Fourier transform infrared (FTIR) analysis. 1H NMR spectrum was recorded to confirm the presence of hydrogen nuclei in the synthesized material. The optical property of the title crystal was studied by UV-Vis-NIR spectroscopic analysis. The melting point and thermal property of DEASI were studied using TGA/DSC technique. The Vicker’s hardness (Hv) was carried out to know the category. The dielectric constant and dielectric loss of the compound decreases with an increase in frequencies. Chemical etching studies showed that the DEASI grows in the two dimensional growth mechanisms. The Kurtz-Perry powder second harmonic generation (SHG) test has done for title crystal.

Growth and characterization of an organic single crystal: 2-[2-(4-diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide.

PubMed

Senthil, K; Kalainathan, S; Ruban Kumar, A

2014-05-05

Optically transparent crystal of the organic salt DEASI (2-[2-(4-Diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide) has been synthesized by using knoevenagel condensation reaction method. The synthesized material has been purified by successfully recrystallization process. Single crystals of DEASI have been grown by slow evaporation technique at room temperature. The solubility of the title material has been determined at different temperature in acetonitrile/methanol mixture. The cell parameters and crystallinity of the title crystal were determined by single crystal XRD. The powder diffraction was carried out to study the reflection plane of the grown crystal and diffraction peaks were indexed. The presence of different functional groups in the crystal was confirmed by Fourier transform infrared (FTIR) analysis. (1)H NMR spectrum was recorded to confirm the presence of hydrogen nuclei in the synthesized material. The optical property of the title crystal was studied by UV-Vis-NIR spectroscopic analysis. The melting point and thermal property of DEASI were studied using TGA/DSC technique. The Vicker's hardness (Hv) was carried out to know the category. The dielectric constant and dielectric loss of the compound decreases with an increase in frequencies. Chemical etching studies showed that the DEASI grows in the two dimensional growth mechanisms. The Kurtz-Perry powder second harmonic generation (SHG) test has done for title crystal. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis of chalcogenide and pnictide crystals in salt melts using a steady-state temperature gradient

NASA Astrophysics Data System (ADS)

Chareev, D. A.; Volkova, O. S.; Geringer, N. V.; Koshelev, A. V.; Nekrasov, A. N.; Osadchii, V. O.; Osadchii, E. G.; Filimonova, O. N.

2016-07-01

Some examples of growing crystals of metals, alloys, chalcogenides, and pnictides in melts of halides of alkali metals and aluminum at a steady-state temperature gradient are described. Transport media are chosen to be salt melts of eutectic composition with the participation of LiCl, NaCl, KCl, RbCl, CsCl, AlCl3, AlBr3, KBr, and KI in a temperature range of 850-150°C. Some crystals have been synthesized only using a conducting contour. This technique of crystal growth is similar to the electrochemical method. In some cases, to exclude mutual influence, some elements have been isolated and forced to migrate to the crystal growth region through independent channels. As a result, crystals of desired quality have been obtained using no special equipment and with sizes sufficient for study under laboratory conditions.

Diagnosing the Internal Architecture of Zeolite Ferrierite

PubMed Central

Schmidt, Joel E.; Hendriks, Frank C.; Lutz, Martin; Post, L. Christiaan; Fu, Donglong

2017-01-01

Abstract Large crystals of zeolite ferrierite (FER) are important model systems for spatially resolved catalysis and diffusion studies, though there is considerable variation in crystal habit depending on the chemical composition and employed synthesis conditions. A synergistic combination of techniques has been applied, including single crystal X‐ray diffraction, high‐temperature in situ confocal fluorescence microscopy, fluorescent probe molecules, wide‐field microscopy and atomic force microscopy to unravel the internal architecture of three distinct FER zeolites. Pyrolyzed template species can be used as markers for the 8‐membered ring direction as they are trapped in the terraced roof of the FER crystals. This happens as the materials grow in a layer‐by‐layer, defect‐free manner normal to the large crystal surface, and leads to a facile method to diagnose the pore system orientation, which avoids tedious single crystal X‐ray diffraction experiments. PMID:28809081

Draft Tube Baffle (DTB) crystallizers: A study of stationary and dynamically behaving Crystal Size Distributions (CSD)

NASA Astrophysics Data System (ADS)

Deleer, B. G. M.

1981-11-01

Based on population balance, CSD behavior as a function of geometrical and operating variables was studied, using a crystallizer. A potash alum-water system, involving a separation technique which uses surface active agents and an apolar, organic liquid to separate potash alum crystals from mother liquid under the influence of gravity was used to check experimental findings against literature data. Results show action of annular settling spaces is strongly influenced by fluid velocities perpendicular to those directed upwards. The well-mixed volume decreases with increasing crystallizer size until a minimum effective volume is reached. As supersaturation is constant throughout the crystallizer volume under stationary operating conditions, the annular settling space behaves like a growth chamber for crystals in its volume. Swirl in the lower part of the annular volume introduces significant back mixing. Crystals within this space either grow and return to the well-mixed part, or withdraw from the annular volume permanently.

Preparation of fine single crystals of magnetic superconductor RuSr2GdCu2O8-δ by partial melting

NASA Astrophysics Data System (ADS)

Yamaki, Kazuhiro; Bamba, Yoshihiro; Irie, Akinobu

2018-03-01

In this study, fine uniform RuSr2GdCu2O8-δ (RuGd-1212) single crystals have been successfully prepared by partial melting. Synthesis temperature could be lowered to a value not exceeding the decomposition temperature of RuGd-1212 using the Sr-Gd-Cu-O flux. The crystals grown by alumina boats are cubic, which coincides with the result of a previous study of RuGd-1212 single crystals using platinum crucibles. The single crystals were up to 15 × 15 × 15 µm3 in size and their lattice constants were consistent with those of polycrystalline samples reported previously. Although the present size of single crystals is not sufficient for measurements, the partial melting technique will be beneficial for future progress of research using RuGd-1212 single crystals. Appropriate nominal composition, sintering atmosphere, and temperature are essential factors for growing RuGd-1212 single crystals.

Bulk growth of undoped and Nd3+ doped zinc thiourea chloride (ZTC) monocrystal: Exploring the remarkably enhanced structural, optical, electrical and mechanical performance of Nd3+ doped ZTC crystal for NLO device applications

NASA Astrophysics Data System (ADS)

Anis, Mohd; Muley, Gajanan. G.

2017-05-01

In current scenario good quality crystals are demanded for NLO device application hence present communication is aimed to grow bulk crystal and investigate the doping effect of rare earth element Nd3+ on structural, linear-nonlinear optical, luminescence, mechanical and dielectric properties of zinc thiourea chloride (ZTC) crystal. The ZTC crystal of dimension 21×10×8 mm3 and the Nd3+ doped ZTC crystal of dimension 27×17×5 mm3 have been grown from aqueous solution by slow evaporation technique. The elemental analysis of Nd3+ doped ZTC single crystal has been performed by means of energy dispersive spectroscopic technique. The powder X-ray diffraction technique has been employed to confirm the crystalline phase and identify the effect of Nd3+ doping on structural dimensions of ZTC crystal. The grown crystals have been characterized by UV-Vis-NIR study in the range of 190-1100 nm to ascertain the enhancement in optical transparency of ZTC crystal facilitated by dopant Nd3+. The recorded transmittance data has been utilized to investigate the vital optical constants of grown crystals. The second order nonlinear optical behavior of grown crystals has been evaluated by means of Kurtz-Perry test and the second harmonic generation efficiency of Nd3+ doped ZTC crystal is found to be 1.24 times higher than ZTC crystal. The luminescence analysis has been performed to examine the electronic purity and the color centered photoluminescence emission nature of pure and Nd3+ doped ZTC crystals. The influence of Nd3+ ion on mechanical behavior of ZTC crystal has been investigated by means of microhardness studies. The nature of dielectric constant and dielectric loss of pure and Nd3+ doped ZTC crystal has been examined in the range of 40-100 °C under dielectric study. The Z-scan technique has been employed using the He-Ne laser to investigate the third order nonlinear optical (TONLO) nature of Nd3+ doped ZTC single crystal. The magnitude of TONLO susceptibility, absorption coefficient and refraction has been determined using the Z-scan transmittance data.

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.

Lessons from high-throughput protein crystallization screening: 10 years of practical experience

PubMed Central

JR, Luft; EH, Snell; GT, DeTitta

2011-01-01

Introduction X-ray crystallography provides the majority of our structural biological knowledge at a molecular level and in terms of pharmaceutical design is a valuable tool to accelerate discovery. It is the premier technique in the field, but its usefulness is significantly limited by the need to grow well-diffracting crystals. It is for this reason that high-throughput crystallization has become a key technology that has matured over the past 10 years through the field of structural genomics. Areas covered The authors describe their experiences in high-throughput crystallization screening in the context of structural genomics and the general biomedical community. They focus on the lessons learnt from the operation of a high-throughput crystallization screening laboratory, which to date has screened over 12,500 biological macromolecules. They also describe the approaches taken to maximize the success while minimizing the effort. Through this, the authors hope that the reader will gain an insight into the efficient design of a laboratory and protocols to accomplish high-throughput crystallization on a single-, multiuser-laboratory or industrial scale. Expert Opinion High-throughput crystallization screening is readily available but, despite the power of the crystallographic technique, getting crystals is still not a solved problem. High-throughput approaches can help when used skillfully; however, they still require human input in the detailed analysis and interpretation of results to be more successful. PMID:22646073

Development of silicon growth techniques from melt with surface heating

NASA Astrophysics Data System (ADS)

Kravtsov, Anatoly

2018-05-01

The paper contains literary and personal data on the development history of silicon-growing technology with volumetric and surface melt heating. It discusses the advantages and disadvantages of surface-heating technology. Examples are given of the implementation of such processes in the 60s-70s of the last century, and the reasons for the discontinuation of the relevant work. It describes the main solutions for the implementation of crystal growth process with the electron-beam heating of the melt surface, implemented by KEPP EU (Latvia). It discusses differences in the management of the growth process for the crystals with constant diameters compared to the Czochralski method. It lists geometrical and electro-physical properties of the obtained crystals. It describes the possible use of such crystals and the immediate challenges of technology development.

Scanning electron microscope view of iron crystal growing on pyroxene crystal

NASA Technical Reports Server (NTRS)

1972-01-01

A scanning electron microscope photograph of a four-micron size iron crystal growing on a pyroxene crystal (calcium-magnesium-iron silicate) from the Apollo 15 Hadley-Apennino lunar landing site. The well developed crystal faces indicate that the crystal was formed from a hot vapor as the rock was cooling.

Bulk Crystal Growth of Piezoelectric PMN-PT Crystals Using Gradient Freeze Technique for Improved SHM Sensors

NASA Technical Reports Server (NTRS)

Aggarwal, Mohan D.; Kochary, F.; Penn, Benjamin G.; Miller, Jim

2007-01-01

There has been a growing interest in recent years in lead based perovskite ferroelectric and relaxor ferroelectric solid solutions because of their excellent dielectric, piezoelectric and electrostrictive properties that make them very attractive for various sensing, actuating and structural health monitoring (SHM) applications. We are interested in the development of highly sensitive and efficient PMN-PT sensors based on large single crystals for the structural health monitoring of composite materials that may be used in future spacecrafts. Highly sensitive sensors are needed for detection of defects in these materials because they often tend to fail by distributed and interacting damage modes and much of the damage occurs beneath the top surface of the laminate and not detectable by visual inspection. Research is being carried out for various combinations of solid solutions for PMN-PT piezoelectric materials and bigger size crystals are being sought for improved sensor applications. Single crystals of this material are of interest for sensor applications because of their high piezoelectric coefficient (d33 greater than 1700 pC/N) and electromechanical coefficients (k33 greater than 0.90). For comparison, the commonly used piezoelectric ceramic lead zirconate titanate (PZT) has a d33 of about 600 pC/N and electromechanical coefficients k33 of about 0.75. At the present time, these piezoelectric relaxor crystals are grown by high temperature flux growth method and the size of these crystals are rather small (3x4x5 mm(exp 3). In the present paper, we have attempted to grow bulk single crystals of PMN-PT in a 2 inch diameter platinum crucible and successfully grown a large size crystal of 67%PMN-33%PT using the vertical gradient freeze technique with no flux. Piezoelectric properties of the grown crystals are investigated. PMN-PT plates show excellent piezoelectric properties. Samples were poled under an applied electric field of 5 kV/cm. Dielectric properties at a frequency of 1 kHz are examined. The grown PMN-PT crystals show typical relaxor dielectric properties. Additionally, the thermal properties of the sample are tested. The results are in good agreement with those found in the literature and some are reported for the first time.

My Spring with Graphene

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

O'Leary, Timothy Sean

2015-06-08

Graphene is a two-dimensional structure, one atom thick, with many uses in the world of technology. It has many useful electrical properties, is a very strong and durable material, and can be used to protect different types of substances. The world would be able to use these properties to further the strength of cars, protect metals from oxidation, increase computer speeds, use to improve superconductors, and whatever future uses that scientist invent or discover. We sought to optimize the growth and transfer of graphene. We grew graphene on copper foils by heating the foil in a furnace, and having variousmore » gases flow through a tube, where the copper foil was placed. We varied some of the concentrations of gases, along with having different times for heating the copper foil, different times for graphene growth, or a combination of the two. The focus of our experiment was to specifically grow monolayer single crystal graphene, which means that we do not want multiplayers of graphene, and do not want multiple crystals growing to form a bigger crystal. Our goal was to grow large single crystals from the growth experiment. We used a few different types of transfer methods that ranged from: using heat and pressure to press the graphene on different materials, using a polymer to cover the graphene with a method to destroy the copper, but leave the graphene and polymer intact, and using a type of heat tape with a combination of varying pressures to transfer the graphene, and then destroy the copper foil. To discover if we grew graphene we used different techniques involving lasers and microscopes to take different types of measurements. Discovering the best way of growing and transferring graphene will help with managing the cost of the future uses of graphene.« less

A study on ice crystal formation behavior at intracellular freezing of plant cells using a high-speed camera.

PubMed

Ninagawa, Takako; Eguchi, Akemi; Kawamura, Yukio; Konishi, Tadashi; Narumi, Akira

2016-08-01

Intracellular ice crystal formation (IIF) causes several problems to cryopreservation, and it is the key to developing improved cryopreservation techniques that can ensure the long-term preservation of living tissues. Therefore, the ability to capture clear intracellular freezing images is important for understanding both the occurrence and the IIF behavior. The authors developed a new cryomicroscopic system that was equipped with a high-speed camera for this study and successfully used this to capture clearer images of the IIF process in the epidermal tissues of strawberry geranium (Saxifraga stolonifera Curtis) leaves. This system was then used to examine patterns in the location and formation of intracellular ice crystals and to evaluate the degree of cell deformation because of ice crystals inside the cell and the growing rate and grain size of intracellular ice crystals at various cooling rates. The results showed that an increase in cooling rate influenced the formation pattern of intracellular ice crystals but had less of an effect on their location. Moreover, it reduced the degree of supercooling at the onset of intracellular freezing and the degree of cell deformation; the characteristic grain size of intracellular ice crystals was also reduced, but the growing rate of intracellular ice crystals was increased. Thus, the high-speed camera images could expose these changes in IIF behaviors with an increase in the cooling rate, and these are believed to have been caused by an increase in the degree of supercooling. Copyright © 2016 Elsevier Inc. All rights reserved.

Advances in crystal growth, device fabrication and characterization of thallium bromide detectors for room temperature applications

NASA Astrophysics Data System (ADS)

Datta, Amlan; Moed, Demi; Becla, Piotr; Overholt, Matthew; Motakef, Shariar

2016-10-01

Thallium bromide (TlBr) is a promising room-temperature radiation detector candidate with excellent charge transport properties. However, several critical issues need to be addressed before deployment of this material for long-term field applications can be realized. In this paper, progress made towards solving some of these challenges is discussed. The most significant factors for achieving long-term performance stability for TlBr devices include residual stress as generated during crystal growth and fabrication processes, surface conditions, and the choice of contact metal. Modifications to the commonly used traveling molten zone growth technique for TlBr crystals can significantly minimize the stresses generated by large temperature gradients near the melt-solid interface of the growing crystal. Plasma processing techniques were introduced for the first time to modify the Br-etched TlBr surfaces, which resulted in improvements to the surface conditions, and consequently the spectroscopic response of the detectors. Palladium electrodes resulted a 20-fold improvement in the room-temperature device lifetime when compared to its Br-etched Pt counterpart.

Growth of zinc selenide single crystals by physical vapor transport in microgravity

NASA Technical Reports Server (NTRS)

Rosenberger, Franz

1993-01-01

The goals of this research were the optimization of growth parameters for large (20 mm diameter and length) zinc selenide single crystals with low structural defect density, and the development of a 3-D numerical model for the transport rates to be expected in physical vapor transport under a given set of thermal and geometrical boundary conditions, in order to provide guidance for an advantageous conduct of the growth experiments. In the crystal growth studies, it was decided to exclusively apply the Effusive Ampoule PVT technique (EAPVT) to the growth of ZnSe. In this technique, the accumulation of transport-limiting gaseous components at the growing crystal is suppressed by continuous effusion to vacuum of part of the vapor contents. This is achieved through calibrated leaks in one of the ground joints of the ampoule. Regarding the PVT transport rates, a 3-D spectral code was modified. After introduction of the proper boundary conditions and subroutines for the composition-dependent transport properties, the code reproduced the experimentally determined transport rates for the two cases with strongest convective flux contributions to within the experimental and numerical error.

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.

Columnar and subsurface silicide growth with novel molecular beam epitaxy techniques

NASA Technical Reports Server (NTRS)

Fathauer, R. W.; George, T.; Pike, W. T.

1992-01-01

We have found novel growth modes for epitaxial CoSi2 at high temperatures coupled with Si-rich flux ratios or low deposition rates. In the first of these modes, codeposition of metal and Si at 600-800 C with excess Si leads to the formation of epitaxial silicide columns surrounded by single-crystal Si. During the initial stages of the deposition, the excess Si grows homoepitaxially in between the silicide, which forms islands, so that the lateral growth of the islands is confined. Once a template layer is established by this process, columns of silicide form as a result of selective epitaxy of silicide on silicide and Si on Si. This growth process allows nanometer control over silicide particles in three dimensions. In the second of these modes, a columnar silicide seed layer is used as a template to nucleate subsurface growth of CoSi2. With a 100 nm Si layer covering CoSi2 seeds, Co deposited at 800C and 0.01 nm/s diffuses down to grow on the buried seeds rather than nucleating surface silicide islands. For thicker Si caps or higher deposition rates, the surface concentration of Co exceeds the critical concentration for nucleation of islands, preventing this subsurface growth mode from occurring. Using this technique, single-crystal layers of CoSi2 buried under single-crystal Si caps have been grown.

Bridgman Growth of Germanium

NASA Technical Reports Server (NTRS)

Szofran, F. R.; Volz, M. P.; Cobb, S. D.; Motakef, S.

1997-01-01

The high-magnetic-field crystal growth facility at the Marshall Space Flight Center will be briefly described. This facility has been used to grow bulk germanium by the Bridgman technique in magnetic fields up to 5 Tesla. The results of investigations of ampoule material on the interface shape and thermal field applied to the melt on stability against convection will be discussed.

Quantitative RHEED Studies of MBE Growth of 3-5 Compounds

DTIC Science & Technology

1991-06-03

Vertical - Cavity Surface - Emitting Laser Using Molecular Beam Epitaxial ...Growth of Vertical Cavity Surface - emitting Lasers Our work under this ARO contract on the control of MBE growth has enhanced our ability to grow...pattern about the surface structure of nearly perfect crystals prepared by Molecular Beam Epitaxy ( MBE ) and to use these techniques

Status of holographic interferometry at University of Michigan

NASA Technical Reports Server (NTRS)

Vest, Charles

1987-01-01

Reflection holograms were taken of a jet of air injected traverse to a subsonic stream. The technique of reflection holograms allowed maximum viewing angle and minimum distance to the jet. Holographic interferometry is being used to measure the temperature distribution in a growing crystal. Computations of the temperatures are being made. A phase shift interferometer was used to study flows with very weak changes in refractive index, of the order of 1 shift. Tomographic techniques are being developed for strong refractive cases.

Silicon ribbon growth by a capillary action shaping technique

NASA Technical Reports Server (NTRS)

Schwuttke, G. H.; Ciszek, T. F.; Kran, A.

1976-01-01

The crystal growth method described is a capillary action shaping technique. Meniscus shaping for the desired ribbon geometry occurs at the vertex of a wettable die. As ribbon growth depletes the melt meniscus, capillary action supplies replacement material. A capillary die is so designed that the bounding edges of the die top are not parallel or concentric with the growing ribbon. The new dies allow a higher melt meniscus with concomitant improvements in surface smoothness and freedom from SiC surface particles, which can degrade perfection.

Effects of micro electric current load during cooling of plant tissues on intracellular ice crystal formation behavior and pH.

PubMed

Ninagawa, Takako; Kawamura, Yukio; Konishi, Tadashi; Narumi, Akira

2016-08-01

Cryopreservation techniques are expected to evolve further to preserve biomaterials and foods in a fresh state for extended periods of time. Long-term cryopreservation of living materials such as food and biological tissue is generally achieved by freezing; thus, intracellular freezing occurs. Intracellular freezing injures the cells and leads to cell death. Therefore, a dream cryopreservation technique would preserve the living materials without internal ice crystal formation at a temperature low enough to prevent bacterial activity. This study was performed to investigate the effect of micro electrical current loading during cooling as a new cryopreservation technique. The behavior of intracellular ice crystal formation in plant tissues with or without an electric current load was evaluated using the degree of supercooling, degree of cell deformation, and grain size and growing rate of intracellular ice crystal. Moreover, the transition of intracellular pH during plant tissue cooling with or without electric current loading was also examined using the fluorescence intensity ratio to comprehend cell activity at lower temperatures. The results indicated that micro electric current load did not only decrease the degree of cell deformation and grain size of intracellular ice crystal but also reduced the decline in intracellular pH due to temperature lowering, compared with tissues subjected to the same cooling rate without an electric current load. Thus, the effect of electric current load on cryopreservation and the potential of a new cryopreservation technique using electric current load were discussed based on these results. Copyright © 2016 Elsevier Inc. All rights reserved.

Solution Growth of a Novel Nonlinear Optical Material: L-Histidine Tetrafluoroborate

NASA Technical Reports Server (NTRS)

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

1998-01-01

Single crystals of L-Histidine tetrafluoroborate (L-HFB), a semiorganic nonlinear optical (NLO) material have been successfully grown by the temperature lowering and evaporation methods in our laboratory. Solubility curves of L-HFB have been determined in different solvents, such as water, ethanol and acetone. The solubility of L-HFB is very low in acetone, and ethanol, therefore, it is not feasible to grow L-HFB single crystals using these solvents. Good quality single crystals of a novel nonlinear optical material L-HFB have been grown from aqueous solution. Effects of seed orientation on morphologies of L-HFB crystals were studied. The advantages and disadvantage of both the evaporation and the temperature lowering techniques are compared. The single crystals in size 20 x 20 x 10 cubic mm were grown with deionized water as solvent in two weeks with an approximate growth rate of 1.4mm/day. The transmission range for these crystals has been found to be from 250 nm to 1500 nm.

Inferring the effects of compositional boundary layers on crystal nucleation, growth textures, and mineral chemistry in natural volcanic tephras through submicron-resolution imaging

NASA Astrophysics Data System (ADS)

Zellmer, Georg; Sakamoto, Naoya; Hwang, Shyh-Lung; Matsuda, Nozomi; Iizuka, Yoshiyuki; Moebis, Anja; Yurimoto, Hisayoshi

2016-09-01

Crystal nucleation and growth are first order processes captured in volcanic rocks and record important information about the rates of magmatic processes and chemical evolution of magmas during their ascent and eruption. We have studied glass-rich andesitic tephras from the Central Plateau of the Southern Taupo Volcanic Zone by electron- and ion-microbeam imaging techniques to investigate down to sub-micrometre scale the potential effects of compositional boundary layers (CBLs) of melt around crystals on the nucleation and growth of mineral phases and the chemistry of crystal growth zones. We find that CBLs may influence the types of mineral phases nucleating and growing, and growth textures such as the development of swallowtails. The chemistry of the CBLs also has the capacity to trigger intermittent overgrowths of nanometre-scale bands of different phases in rapidly growing crystals, resulting in what we refer to as cryptic phase zoning. The existence of cryptic phase zoning has implications for the interpretation of microprobe compositional data, and the resulting inferences made on the conditions of magmatic evolution. Identification of cryptic phase zoning may in future lead to more accurate thermobarometric estimates and thus geospeedometric constraints. In future, a more quantitative characterization of CBL formation and its effects on crystal nucleation and growth may contribute to a better understanding of melt rheology and magma ascent processes at the onset of explosive volcanic eruptions, and will likely be of benefit to hazard mitigation efforts.

Protein crystal growth

NASA Technical Reports Server (NTRS)

2001-01-01

Atomic force microscopy uses laser technology to reveal a defect, a double-screw dislocation, on the surface of this crystal of canavalin, a major source of dietary protein for humans and domestic animals. When a crystal grows, attachment kinetics and transport kinetics are competing for control of the molecules. As a molecule gets close to the crystal surface, it has to attach properly for the crystal to be usable. NASA has funded investigators to look at those attachment kinetics from a theoretical standpoint and an experimental standpoint. Dr. Alex McPherson of the University of California, Irvine, is one of those investigators. He uses X-ray diffraction and atomic force microscopy in his laboratory to answer some of the many questions about how protein crystals grow. Atomic force microscopy provides a means of looking at how individual molecules are added to the surface of growing protein crystals. This helps McPherson understand the kinetics of protein crystal growth. McPherson asks, How fast do crystals grow? What are the forces involved? Investigators funded by NASA have clearly shown that such factors as the level of supersaturation and the rate of growth all affect the habit [characteristic arrangement of facets] of the crystal and the defects that occur in the crystal.

Separation of CsCl from a Ternary CsCl-LiCl-KCl Salt via a Melt Crystallization Technique for Pyroprocessing Waste Minimization

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

Ammon Williams; Supathorn Phongikaroon; Michael Simpson

A parametric study has been conducted to identify the effects of several parameters on the separation of CsCl from molten LiCl-KCl salt via a melt crystallization process. A reverse vertical Bridgman technique was used to grow the salt crystals. The investigated parameters were: (1) the advancement rate, (2) the crucible lid configuration, (3) the amount of salt mixture, (4) the initial composition of CsCl, and (5) the temperature difference between the high and low furnace zones. From each grown crystal, samples were taken axially and analyzed using inductively coupled plasma mass spectrometry (ICP-MS). Results show that CsCl concentrations at themore » top of the crystals were low and increased to a maximum at the bottom of the salt. Salt (LiCl-KCl) recycle percentages for the experiments ranged from 50% to 75% and the CsCl composition in the waste salt was low. To increase the recycle percentage and the concentration of CsCl in the waste form, the possibility of using multiple crystallization stages was explored to further optimize the process. Results show that multiple crystallization stages are practical and the optimal experimental conditions should be operated at 5.0 mm/hr rate with a lid configuration and temperature difference of 200 °C for a total of five crystallization stages. Under these conditions, up to 88% of the salt can be recycled.« less

Raman intensity as a probe of concentration near a crystal growing in solution

NASA Technical Reports Server (NTRS)

Wilkinson, R. Allen

1989-01-01

The feasibility of using Raman spectral scattering signals for measurements of concentration profiles near a crystal interface during growth or dissolution is discussed. With KH2PO4 (KDP) as a test material, optical multichannel analyzer (OMA) detection of a solute Raman vibrational band provided direct quantification of solute concentration with band intensity. The intersection of incident laser and Raman collection optics provided 3-D selective point measurements of the solution concentration field. Unlike many other techniques, the Raman band intensity is not sensitive to the typical temperature variations. Precision calibration of Raman intensity versus KDP concentration with less than 1 pct standard deviation error levels was demonstrated. A fiber optic, which sampled incident laser intensity and coupled it to the OMA, provided a fully synchronized monitor of fluctuations in laser power to correlate with observed Raman signals. With 1 W of laser power at the sample, good data statistics required eight repeated data collections at approximately 2.5 min collection. The accumulated time represents the concentration measurement time at one spatial location. Photomicroscopy documented a 30 micrometer diameter by 200 micrometer of laser Raman scattering region in the solution near the crystal surface. The laser beam was able to approach up to 25 micrometer from the crystal surface. However, a crystal surface reflected intensity contribution was weakly detectable. Nucleated microcrystals were seen in the crystal-growing solution. These microcrystals convect right up to the crystal surface and indicate no quiet diffusion region under normal gravity conditions. Translation of the solution cell with respect to the optics caused systematic intensity errors.

Transrotational Crystals Revealed by TEM in Crystallizing Amorphous Films: New Solid State Order or Novel Extended Imperfection?

NASA Astrophysics Data System (ADS)

Kolosov, Vladimir Yu.

2011-03-01

Uunusual transrotational structure is presented for crystal growth in thin amorphous films. Experimental results have been obtained for the microcrystals of different chemical nature (oxides, chalcogenides, metals and alloys) grown in thin films prepared by various methods. Basically we used transmission electron microscopy (TEM): our original bend contour technique combined with selected area diffraction (HREM, EDX and CBED used in due cases as well as AFM). The unusual phenomenon (also traced inside TEM in situ) resides in strong (up to the whole rotation per micrometer) regular internal bending of crystal lattice planes (transrotation) in a growing crystal. As a result permanent rotation of the lattice orientation (realized round an axis lying in the film plane) is revealed by TEM. Different geometries of transrotational nanostructures are described: cylindrical, ellipsoidal, etc. Such crystal with transrotational atom periodicity resembles ideal single crystal enclosed in a curved space. Transrotational crystals can be considered as endless 2.5 D analogy of nanotubes, nanonions. Transrotation is strongly increasing as the film gets thinner in the range 100-15 nm. Transrotations supplement well known dislocations (in crystals) and disclinations (in liquid crystals). Support of RF Ministry of Education and Science is acknowledged.

Large three-dimensional photonic crystals based on monocrystalline liquid crystal blue phases.

PubMed

Chen, Chun-Wei; Hou, Chien-Tsung; Li, Cheng-Chang; Jau, Hung-Chang; Wang, Chun-Ta; Hong, Ching-Lang; Guo, Duan-Yi; Wang, Cheng-Yu; Chiang, Sheng-Ping; Bunning, Timothy J; Khoo, Iam-Choon; Lin, Tsung-Hsien

2017-09-28

Although there have been intense efforts to fabricate large three-dimensional photonic crystals in order to realize their full potential, the technologies developed so far are still beset with various material processing and cost issues. Conventional top-down fabrications are costly and time-consuming, whereas natural self-assembly and bottom-up fabrications often result in high defect density and limited dimensions. Here we report the fabrication of extraordinarily large monocrystalline photonic crystals by controlling the self-assembly processes which occur in unique phases of liquid crystals that exhibit three-dimensional photonic-crystalline properties called liquid-crystal blue phases. In particular, we have developed a gradient-temperature technique that enables three-dimensional photonic crystals to grow to lateral dimensions of ~1 cm (~30,000 of unit cells) and thickness of ~100 μm (~ 300 unit cells). These giant single crystals exhibit extraordinarily sharp photonic bandgaps with high reflectivity, long-range periodicity in all dimensions and well-defined lattice orientation.Conventional fabrication approaches for large-size three-dimensional photonic crystals are problematic. By properly controlling the self-assembly processes, the authors report the fabrication of monocrystalline blue phase liquid crystals that exhibit three-dimensional photonic-crystalline properties.

Apparatus for growing crystals

NASA Technical Reports Server (NTRS)

Jasinski, Thomas J. (Inventor); Witt, August F. (Inventor)

1986-01-01

An improved apparatus and method for growing crystals from a melt employing a heat pipe, consisting of one or more sections, each section serving to control temperature and thermal gradients in the crystal as it forms inside the pipe.

Stability of Detached Solidification

NASA Technical Reports Server (NTRS)

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

2009-01-01

Bridgman crystal growth can be conducted in the so-called "detached" solidification regime, where the growing crystal is detached from the crucible wall. A small gap between the growing crystal and the crucible wall, of the order of 100 micrometers or less, can be maintained during the process. A meniscus is formed at the bottom of the melt between the crystal and crucible wall. Under proper conditions, growth can proceed without collapsing the meniscus. The meniscus shape plays a key role in stabilizing the process. Thermal and other process parameters can also affect the geometrical steady-state stability conditions of solidification. The dynamic stability theory of the shaped crystal growth process has been developed by Tatarchenko. It consists of finding a simplified autonomous set of differential equations for the radius, height, and possibly other process parameters. The problem then reduces to analyzing a system of first order linear differential equations for stability. Here we apply a modified version of this theory for a particular case of detached solidification. Approximate analytical formulas as well as accurate numerical values for the capillary stability coefficients are presented. They display an unexpected singularity as a function of pressure differential. A novel approach to study the thermal field effects on the crystal shape stability has been proposed. In essence, it rectifies the unphysical assumption of the model that utilizes a perturbation of the crystal radius along the axis as being instantaneous. It consists of introducing time delay effects into the mathematical description and leads, in general, to stability over a broader parameter range. We believe that this novel treatment can be advantageously implemented in stability analyses of other crystal growth techniques such as Czochralski and float zone methods.

Microgravity

NASA Image and Video Library

2001-06-06

Atomic force microscopy uses laser technology to reveal a defect, a double-screw dislocation, on the surface of this crystal of canavalin, a major source of dietary protein for humans and domestic animals. When a crystal grows, attachment kinetics and transport kinetics are competing for control of the molecules. As a molecule gets close to the crystal surface, it has to attach properly for the crystal to be usable. NASA has funded investigators to look at those attachment kinetics from a theoretical standpoint and an experimental standpoint. Dr. Alex McPherson of the University of California, Irvine, is one of those investigators. He uses X-ray diffraction and atomic force microscopy in his laboratory to answer some of the many questions about how protein crystals grow. Atomic force microscopy provides a means of looking at how individual molecules are added to the surface of growing protein crystals. This helps McPherson understand the kinetics of protein crystal growth. McPherson asks, How fast do crystals grow? What are the forces involved? Investigators funded by NASA have clearly shown that such factors as the level of supersaturation and the rate of growth all affect the habit [characteristic arrangement of facets] of the crystal and the defects that occur in the crystal.

Celebrating the International Year of Crystallography with a Wisconsin High School Crystal Growing Competition

ERIC Educational Resources Information Center

Guzei, Ilia A.

2014-01-01

In honor of the 2014 International Year of Crystallography, the first Wisconsin Crystal Growing Competition was successfully organized and conducted. High school students from 26 schools across the state competed for prizes by growing large crystals of CuSO[subscript4]·5(H[subscript2]O). This paper describes how the event was planned and carried…

Electrochemical deposition of silver crystals aboard Skylab 4

NASA Technical Reports Server (NTRS)

Grodzka, P. G.; Facemire, B. R.; Johnston, M. H.; Gates, D. W.

1976-01-01

Silver crystals were grown aboard Skylab 4 by an electro-chemical reaction and subsequently returned to earth for comparison with crystals grown at 1- and 5-g. Both the Skylab and earth-grown crystals show a variety of structures. Certain tendencies in structure dependency on gravity level, however, can be discerned. In addition, downward growing dendrite streamers; upward growing chunky crystal streamers; growth along an air/liquid interface; and ribbon, film, and fiber crystal habits were observed in experiments conducted on the ground with solutions of varying concentrations. It was also observed that the crystal structures of space and ground electro-deposited silver crystals were very similar to the structures of germanium selenide and germanium telluride crystals grown in space and on the ground by a vapor transport technique. Consideration of the data leads to the conclusions that: (1) the rate of electrochemical displacement of silver ions from a 5 percent aqueous solution by copper is predominantly diffussion controlled in space and kinetically controlled in 1- and higher-g because of augmentation of mass transport by convection; (2) downward and upward crystal streamers are the result of gravity-driven convection, the flow patterns of which can be delineated. Lateral growths along an air/liquid interface are the result of surface-tension-driven convection, the pattern of which also can be delineated; (3) electrolysis in space or low-g environments can produce either dendritic crystals with more perfect microcrystalline structures or massive, single crystals with fewer defects than those grown on ground or at higher g-levels. Ribbons or films of space-grown silicon crystals would find a ready market for electronic substrate and photocell applications. Space-grown dendritic, metal crystals present the possibility of unique catalysts. Large perfect crystals of various materials are desired for a number of electronic and optical applications; and (4) vapor transport growth of germanium selenide and germanium telluride is affected by convection mechanisms similar to the mechanisms hypothesized for the electrochemical deposition of silver crystals. Evidence and considerations leading to the preceding summaries and conclusions are presented. The implications of the findings and conclusions for technological applications are discussed, and recommendations for further experiments are presented.

Process for the homoepitaxial growth of single-crystal silicon carbide films on silicon carbide wafers

NASA Technical Reports Server (NTRS)

Powell, J. Anthony (Inventor)

1993-01-01

The invention is a method for growing homoepitaxial films of SiC on low tilt angle vicinal (0001) SiC wafers. The invention proposes and teaches a new theoretical model for the homoepitaxial growth of SiC films on (0001) SiC substrates. The inventive method consists of preparing the growth surface of SiC wafers slightly off-axis (from less the 0.1 to 6 deg) from the (0001) plane, subjecting the growth surface to a suitable etch, and then growing the homoepitaxial film using conventional SiC growth techniques.

Low Temperature Photoluminescence Characterization of Orbitally Grown CdZnTe

NASA Technical Reports Server (NTRS)

Ritter, Timothy M.; Larson, D. J.

1998-01-01

The II-VI ternary alloy CdZnTe is a technologically important material because of its use as a lattice matched substrate for HgCdTe based devices. The increasingly stringent requirements on performance that must be met by such large area infrared detectors also necessitates a higher quality substrate. Such substrate material is typically grown using the Bridgman technique. Due to the nature of bulk semiconductor growth, gravitationally dependent phenomena can adversely affect crystalline quality. The most direct way to alleviate this problem is by crystal growth in a reduced gravity environment. Since it requires hours, even days, to grow a high quality crystal, an orbiting space shuttle or space station provides a superb platform on which to conduct such research. For well over ten years NASA has been studying the effects of microgravity semiconductor crystal growth. This paper reports the results of photoluminescence characterization performed on an arbitrary grown CdZnTe bulk crystal.

Self-adjusted flux for the traveling solvent floating zone growth of YBaCuFeO5 crystal

NASA Astrophysics Data System (ADS)

Lai, Yen-Chung; Shu, Guo-Jiun; Chen, Wei-Tin; Du, Chao-Hung; Chou, Fang-Cheng

2015-03-01

A modified traveling solvent floating zone (TSFZ) technique was used to successfully grow a large size and high quality single crystal of multiferroic material YBaCuFeO5. This modified TSFZ growth uses a stoichiometric feed rod and pure copper oxide as the initial flux without prior knowledge of the complex phase diagram involving four elements, and the optimal flux for the growth of incongruently melt crystal is self-adjusted after a prolonged stable pulling. The wetting of the feed rod edge that often perturbs the molten zone stability was avoided by adding 2 wt% B2O3. The optimal flux concentration for the YBaCuFeO5 growth can be extracted to be near YBaCuFeO5:CuO=13:87 in molar ratio. The crystal quality was confirmed by the satisfactory refinement of crystal structure of space group P4mm and the two consecutive anisotropic antiferromagnetic phase transitions near 455 K and 170 K.

A numerical study of steady crystal growth in a vertical Bridgman device

NASA Astrophysics Data System (ADS)

Jalics, Miklos Kalman

Electronics based on semiconductors creates an enormous demand for high quality semiconductor single crystals. The vertical Bridgman device is commonly used for growing single crystals for a variety of materials such as GaAs, InP and HgCdTe. A mathematical model is presented for steady crystal growth under conditions where crystal growth is determined strictly by heat transfer. The ends of the ampoule are chosen far away from the insulation zone to allow for steady growth. A numerical solution is sought for this mathematical model. The equations are transformed into a rectangular geometry and appropriate finite difference techniques are applied on the transformed equations. Newton's method solves the nonlinear problem. To improve efficiency GMRES with preconditioning is used to compute the Newton iterates. The numerical results are used to compare with two current asymptotic theories that assume small Biot numbers. Results indicate that one of the asymptotic theories is accurate for even moderate Biot numbers.

Thermal, Dielectric Studies on Pure and Amino Acid L-Glutamic Acid, L-Histidine L-Valine Doped Potassium Dihydrogen Phosphate Single Crystals

NASA Astrophysics Data System (ADS)

Kumaresan, P.; Babu, S. Moorthy; Anbarasan, P. M.

Amino acids (L-Glutamic acid, L-Histidine, L-Valine) doped potassium dihydrogen phosphate crystals were grown by the solution growth technique. Slow cooling as well as slow evaporation methods were employed to grow these crystals. The concentration of dopants in the mother solution was varied from 0.1 mole % to 10 mole %. The solubility data for all dopant concentrations were determined. The variation in pH and the corresponding habit modification of the grown crystals were characterized with UV - VIS, FT-IR and SHG trace elements, and dielectric studies reveal slight distortion of lattice parameter for the heavily doped KDP crystals. TGA-DTA studies reveal good thermal stability. The dopants increase the hardness value of the material, which also depends on the concentration of the dopants. Amino acids doping improved the NLO properties. The detailed results on the spectral parameters, habit modifications and constant values will be presented.

Crack - seal veins - what we learnt since the seminal work of John Ramsay

NASA Astrophysics Data System (ADS)

Urai, Janos L.; Bons, Paul D.

2017-04-01

In the nineteen-eighties, John Ramsay and co-workers have laid the basis for much of our current understanding of tectonic veins, by proposing that tectonic veins accrete in many small increments of cracking and sealing, making the link to cyclic stress and fluid pressure cycles and the earthquake cycle, and by proposing that fibrous veins track the opening trajectory, which has created a toolbox to analyse progressive deformation in rocks. They recognised syntaxial and antitaxial veins, which grow depending on the composition of the wall rock and the vein. Following on these seminal contributions, advances in analysing the microstructure and chemical signature in crack-seal veins made a lot of progress, facilitated by the rapid increase in micro analytical tools like cathodeluminescence and EBSD. Initial modelling of crystal growth in crack- seal veins provided an explanation of how crystals become fibrous without being deformed and explained how fibres sometimes do and sometimes don't follow the opening trajectory. This was followed by numerical models of crystal growth to study the development of crystal facets after larger crack increments, and experimental study of the sealing dynamics of syntaxial veins. These models were initially kinematic, using the ELLE microdynamic simulation package, and more recently incorporating the physics of the growing interface using the Phase Field method, which now allows 3D simulation of both syntaxial and antitaxial veins and can simultaneously compute the evolving permeability of the crack using Lattice Boltzmann techniques. Parallel to these developments we developed an understanding of the strength of the vein cement, and, using Discrete Element Techniques, explored the effects of differences of the strength of the vein and its adhesion to the wall rock on fracture patterns in crack-seal systems in changing stress fields. This presentation will review these developments, showing how the ideas of John Ramsay inspired follow up work leading to a much better understanding of the complex feedback systems between fracture growth, crystal growth and fluid flow in crack-seal systems.

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.

Protein Crystal Growth

NASA Technical Reports Server (NTRS)

2003-01-01

In order to rapidly and efficiently grow crystals, tools were needed to automatically identify and analyze the growing process of protein crystals. To meet this need, Diversified Scientific, Inc. (DSI), with the support of a Small Business Innovation Research (SBIR) contract from NASA s Marshall Space Flight Center, developed CrystalScore(trademark), the first automated image acquisition, analysis, and archiving system designed specifically for the macromolecular crystal growing community. It offers automated hardware control, image and data archiving, image processing, a searchable database, and surface plotting of experimental data. CrystalScore is currently being used by numerous pharmaceutical companies and academic and nonprofit research centers. DSI, located in Birmingham, Alabama, was awarded the patent Method for acquiring, storing, and analyzing crystal images on March 4, 2003. Another DSI product made possible by Marshall SBIR funding is VaporPro(trademark), a unique, comprehensive system that allows for the automated control of vapor diffusion for crystallization experiments.

Oriented bottom-up growth of armchair graphene nanoribbons on germanium

DOEpatents

Arnold, Michael Scott; Jacobberger, Robert Michael

2016-03-15

Graphene nanoribbon arrays, methods of growing graphene nanoribbon arrays and electronic and photonic devices incorporating the graphene nanoribbon arrays are provided. The graphene nanoribbons in the arrays are formed using a scalable, bottom-up, chemical vapor deposition (CVD) technique in which the (001) facet of the germanium is used to orient the graphene nanoribbon crystals along the [110] directions of the germanium.

Pharmaceutical Cocrystals and Their Physicochemical Properties

PubMed Central

2009-01-01

Over the last 20 years, the number of publications outlining the advances in design strategies, growing techniques, and characterization of cocrystals has continued to increase significantly within the crystal engineering field. However, only within the last decade have cocrystals found their place in pharmaceuticals, primarily due to their ability to alter physicochemical properties without compromising the structural integrity of the active pharmaceutical ingredient (API) and thus, possibly, the bioactivity. This review article will highlight and discuss the advances made over the last 10 years pertaining to physical and chemical property improvements through pharmaceutical cocrystalline materials and, hopefully, draw closer the fields of crystal engineering and pharmaceutical sciences. PMID:19503732

Study of the possibility of growing germanium single crystals under low temperature gradients

NASA Astrophysics Data System (ADS)

Moskovskih, V. A.; Kasimkin, P. V.; Shlegel, V. N.; Vasiliev, Y. V.; Gridchin, V. A.; Podkopaev, O. I.; Zhdankov, V. N.

2014-03-01

The possibility of growing germanium single crystals under low temperature gradients in order to produce a dislocation-free material has been studied. Germanium crystals with a dislocation density of about 100-200 cm-2 have been grown in a system with a weight control of crystal growth at maximum axial gradients of about 1.5 K/cm.

Using Depletion Force to synthesize PBG crystals

NASA Astrophysics Data System (ADS)

Sanyal, Subrata; Zhang, Jian; Lin, Keng-Hui; Work, William J.; Yodh, A. G.

2000-03-01

Using the pathway of depletion-mediated crystallization, we have undertaken an exhaustive set of experiments in order to synthesize materials with novel optical and rheological properties, e.g., photonic bandgap (PBG) crystals. With the primary use of miceller depletion, we grow crystals of submicron-sized model colloidal (e.g., aqueous suspensions of polyballs or silica) particles from the walls of our sample microchambers, used for optical microscopy. Furthermore, the order of such crystals can be controlled by patterning one of the cell walls(K. H. Lin et al.), Manuscript under preparation (1999)., and after the formation of crystals the particles can be ``locked'' in their positions using chemical techniques(G. Pan et al.), Phys. Rev. Lett., 78, 3860 (1997); P. V. Braun (private communication).. The locked arrangements of particles serve as templates to fabricate(B. T. Holland et al.), Science, 281, 538 (1998); J. E. G. J. Wijnhoven et al., Science, 281, 802 (1998). microporous PBG materials. Experiments are underway to synthesize solid microspheres of high dielectric constant materials, and hollow microspheres, that can be arranged on patterned surfaces.

Growing Crystals on the Ceiling.

ERIC Educational Resources Information Center

Christman, Robert A.

1980-01-01

Described is a method of studying growing crystals in a classroom utilizing a carrousel projector standing vertically. A saturated salt solution is placed on a slide on the lens of the projector and the heat from the projector causes the water to evaporate and salt to crystalize. (Author/DS)

On the Role of Boron in CdTe and CdZnTe Crystals

NASA Astrophysics Data System (ADS)

Pavesi, M.; Marchini, L.; Zha, M.; Zappettini, A.; Zanichelli, M.; Manfredi, M.

2011-10-01

It is well known that group III elements act as donors if they play a substitutional role at the metallic site in II-tellurides; nevertheless, several studies report both on the creation of complexes with vacancies, named A-centers, and on the involvement in self-compensation mechanisms, especially for indium. The boron concentration in II-tellurides is negligible, and its contribution to transport mechanisms has not been studied yet. For the last few years the authors have been developing a new technique to grow CdZnTe by the vertical Bridgman technique, taking advantage of encapsulation by means of boron oxide. In this way, crystals characterized by large single grains, low etch pit density, and high resistivity have been obtained. Recently, x-ray detectors with state-of-the-art performance have been produced from such crystals. Boron contamination, as a consequence of this growth method, is quite low but at least one order of magnitude above values obtained with other growth techniques. Besides being a low-cost technique which is also suitable for large-scale mass production, the encapsulated vertical Bridgman technique is quite useful to prevent dislocations, grain boundaries, and stacking faults; for these reasons, careful characterization was performed to understand the effect of boron both on the electrical properties and on the spectroscopic performance of the final crystals. Our characterization is mainly based on low-temperature photoluminescence in addition to electrical current-voltage measurements, photostimulated current, and x-ray spectroscopy. The results indicate that boron behaves like other group III elements; in fact, boron forms a complex that does not affect the good performance of our x-ray detectors, even if it shows some properties which are typical of A-centers.

A Fundamental Study of Inorganic Clathrate and Other Open-Framework Materials

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

Nolas, George

Due to formidable synthetic challenges, many materials of scientific and technological interest are first obtained as microcrystalline powders. High purity, high yield processing techniques are often lacking and thus care must be taken in interpretation of the observed structural, chemical, and physical properties of powder or polycrystalline materials, which can be strongly influenced by extrinsic properties. Furthermore, the preparation of high-quality single crystals for many materials by traditional techniques can be especially challenging in cases where the elemental constituents have greatly differing melting points and/or vapor pressures, when the desired compound is thermodynamically metastable, or where growth with participation ofmore » the melt is generally not possible. New processing techniques are therefore imperative in order to investigate the intrinsic properties of these materials and elucidate their fundamental physical properties. Intermetallic clathrates constitute one such class of materials. The complex crystal structures of intermetallic clathrates are characterized by mainly group 14 host frameworks encapsulating guest-ions in polyhedral cages. The unique features of clathrate structures are intimately related to their physical properties, offering ideal systems for the study of structure-property relationships in crystalline solids. Moreover, intermetallic clathrates are being actively investigated due to their potential for application in thermoelectrics, photovoltaics and opto-electronics, superconductivity, and magnetocaloric technologies. We have developed different processing techniques in order to synthesize phase-pure high yield clathrates reproducibly, as well as grow single crystals for the first time. We also employed these techniques to synthesize new “open-framework” compounds. These advances in materials processing and crystal growth allowed for the investigation of the physical properties of a variety of different clathrate compositions for the first time.« less

Apparatus for growing HgI.sub.2 crystals

DOEpatents

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

1978-01-01

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.

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.

Divalent europium doped and un-doped calcium iodide scintillators: Scintillator characterization and single crystal growth

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

Boatner, L. A.; Ramey, J. O.; Kolopus, J. A.

2015-02-21

Initially, the alkaline-earth scintillator, CaI 2:Eu 2+, was discovered around 1964 by Hofstadter, Odell, and Schmidt. Serious practical problems quickly arose, however, that were associated with the growth of large monolithic single crystals of this material due to its lamellar, mica-like structure. As a result of its theoretically higher light yield, CaI 2:Eu 2+ has the potential to exceed the excellent scintillation performance of SrI 2:Eu 2+. In fact, theoretical predictions for the light yield of CaI2:Eu 2+ scintillators suggested that an energy resolution approaching 2% at 662 keV could be achievable. Like the early SrI 2:Eu 2+ scintillator, themore » performance of CaI 2:Eu 2+ scintillators has traditionally suffered due, at least in part, to outdated materials synthesis, component stoichiometry/purity, and single-crystal-growth techniques. Based on our recent work on SrI 2:Eu 2+ scintillators in single-crystal form, we have developed new techniques that are applied here to CaI 2:Eu 2+ and pure CaI 2 with the goal of growing large un-cracked crystals and, potentially, realizing the theoretically predicted performance of the CaI 2:Eu 2+ form of this material. Calcium iodide does not adhere to modern glassy carbon Bridgman crucibles - so there should be no differential thermal-contraction-induced crystal/crucible stresses on cooling that would result in crystal cracking of the lamellar structure of CaI 2. Here we apply glassy carbon crucible Bridgman growth, high-purity growth-charge compounds, our molten salt processing/filtration technique, and extended vacuum-melt-pumping methods to the growth of both CaI 2:Eu 2+ and un-doped CaI 2. Moreover, large scintillating single crystals were obtained, and detailed characterization studies of the scintillation properties of CaI 2:Eu 2+ and pure CaI 2 single crystals are presented that include studies of the effects of plastic deformation of the crystals on the scintillator performance.« less

Early stages of carbonate mineralization revealed from molecular simulations: Implications for biomineral formation

NASA Astrophysics Data System (ADS)

Wallace, A. F.; DeYoreo, J.; Banfield, J. F.

2011-12-01

The carbonate mineral constituents of many biomineralized products, formed both in and ex vivo, grow by a multi-stage crystallization process that involves the nucleation and structural reorganization of transient amorphous phases. The existence of transient phases and cluster species has significant implications for carbonate nucleation and growth in natural and engineered environments, both modern and ancient. The structure of these intermediate phases remains elusive, as does the nature of the disorder to order transition, however, these process details may strongly influence the interpretation of elemental and isotopic climate proxy data obtained from authigenic and biogenic carbonates. While molecular simulations have been applied to certain aspects of crystal growth, studies of metal carbonate nucleation are strongly inhibited by the presence of kinetic traps that prevent adequate sampling of the potential landscape upon which the growing clusters reside within timescales accessible by simulation. This research addresses this challenge by marrying the recent Kawska-Zahn (KZ) approach to simulation of crystal nucleation and growth from solution with replica-exchange molecular dynamics (REMD) techniques. REMD has been used previously to enhance sampling of protein conformations that occupy energy wells that are separated by sizable thermodynamic and kinetic barriers, and is used here to probe the initial formation and onset of order within hydrated calcium and iron carbonate cluster species during nucleation. Results to date suggest that growing clusters initiate as short linear ion chains that evolve into two- and three-dimensional structures with continued growth. The planar structures exhibit an obvious 2d lattice, while establishment of a 3d lattice is hindered by incomplete ion desolvation. The formation of a dehydrated core consisting of a single carbonate ion is observed when the clusters are ~0.75 nm. At the same size a distorted, but discernible calcite-type lattice is also apparent. Continued growth results in expansion of the dehydrated core, however, complete desolvation and incorporation of cations into the growing carbonate phase is not achieved until the cluster grows to ~1.2 nm. Exploration of the system free energy along the crystallization path reveals "special" cluster sizes that correlate with ion desolvation milestones. The formation of these species comprise critical bottlenecks on the energy landscape and for the establishment of order within the growing clusters.

Numerical simulation of flow and mass transfer for large KDP crystal growth via solution-jet method

NASA Astrophysics Data System (ADS)

Yin, Huawei; Li, Mingwei; Hu, Zhitao; Zhou, Chuan; Li, Zhiwei

2018-06-01

A novel technique of growing large crystals of potassium dihydrogen phosphate (KDP) named solution-jet method is proposed. The aim is to increase supersaturation on the pyramidal face, especially for crystal surface regions close to the rotation axis. The fluid flow and surface supersaturation distribution of crystals grown under different conditions were computed using the finite-volume method. Results indicate that the time-averaged supersaturation of the pyramidal face in the proposed method significantly increases and the supersaturation difference from the crystal center to edge clearly decreases compared with the rotating-crystal method. With increased jet velocity, supersaturation on the pyramidal face steadily increases. Rotation rate considerably affects the magnitude and distribution of the prismatic surface supersaturation. With increased crystal size, the mean value of surface supersaturation averaged over the pyramid gradually decreases; conversely, standard deviation increases, which is detrimental to crystal growth. Moreover, the significant roles played by natural and forced convection in the process of mass transport are discussed. Results show that further increased jet velocity to 0.6 m/s renders negligible the effects of natural convection around the pyramid. The simulation for step propagation indicates that solution-jet method can promote a steady step migration and enhance surface morphology stability, which can improve the crystal quality.

Thermal, dielectric studies on pure and amino acid ( L-glutamic acid, L-histidine, L-valine) doped KDP single crystals

NASA Astrophysics Data System (ADS)

Kumaresan, P.; Moorthy Babu, S.; Anbarasan, P. M.

2008-05-01

Amino acids ( L-glutamic acid, L-histidine, L-valine) doped potassium dihydrogen phospate crystals are grown by solution growth technique. Slow cooling as well as slow evaporation methods were employed to grow these crystals. The concentration of dopants in the mother solution was varied from 0.1 mol% to 10 mol%. The solubility data for all dopants concentration were determined. There is variation in pH value and hence, there is habit modification of the grown crystals were characterized with UV-VIS, FT-IR studies, SHG trace elements and dielectric studies reveal slight distortion of lattice parameter for the heavily doped KDP crystals. UV-Visible spectra confirm the improvement in the transparency of these crystals on doping metal ions. FT-IR spectra reveal strong absorption band between 1400 and 1600 cm -1 for metal ion doped crystals. TGA-DTA studies reveal good thermal stability. The dopants increase the hardness value of the material and it also depends on the concentration of the dopants. Amino acids doping improved the NLO properties. The detailed results on the spectral parameters, habit modifications and constant values will be presented.

Inkjet printing of single-crystal films.

PubMed

Minemawari, Hiromi; Yamada, Toshikazu; Matsui, Hiroyuki; Tsutsumi, Jun'ya; Haas, Simon; Chiba, Ryosuke; Kumai, Reiji; Hasegawa, Tatsuo

2011-07-13

The use of single crystals has been fundamental to the development of semiconductor microelectronics and solid-state science. Whether based on inorganic or organic materials, the devices that show the highest performance rely on single-crystal interfaces, with their nearly perfect translational symmetry and exceptionally high chemical purity. Attention has recently been focused on developing simple ways of producing electronic devices by means of printing technologies. 'Printed electronics' is being explored for the manufacture of large-area and flexible electronic devices by the patterned application of functional inks containing soluble or dispersed semiconducting materials. However, because of the strong self-organizing tendency of the deposited materials, the production of semiconducting thin films of high crystallinity (indispensable for realizing high carrier mobility) may be incompatible with conventional printing processes. Here we develop a method that combines the technique of antisolvent crystallization with inkjet printing to produce organic semiconducting thin films of high crystallinity. Specifically, we show that mixing fine droplets of an antisolvent and a solution of an active semiconducting component within a confined area on an amorphous substrate can trigger the controlled formation of exceptionally uniform single-crystal or polycrystalline thin films that grow at the liquid-air interfaces. Using this approach, we have printed single crystals of the organic semiconductor 2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene (C(8)-BTBT) (ref. 15), yielding thin-film transistors with average carrier mobilities as high as 16.4 cm(2) V(-1) s(-1). This printing technique constitutes a major step towards the use of high-performance single-crystal semiconductor devices for large-area and flexible electronics applications.

Gallium arsenide single crystal solar cell structure and method of making

NASA Technical Reports Server (NTRS)

Stirn, Richard J. (Inventor)

1983-01-01

A production method and structure for a thin-film GaAs crystal for a solar cell on a single-crystal silicon substrate (10) comprising the steps of growing a single-crystal interlayer (12) of material having a closer match in lattice and thermal expansion with single-crystal GaAs than the single-crystal silicon of the substrate, and epitaxially growing a single-crystal film (14) on the interlayer. The material of the interlayer may be germanium or graded germanium-silicon alloy, with low germanium content at the silicon substrate interface, and high germanium content at the upper surface. The surface of the interface layer (12) is annealed for recrystallization by a pulsed beam of energy (laser or electron) prior to growing the interlayer. The solar cell structure may be grown as a single-crystal n.sup.+ /p shallow homojunction film or as a p/n or n/p junction film. A Ga(Al)AS heteroface film may be grown over the GaAs film.

Investigation of single crystal ferrite thin films

NASA Technical Reports Server (NTRS)

Mee, J. E.; Besser, P. J.; Elkins, P. E.; Glass, H. L.; Whitcomb, E. C.

1972-01-01

Materials suitable for use in magnetic bubble domain memories were developed for aerospace applications. Practical techniques for the preparation of such materials in forms required for fabrication of computer memory devices were considered. The materials studied were epitaxial films of various compositions of the gallium-substituted yttrium gadolinium iron garnet system. The major emphasis was to determine their bubble properties and the conditions necessary for growing uncracked, high quality films.

Growth and transfer of monolithic horizontal nanowire superstructures onto flexible substrates

DOEpatents

Wang, Zhong L; Xu, Sheng

2013-08-27

In a method of making a monolithic elongated nanowire, a mask polymer layer is applied to a selected crystal surface of a seed crystal. A plurality of spaced apart elongated openings is defined through the mask polymer layer, thereby exposing a corresponding plurality of portions of the crystal surface. The openings are disposed so as to be aligned with and parallel to a selected crystal axis of the seed crystal. The portions of the crystal surface are subjected to a chemical nutrient environment that causes crystalline material to grow from the plurality of portions for at least a period of time so that monocrystalline members grow from the elongated openings and until the monocrystalline members laterally expand so that each monocrystalline member grows into and merges with an adjacent one of the monocrystalline members, thereby forming a monolithic elongated nanowire.

Using Synchrotron Radiation and Electron Microscopy to Map the Huge Structural Changes that Occur in Viruses During Their Life Cycle

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

Rossman, Michael

2011-09-07

The crystallographic techniques for structure determination of proteins and neucleic acids at near atomic resolution using synchrotron X-radiation has become almost automatic. However the limits of this procedure are determined by the availability of crystals. As the size and complexity of the molecular assemblies being studied increases, the likelihood of growing useful crystals diminishes. Cryo electron microscopy and tomography have extended the range of biological objects that can be determined at near atomic resolution. Furthermore it is now becoming apparent that the function of the molecular assemblies most often requires very large conformational changes that could never be contained withinmore » a crystal, Examples will be presented of the structural changes that occur in viruses as they assembly and prepare to infect new cells.« less

Advantage of low-temperature hydrothermal synthesis to grow stoichiometric crednerite crystals

NASA Astrophysics Data System (ADS)

Poienar, Maria; Martin, Christine; Lebedev, Oleg I.; Maignan, Antoine

2018-06-01

This work reports a new approach for the growth of stoichiometric crednerite CuMnO2 crystals. The hydrothermal reaction, starting from soluble metal sulphates as precursors, is assisted by ethylene glycol and the formation of crednerite is found to depend strongly on pH and temperature. This method allows obtaining small hexagonal platelets with the larger dimension about 1.0-1.5 μm and with a composition characterized by a Cu/Mn ratio of 1. Thus, these crystals differ from the needle-like millimetric ones obtained by the flux technique for which the composition departs from the expected one and is close to Cu1.04Mn0.96. This monitoring of the cationic composition in crednerite, using hydrothermal synthesis, is important as the Cu/Mn ratio controls the low temperature antiferromagnetic ground-state.

Crystallization Mechanism and Charge Carrier Transport in MAPLE-Deposited Conjugated Polymer Thin Films

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

Dong, Ban Xuan; Strzalka, Joseph; Jiang, Zhang

Although spin casting and chemical surface reactions are the most common methods used for fabricating functional polymer films onto substrates, they are limited with regard to producing films of certain morphological characteristics on different wetting and nonwetting substrates. The matrix-assisted pulsed laser evaporation (MAPLE) technique offers advantages with regard to producing films of different morphologies on different types of substrates. Here, we provide a quantitative characterization, using X-ray diffraction and optical methods, to elucidate the additive growth mechanism of MAPLE-deposited poly(3-hexylthiophene) (P3HT) films on substrates that have undergone different surface treatments, enabling them to possess different wettabilities. We show thatmore » MAPLE-deposited films are composed of crystalline phases, wherein the overall P3HT aggregate size and crystallite coherence length increase with deposition time. A complete pole figure constructed from X-ray diffraction measurements reveals that in these MAPLE-deposited films, there exist two distinct crystallite populations: (i) highly oriented crystals that grow from the flat dielectric substrate and (ii) misoriented crystals that preferentially grow on top of the existing polymer layers. The growth of the highly oriented crystals is highly sensitive to the chemistry of the substrate, whereas the effect of substrate chemistry on misoriented crystal growth is weaker. The use of a self-assembled monolayer to treat the substrate greatly enhances the population and crystallite coherence length at the buried interfaces, particularly during the early stage of deposition. Furthermore, the evolution of the in-plane carrier mobilities during the course of deposition is consistent with the development of highly oriented crystals at the buried interface, suggesting that this interface plays a key role toward determining carrier transport in organic thin-film transistors.« less

Crystallization Mechanism and Charge Carrier Transport in MAPLE-Deposited Conjugated Polymer Thin Films

DOE PAGES

Dong, Ban Xuan; Strzalka, Joseph; Jiang, Zhang; ...

2017-11-23

Although spin casting and chemical surface reactions are the most common methods used for fabricating functional polymer films onto substrates, they are limited with regard to producing films of certain morphological characteristics on different wetting and nonwetting substrates. The matrix-assisted pulsed laser evaporation (MAPLE) technique offers advantages with regard to producing films of different morphologies on different types of substrates. Here, we provide a quantitative characterization, using X-ray diffraction and optical methods, to elucidate the additive growth mechanism of MAPLE-deposited poly(3-hexylthiophene) (P3HT) films on substrates that have undergone different surface treatments, enabling them to possess different wettabilities. We show thatmore » MAPLE-deposited films are composed of crystalline phases, wherein the overall P3HT aggregate size and crystallite coherence length increase with deposition time. A complete pole figure constructed from X-ray diffraction measurements reveals that in these MAPLE-deposited films, there exist two distinct crystallite populations: (i) highly oriented crystals that grow from the flat dielectric substrate and (ii) misoriented crystals that preferentially grow on top of the existing polymer layers. The growth of the highly oriented crystals is highly sensitive to the chemistry of the substrate, whereas the effect of substrate chemistry on misoriented crystal growth is weaker. The use of a self-assembled monolayer to treat the substrate greatly enhances the population and crystallite coherence length at the buried interfaces, particularly during the early stage of deposition. Furthermore, the evolution of the in-plane carrier mobilities during the course of deposition is consistent with the development of highly oriented crystals at the buried interface, suggesting that this interface plays a key role toward determining carrier transport in organic thin-film transistors.« less

Numerical modeling of crystal growth in Bridgman device

NASA Astrophysics Data System (ADS)

Vompe, Dmitry Aleksandrovich

1997-12-01

The standard model for the growth of a crystal from a pure substance or diluted binary mixture contains transport equations for heat and phase change conditions at the solidification front. A numerical method is constructed for simulations of crystal growth in a vertical Bridgman device. The method is based on a boundary fitting technique in which melted and solidified regions are mapped onto a fixed rectangular logical domain. The Alternating Directions scheme (ADI) is used to treat the diffusive terms implicitly, with explicit methods are used for the remaining terms in the mapped temperature equations with variable coefficients. The nonlinear equation for the solid/liquid interface motion is solved by the modified Euler technique. Results obtained from the calculations have been used to study the influence of various boundary conditions imposed on the sidewalls and the top and bottom of the ampoule. Conditions are identified that lead to a steadily growing crystal and results are compared with an asymptotic one- dimensional model. Criteria based on ampoule length and boundary conditions being derived and compared with a previously developed one-dimensional model. Various cases have been considered to determine conditions for maintaining a nearly flat interface. It was found that the interface amplitude can be decreased by a factor of 100 (even 1,000) by optimizing temperature boundary conditions.

Growth of single-crystal YAG fiber optics.

PubMed

Nie, Craig D; Bera, Subhabrata; Harrington, James A

2016-07-11

Single-crystal YAG (Y₃Al₅O₁₂) fibers have been grown by the laser heated pedestal growth technique with losses as low as 0.3 dB/m at 1.06 μm. These YAG fibers are as long as about 60 cm with diameters around 330 μm. The early fibers were grown from unoriented YAG seed fibers and these fibers exhibited facet steps or ridges on the surface of the fiber. However, recently we have grown fibers using an oriented seed to grow step-free fibers. Scattering losses made on the fibers indicate that the scattering losses are equal to about 30% of the total loss.

The Pressure induced by salt crystallization in confinement.

PubMed

Desarnaud, J; Bonn, D; Shahidzadeh, N

2016-08-05

Salt crystallization is a major cause of weathering of rocks, artworks and monuments. Damage can only occur if crystals continue to grow in confinement, i.e. within the pore space of these materials, thus generating mechanical stress. We report the direct measurement, at the microscale, of the force exerted by growing alkali halide salt crystals while visualizing their spontaneous nucleation and growth. The experiments reveal the crucial role of the wetting films between the growing crystal and the confining walls for the development of the pressure. Our results suggest that the measured force originates from repulsion between the similarly charged confining wall and the salt crystal separated by a ~1.5 nm liquid film. Indeed, if the walls are made hydrophobic, no film is observed and no repulsive forces are detected. We also show that the magnitude of the induced pressure is system specific explaining why different salts lead to different amounts of damage to porous materials.

Collection of Ni-bearing material from electroless plating waste by magnetic separation with HTS bulk magnet

NASA Astrophysics Data System (ADS)

Oka, T.; Fukazawa, H.; Fukui, S.; Ogawa, J.; Sato, T.; Ooizumi, M.; Tsujimura, M.; Yokoyama, K.

2014-01-01

The magnetic separation experiment to collect the Ni compounds from the waste liquid of electroless plating processes was conducted in the open-gradient magnetic separation process with the high temperature superconducting bulk magnet system. The magnetic pole containing Gd-based bulk superconductors was activated to 3.45 T at 35 K in the static magnetic field of 5 T with use of a superconducting solenoid magnet. The coarse Ni-sulfate crystals were formed by adding the concentrated sulfuric acid to the Ni-phosphite precipitates which yielded from the plating waste liquid by controlling the temperature and the pH value. The open-gradient magnetic separation technique was employed to separate the Ni-sulfate crystals from the mixture of the Ni-sulfate and Ni-phosphite compounds by the difference between their magnetic properties. And we succeeded in collecting Ni-sulfate crystals preferentially to the Ni-phosphite by attracting them to the magnetic pole soon after the Ni-sulfate crystals began to grow.

Neutron protein crystallography: A complementary tool for locating hydrogens in proteins.

PubMed

O'Dell, William B; Bodenheimer, Annette M; Meilleur, Flora

2016-07-15

Neutron protein crystallography is a powerful tool for investigating protein chemistry because it directly locates hydrogen atom positions in a protein structure. The visibility of hydrogen and deuterium atoms arises from the strong interaction of neutrons with the nuclei of these isotopes. Positions can be unambiguously assigned from diffraction at resolutions typical of protein crystals. Neutrons have the additional benefit to structural biology of not inducing radiation damage in protein crystals. The same crystal could be measured multiple times for parametric studies. Here, we review the basic principles of neutron protein crystallography. The information that can be gained from a neutron structure is presented in balance with practical considerations. Methods to produce isotopically-substituted proteins and to grow large crystals are provided in the context of neutron structures reported in the literature. Available instruments for data collection and software for data processing and structure refinement are described along with technique-specific strategies including joint X-ray/neutron structure refinement. Examples are given to illustrate, ultimately, the unique scientific value of neutron protein crystal structures. Copyright © 2015 Elsevier Inc. All rights reserved.

An effective approach to synthesize monolayer tungsten disulphide crystals using tungsten halide precursor

NASA Astrophysics Data System (ADS)

Thangaraja, Amutha; Shinde, Sachin M.; Kalita, Golap; Tanemura, Masaki

2016-02-01

The synthesis of large-area monolayer tungsten disulphide (WS2) single crystal is critical for realistic application in electronic and optical devices. Here, we demonstrate an effective approach to synthesize monolayer WS2 crystals using tungsten hexachloride (WCl6) as a solid precursor in atmospheric chemical vapor deposition process. In this technique, 0.05M solution of WCl6 in ethanol was drop-casted on SiO2/Si substrate to create an even distribution of the precursor, which was reduced and sulfurized at 750 °C in Ar atmosphere. We observed growth of triangular, star-shaped, as well as dendritic WS2 crystals on the substrate. The crystal geometry evolves with the shape and size of the nuclei as observed from the dendritic structures. These results show that controlling the initial nucleation and growth process, large WS2 single crystalline monolayer can be grown using the WCl6 precursor. Our finding shows an easier and effective approach to grow WS2 monolayer using tungsten halide solution-casting, rather than evaporating the precursor for gas phase reaction.

Adsorption mechanisms of the nonequilibrium incorporation of admixtures in a growing crystal

NASA Astrophysics Data System (ADS)

Franke, V. D.; Punin, Yu. O.; Smetannikova, O. G.; Kenunen, D. S.

2007-12-01

The nonequilibrium partition of components between a crystal and solution is mainly controlled by impurity adsorption on the surface of the growing crystal. The specificity of adsorption on the faces of various simple forms leads to the sectorial zoning of crystals. This effect was studied experimentally for several crystallizing systems with different impurities, including isomorphous, 2d-isomorphous, and nonisomorphous, readily adsorbed impurities. In all systems, the sectorial selectivity of impurity incorporation into host crystals has been detected with partition coefficients many times higher than in the case of equilibrium partition. Specific capture of impurities by certain faces is accompanied by inhibition of their growth and modification of habit. The decrease in nonequilibrium partition coefficients with degree of oversaturation provides entrapment of impurities in the growing crystals. Thereby, the adsorption mechanism works in much the same mode for impurities of quite different nature. The behavior of partition coefficient differs drastically from impurity capturing by diffusion mechanism.

Raman, AFM and SNOM high resolution imaging of carotene crystals in a model carrot cell system.

PubMed

Rygula, Anna; Oleszkiewicz, Tomasz; Grzebelus, Ewa; Pacia, Marta Z; Baranska, Malgorzata; Baranski, Rafal

2018-05-15

Three non-destructive and complementary techniques, Raman imaging, Atomic Force Microscopy and Scanning Near-field Optical Microscopy were used simultaneously to show for the first time chemical and structural differences of carotenoid crystals. Spectroscopic and microscopic scanning probe measurements were applied to the released crystals or to crystals accumulated in a unique, carotenoids rich callus tissue growing in vitro that is considered as a new model system for plant carotenoid research. Three distinct morphological crystal types of various carotenoid composition were identified, a needle-like, rhomboidal and helical. Raman imaging using 532 and 488 nm excitation lines provided evidence that the needle-like and rhomboidal crystals had similar carotenoid composition and that they were composed mainly of β-carotene accompanied by α-carotene. However, the presence of α-carotene was not identified in the helical crystals, which had the characteristic spatial structure. AFM measurements of crystals identified by Raman imaging revealed the crystal topography and showed the needle-like and rhomboidal crystals were planar but they differed in all three dimensions. Combining SNOM and Raman imaging enabled indication of carotenoid rich structures and visualised their distribution in the cell. The morphology of identified subcellular structures was characteristic for crystalline, membraneous and tubular chromoplasts that are plant organelles responsible for carotenoid accumulation in cells. Copyright © 2018 Elsevier B.V. All rights reserved.

The Effect of Solution Conditions on the Nucleation Kinetics of Tetragonal Lysozyme Crystals

NASA Technical Reports Server (NTRS)

Judge, Russell A.; Baird, James K.; Pusey, Marc L.

1998-01-01

An understanding of protein crystal nucleation rates and the effect of solution conditions upon them, is fundamental to the preparation of protein crystals of the desired size and shape for X-ray diffraction analysis. The ability to predict the effect of supersaturation, temperature, pH and precipitant concentration on the number and size of crystals formed is of great benefit in the pursuit of protein structure analysis. In this study we experimentally examine the effect of supersaturation, temperature, pH and sodium chloride concentration on the nucleation rate of tetragonal chicken egg white lysozyme crystals. In order to do this batch crystallization plates were prepared at given solution concentrations and incubated at three different temperatures over the period of one week. The number of crystals per well with their size and dimensions were recorded and correlated against solution conditions. Duplicate experiments indicate the reproducibility of the technique. Although it is well known that crystal numbers increase with increasing supersaturation, large changes in crystal number were also correlated against solution conditions of temperature, pH and salt concentration over the same supersaturation ranges. Analysis of these results enhance our understanding of the effect of solution conditions such as the dramatic effect that small changes in charge and ionic strength can have on the number of tetragonal lysozyme crystals that form and grow in solution.

Low cost solution-based materials processing methods for large area OLEDs and OFETs

NASA Astrophysics Data System (ADS)

Jeong, Jonghwa

In Part 1, we demonstrate the fabrication of organic light-emitting devices (OLEDs) with precisely patterned pixels by the spin-casting of Alq3 and rubrene thin films with dimensions as small as 10 mum. The solution-based patterning technique produces pixels via the segregation of organic molecules into microfabricated channels or wells. Segregation is controlled by a combination of weak adsorbing characteristics of aliphatic terminated self-assembled monolayers (SAMs) and by centrifugal force, which directs the organic solution into the channel or well. This novel patterning technique may resolve the limitations of pixel resolution in the method of thermal evaporation using shadow masks, and is applicable to the fabrication of large area displays. Furthermore, the patterning technique has the potential to produce pixel sizes down to the limitation of photolithography and micromachining techniques, thereby enabling the fabrication of high-resolution microdisplays. The patterned OLEDs, based upon a confined structure with low refractive index of SiO2, exhibited higher current density than an unpatterned OLED, which results in higher electroluminescence intensity and eventually more efficient device operation at low applied voltages. We discuss the patterning method and device fabrication, and characterize the morphological, optical, and electrical properties of the organic pixels. In part 2, we demonstrate a new growth technique for organic single crystals based on solvent vapor assisted recrystallization. We show that, by controlling the polarity of the solvent vapor and the exposure time in a closed system, we obtain rubrene in orthorhombic to monoclinic crystal structures. This novel technique for growing single crystals can induce phase shifting and alteration of crystal structure and lattice parameters. The organic molecules showed structural change from orthorhombic to monoclinic, which also provided additional optical transition of hypsochromic shift from that of the orthorhombic form. An intermediate form of the crystal exhibits an optical transition to the lowest vibrational energy level that is otherwise disallowed in the single-crystal orthorhombic form. The monoclinic form exhibits entirely new optical transitions and showed a possible structural rearrangement for increasing charge carrier mobility, making it promising for organic devices. These phenomena can be explained and proved by the chemical structure and molecular packing of the monoclinic form, transformed from orthorhombic crystalline structure.

Rapid crystallization and morphological adjustment of zeolite ZSM-5 in nonionic emulsions

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

Zhang Ying, E-mail: yingzh1977@163.co; Jin Chao; Research Institute of Petroleum Processing, Beijing 100083

2011-01-15

Zeolite ZSM-5 was synthesized for the first time in a nonionic emulsion composed of polyoxyethylated alkylphenol, butanol, cyclohexane and tetraethylammonium hydroxide (TEAOH)-containing zeolite synthesis mixture. The crystallization kinetics in the emulsion was investigated and the ZSM-5 product was characterized in detail by XRD, SEM, FT-IR, TG, N{sub 2} adsorption and CHN analysis techniques. Compared with the conventionally hydrothermal synthesis with the same structure directing agent TEAOH, the emulsion system allows rapid crystallization of ZSM-5. The ZSM-5 product exhibits unusual agglomerated structure and possesses larger specific surface area. The FT-IR, TG results plus CHN analysis show the encapsulation of a tracemore » of emulsion components in the emulsion ZSM-5. Control experiments show the emulsion system exerts the crystallization induction and morphological adjustment effects mainly during the aging period. The effects are tentatively attributed to the confined space domains, surfactant-water interaction as well as surfactant-growing crystals interaction existing in the emulsion. -- Graphical abstract: The nonionic emulsion synthesis allows rapid crystallization and morphological adjustment of zeolite ZSM-5 compared with the conventional hydrothermal synthesis. Display Omitted« less

Solution-grown crystals for neutron radiation detectors, and methods of solution growth

DOEpatents

Zaitseva, Natalia P; Hull, Giulia; Cherepy, Nerine J; Payne, Stephen A; Stoeffl, Wolfgang

2012-06-26

A method according to one embodiment includes growing an organic crystal from solution, the organic crystal exhibiting a signal response signature for neutrons from a radioactive source. A system according to one embodiment includes an organic crystal having physical characteristics of formation from solution, the organic crystal exhibiting a signal response signature for neutrons from a radioactive source; and a photodetector for detecting the signal response of the organic crystal. A method according to another embodiment includes growing an organic crystal from solution, the organic crystal being large enough to exhibit a detectable signal response signature for neutrons from a radioactive source. An organic crystal according to another embodiment includes an organic crystal having physical characteristics of formation from solution, the organic crystal exhibiting a signal response signature for neutrons from a radioactive source, wherein the organic crystal has a length of greater than about 1 mm in one dimension.

Reconfigurable photonic crystals enabled by pressure-responsive shape-memory polymers

PubMed Central

Fang, Yin; Ni, Yongliang; Leo, Sin-Yen; Taylor, Curtis; Basile, Vito; Jiang, Peng

2015-01-01

Smart shape-memory polymers can memorize and recover their permanent shape in response to an external stimulus (for example, heat). They have been extensively exploited for a wide spectrum of applications ranging from biomedical devices to aerospace morphing structures. However, most of the existing shape-memory polymers are thermoresponsive and their performance is hindered by heat-demanding programming and recovery steps. Although pressure is an easily adjustable process variable such as temperature, pressure-responsive shape-memory polymers are largely unexplored. Here we report a series of shape-memory polymers that enable unusual ‘cold' programming and instantaneous shape recovery triggered by applying a contact pressure at ambient conditions. Moreover, the interdisciplinary integration of scientific principles drawn from two disparate fields—the fast-growing photonic crystal and shape-memory polymer technologies—enables fabrication of reconfigurable photonic crystals and simultaneously provides a simple and sensitive optical technique for investigating the intriguing shape-memory effects at nanoscale. PMID:26074349

Large-scale grain growth in the solid-state process: From "Abnormal" to "Normal"

NASA Astrophysics Data System (ADS)

Jiang, Minhong; Han, Shengnan; Zhang, Jingwei; Song, Jiageng; Hao, Chongyan; Deng, Manjiao; Ge, Lingjing; Gu, Zhengfei; Liu, Xinyu

2018-02-01

Abnormal grain growth (AGG) has been a common phenomenon during the ceramic or metallurgy processing since prehistoric times. However, usually it had been very difficult to grow big single crystal (centimeter scale over) by using the AGG method due to its so-called occasionality. Based on the AGG, a solid-state crystal growth (SSCG) method was developed. The greatest advantages of the SSCG technology are the simplicity and cost-effectiveness of the technique. But the traditional SSCG technology is still uncontrollable. This article first summarizes the history and current status of AGG, and then reports recent technical developments from AGG to SSCG, and further introduces a new seed-free, solid-state crystal growth (SFSSCG) technology. This SFSSCG method allows us to repeatedly and controllably fabricate large-scale single crystals with appreciable high quality and relatively stable chemical composition at a relatively low temperature, at least in (K0.5Na0.5)NbO3(KNN) and Cu-Al-Mn systems. In this sense, the exaggerated grain growth is no longer 'Abnormal' but 'Normal' since it is able to be artificially controllable and repeated now. This article also provides a crystal growth model to qualitatively explain the mechanism of SFSSCG for KNN system. Compared with the traditional melt and high temperature solution growth methods, the SFSSCG method has the advantages of low energy consumption, low investment, simple technique, composition homogeneity overcoming the issues with incongruent melting and high volatility. This SFSSCG could be helpful for improving the mechanical and physical properties of single crystals, which should be promising for industrial applications.

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.

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

Crystal face temperature determination means

DOEpatents

Nason, D.O.; Burger, A.

1994-11-22

An optically transparent furnace having a detection apparatus with a pedestal enclosed in an evacuated ampule for growing a crystal thereon is disclosed. Temperature differential is provided by a source heater, a base heater and a cold finger such that material migrates from a polycrystalline source material to grow the crystal. A quartz halogen lamp projects a collimated beam onto the crystal and a reflected beam is analyzed by a double monochromator and photomultiplier detection spectrometer and the detected peak position in the reflected energy spectrum of the reflected beam is interpreted to determine surface temperature of the crystal. 3 figs.

Effect of Gravity Level on the Particle Shape and Size During Zeolite Crystal Growth

NASA Technical Reports Server (NTRS)

Song, Hong-Wei; Ilebusi, Olusegun J.; Sacco, Albert, Jr.

2003-01-01

A microscopic diffusion model is developed to represent solute transport in the boundary layer of a growing zeolite crystal. This model is used to describe the effect of gravity on particle shape and solute distribution. Particle dynamics and crystal growth kinetics serve as the boundary conditions of flow and convection-diffusion equations. A statistical rate theory is used to obtain the rate of solute transport across the growing interface, which is expressed in terms of concentration and velocity of solute species. Microgravity can significantly decrease the solute velocity across the growing interface compared to its earth-based counterpart. The extent of this reduction highly depends on solute diffusion constant in solution. Under gravity, the flow towards the crystal enhances solute transport rate across the growing interface while the flow away from crystals reduces this rate, suggesting a non-uniform growth rate and thus an elliptic final shape. However, microgravity can significantly reduce the influence of flow and obtain a final product with perfect spherical shape. The model predictions compare favorably with the data of space experiment of zeolites grown in space.

Seed-mediated growth of patterned graphene nanoribbon arrays

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

Arnold, Michael Scott; Way, Austin James; Jacobberger, Robert Michael

Graphene nanoribbon arrays, methods of growing graphene nanoribbon arrays, and electronic and photonic devices incorporating the graphene nanoribbon arrays are provided. The graphene nanoribbons in the arrays are formed using a seed-mediated, bottom-up, chemical vapor deposition (CVD) technique in which the (001) facet of a semiconductor substrate and the orientation of the seed particles on the substrate are used to orient the graphene nanoribbon crystals preferentially along a single [110] direction of the substrate.

Flux growth in a horizontal configuration: An analog to vapor transport growth

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

Yan, J. -Q.; Sales, B. C.; Susner, M. A.

Flux growth of single crystals is normally performed in a vertical configuration with an upright refractory container holding the flux melt. At high temperatures, flux dissolves the charge, forming a homogeneous solution before nucleation and growth of crystals takes place under proper supersaturation generated by cooling or evaporating the flux. In this paper, we report flux growth in a horizontal configuration with a temperature gradient along the horizontal axis: a liquid transport growth analogous to the vapor transport technique. In a typical liquid transport growth, the charge is kept at the hot end of the refractory container and the fluxmore » melt dissolves the charge and transfers it to the cold end. Once the concentration of charge is above the solubility limit at the cold end, the thermodynamically stable phase nucleates and grows. Compared to the vertical flux growth, the liquid transport growth can provide a large quantity of crystals in a single growth since the charge/flux ratio is not limited by the solubility limit at the growth temperature. This technique is complementary to the vertical flux growth and can be considered when a large amount of crystals is needed but the yield from the conventional vertical flux growth is limited. Finally, we applied this technique to the growth of IrSb 3, Mo 3Sb 7, and MnBi from self-flux, and the growth of FeSe, CrTe 3, NiPSe 3, FePSe 3, CuInP 2S 6, RuCl 3, and OsCl 4 from a halide flux.« less

Flux growth in a horizontal configuration: An analog to vapor transport growth

DOE PAGES

Yan, J. -Q.; Sales, B. C.; Susner, M. A.; ...

2017-07-05

Flux growth of single crystals is normally performed in a vertical configuration with an upright refractory container holding the flux melt. At high temperatures, flux dissolves the charge, forming a homogeneous solution before nucleation and growth of crystals takes place under proper supersaturation generated by cooling or evaporating the flux. In this paper, we report flux growth in a horizontal configuration with a temperature gradient along the horizontal axis: a liquid transport growth analogous to the vapor transport technique. In a typical liquid transport growth, the charge is kept at the hot end of the refractory container and the fluxmore » melt dissolves the charge and transfers it to the cold end. Once the concentration of charge is above the solubility limit at the cold end, the thermodynamically stable phase nucleates and grows. Compared to the vertical flux growth, the liquid transport growth can provide a large quantity of crystals in a single growth since the charge/flux ratio is not limited by the solubility limit at the growth temperature. This technique is complementary to the vertical flux growth and can be considered when a large amount of crystals is needed but the yield from the conventional vertical flux growth is limited. Finally, we applied this technique to the growth of IrSb 3, Mo 3Sb 7, and MnBi from self-flux, and the growth of FeSe, CrTe 3, NiPSe 3, FePSe 3, CuInP 2S 6, RuCl 3, and OsCl 4 from a halide flux.« less

Solutal Convection Around Growing Protein Crystal and Diffusional Purification in Space

NASA Technical Reports Server (NTRS)

Lee, Chun P.; Chernov, Alexander A.

2004-01-01

At least some protein crystals were found to preferentially trap microheterogeneous impurities. The latter are, for example, dimmer molecules of the crystallizing proteines (e.g. ferritin, lysozyme), or the regular molecules on which surfaces small molecules or ions are adsorbed (e.g. acetilated lysozyme) and modi@ molecular charge. Impurities may induce lattice defects and deteriorate structural resolution. Distribution of impurities between mother solution and gorwing crystal is defined by two interrelated distribution coefficients: kappa = rho(sup c, sub 2) and K = (rho(sup c, sub 2)/rho(sup c, sub 1)/rho(sub 2)/rho(sub 1). Here, rho(sub 2), rho(sub 1) and rho(sup c, sub 2) are densities of impurity (2) and regular protein (1) in solution at the growing interface and within the crystal ("c"). For the microheterogeneous impurities studied, K approx. = 2 - 4, so that kappa approx. - 10(exp 2) - 10(exp 3), since K = kappa (rho(sub 1)/rho(sup c, sub 1) and protein solubility ratio rho(sub 1)/rho(sub=p c, sub 2) much less than 1. Therefore, a crystal growing in absence of convection purifies mother solution around itself, grows cleaner and, probably, more perfect. If convection is present, the solution flow permanently brings new impurities to the crystal. This work theoretically addressed two subjects: 1) onset of convection, 2) distribution of impurities.

Interfacial characterization in carbon nanotube reinforced aluminum matrix composites

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

Housaer, F., E-mail: francois.housaer@ed.univ-lille1.fr; Beclin, F., E-mail: franck.beclin@univ-lille1.fr; Touzin, M., E-mail: matthieu.touzin@univ-lille1.fr

2015-12-15

In this work, the effects of the sintering parameters, such as temperature and the techniques used (HP and SPS), on CNT/Al composite interfaces are studied. The major role of the native aluminum oxide (Al{sub 2}O{sub 3}) layer covering the aluminum grains is highlighted. It is shown that, for a sintering temperature below 620 °C, the amorphous Al{sub 2}O{sub 3} layer prevents the reaction between aluminum and carbon. For greater sintering temperatures, the breaking of the oxide layer due to its crystallization leads to the formation of aluminum carbide (Al{sub 4}C{sub 3}) by reaction between aluminum and the CNT. The Al{submore » 4}C{sub 3} crystals grow perpendicularly to the matrix grain boundaries by thermally activated diffusion of the carbon atoms coming from the CNT. It is also demonstrated that, by limiting the sintering time, which is the case in SPS, it is possible to limit the growth of the Al{sub 4}C{sub 3} crystals and thus to preserve the CNT. - Highlights: • The high reactivity between CNT and Al matrix, resulting Al{sub 4}C{sub 3} formation during the sintering process is highlighted. • We demonstrate, thanks to in-situ TEM observations, that Al{sub 4}C{sub 3} crystals grow into aluminum grains by carbon diffusion. • The native aluminum oxide around the aluminum particles prevents the diffusion of carbon into the aluminum grains. • We show that the protective layer can be broken because of its crystallization, leading to the formation of Al{sub 4}C{sub 3}. • SPS, by limiting the sintering duration, is an interesting way for preparing CNT/Al composites without carbide formation.« less

Growth and nonlinear optical characterization of organic single crystal films

NASA Astrophysics Data System (ADS)

Zhou, Ligui

1997-12-01

Organic single crystal films are important for various future applications in photonics and integrated optics. The conventional method for inorganic crystal growth is not suitable for organic materials, and the high temperature melting method is not good for most organic materials due to decomposition problems. We developed a new method-modified shear method-to grow large area organic single crystal thin films which have exceptional nonlinear optical properties and high quality surfaces. Several organic materials (NPP, PNP and DAST) were synthesized and purified before the thin film crystal growth. Organic single crystal thin films were grown from saturated organic solutions using modified shear method. The area of single crystal films were about 1.5 cm2 for PNP, 1 cm2 for NPP and 5 mm2 for DAST. The thickness of the thin films which could be controlled by the applied pressure ranged from 1μm to 10 μm. The single crystal thin films of organic materials were characterized by polarized microscopy, x-ray diffraction, polarized UV-Visible and polarized micro-FTIR spectroscopy. Polarized microscopy showed uniform birefringence and complete extinction with the rotation of the single crystal thin films under crossed- polarization, which indicated high quality single crystals with no scattering. The surface orientation of single crystal thin films was characterized by x-ray diffraction. The molecular orientation within the crystal was further studied by the polarized UV-Visible and Polarized micro-FTIR techniques combined with the x-ray and polarized microscopy results. A Nd:YAG laser with 35 picosecond pulses at 1064nm wavelength was employed to perform the nonlinear optical characterization of the organic single crystal thin films. Two measurement techniques were used to study the crystal films: second harmonic generation (SHG) and electro-optic (EO) effect. SHG results showed that the nonlinear optical coefficient of NPP was 18 times that of LiNbO3, a standard inorganic crystal material, and the nonlinear optical coefficient of PNP was 11 times that of LiNbO3. Electro-optic measurements showed that r11 = 65 pm/V for NPP and r12 = 350 pm/V for DAST. EO modulation effect was also observed using Fabry-Perot interferometry. Waveguide devices are very important for integrated optics. But the fabrication of waveguide devices on the organic single crystal thin films was difficult due to the solubility of the film in common organic solvents. A modified photolithographic technique was employed to make channel waveguides and poly(vinyl alcohol) (PVA) was used as a protective layer in the fabrication of the waveguides. Waveguides with dimensions about 7/mum x 1μm x 1mm were obtained.

Numerical analysis of melt-solid interface shapes and growth rates of gallium antimonide in a single-zone vertical Bridgman furnace

NASA Astrophysics Data System (ADS)

Dutta, P. S.; Bhat, H. L.; Kumar, Vikram

1995-09-01

Numerical analysis has been carried out to determine the deviation of the growth rate from the ampoule lowering rate and the shape of the isotherms during the growth of gallium antimonide using the vertical Bridgman technique in a single-zone furnace. Electrical analogues have been used to model the thermal behaviour of the growth system. The standard circuit analysis technique has been used to calculate the temperature distribution in the growing crystal under various growth conditions. The effects of furnace temperature gradient near the melt-solid interface, the ampoule lowering rate, the ampoule geometry, the thermal conductivity of the melt, the mode of heat extraction from the tip of the ampoule and the extent of lateral heat loss from the side walls of the ampoule on the shape of isotherms in the crystal have been evaluated. The theoretical results presented here agree well with our previously obtained experimental results.

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.

Growth of lead tin telluride crystals in gels

NASA Technical Reports Server (NTRS)

Barber, Patrick G.

1986-01-01

Improved gels and several geometries were investigated for use in growing crystals. The use of lead sulfide test crystals proved workable, but it was impossible to obtain and maintain a sufficiently concentrated telluride ion solution to successfully grow lead telluride crystals. It appears that oxygen in the solution is capable of oxidizing the telluride ion up to tellurium metal. The method may still be successful, but only if precautions are taken to eliminate dissolved oxygen from the gels and aqueous solutions and to maintain a suitable concentration of telluride, Te(2)-(aq.).

Crystals of Human Serum Albumin for Use in Genetic Engineering and Rational Drug Design

NASA Technical Reports Server (NTRS)

Carter, Daniel C. (Inventor)

1994-01-01

This invention pertains to crystals of serum albumin and processes for growing them. The purpose of the invention is to provide crystals of serum albumin which can be studied to determine binding sites for drugs. Form 2 crystals grow in the monoclinic space P2(sub 1), and possesses the following unit cell constraints: a = 58.9 +/- 7, b = 88.3 +/- 7, c = 60.7 +/- 7, Beta = 101.0 +/- 2 degrees. One advantage of the invention is that it will allow rational drug design

Microgravity

NASA Image and Video Library

2004-04-15

The Commercial Vapor Diffusion Apparatus will be used to perform 128 individual crystal growth investigations for commercial and science research. These experiments will grow crystals of several different proteins, including HIV-1 Protease Inhibitor, Glycogen Phosphorylase A, and NAD Synthetase. The Commercial Vapor Diffusion Apparatus supports multiple commercial investigations within a controlled environment. The goal of the Commercial Protein Crystal Growth payload on STS-95 is to grow large, high-quality crystals of several different proteins of interest to industry, and to continue to refine the technology and procedures used in microgravity for this important commercial research.

Understanding Growth Rate Limitations in Production of Single-Crystal Cadmium Zinc Telluride (CZT) by the Traveling Heater Method (THM)

NASA Astrophysics Data System (ADS)

Peterson, Jeffrey H.

Cadmium telluride (CdTe) and cadmium zinc telluride (CZT) are important optoelectronic materials with applications ranging from medical imaging to nuclear materials monitoring. However, CZT and CdTe have long been plagued by second-phase particles, inhomogeneity, and other defects. The traveling heater method (THM) is a promising approach for growing CZT and other compound semiconductors that has been shown to grow detector-grade crystals. In contrast to traditional directional solidification, the THM consists of a moving melt zone that simultaneously dissolves a polycrystalline feed while producing a single-crystal of material. Additionally, the melt is highly enriched in tellurium, which allows for growth at lower temperatures, limiting the presence of precipitated tellurium second-phase particles in the final crystal. Unfortunately, the THM growth of CZT is limited to millimeters per day when other growth techniques can grow an order of magnitude faster. To understand these growth limits, we employ a mathematical model of the THM system that is formulated to realistically represent the interactions of heat and species transport, fluid flow, and interfacial dissolution and growth under conditions of local thermodynamic equilibrium and steady-state growth. We examine the complicated interactions among zone geometry, continuum transport, phase change, and fluid flow driven by buoyancy. Of particular interest and importance is the formation of flow structures in the liquid zone of the THM that arise from the same physical mechanism as lee waves in atmospheric flows and demonstrate the same characteristic Brunt-Vaisala scaling. We show that flow stagnation and reversal associated with lee-wave formation are responsible for the accumulation of tellurium and supercooled liquid near the growth interface, even when the lee-wave vortex is not readily apparent in the overall flow structure. The supercooled fluid is posited to result in morphological instability at growth rates far below the limit predicted by the classical criterion by Tiller et al. for constitutional supercooling.

Sponge-like nanoporous single crystals of gold

PubMed Central

Khristosov, Maria Koifman; Bloch, Leonid; Burghammer, Manfred; Kauffmann, Yaron; Katsman, Alex; Pokroy, Boaz

2015-01-01

Single crystals in nature often demonstrate fascinating intricate porous morphologies rather than classical faceted surfaces. We attempt to grow such crystals, drawing inspiration from biogenic porous single crystals. Here we show that nanoporous single crystals of gold can be grown with no need for any elaborate fabrication steps. These crystals are found to grow following solidification of a eutectic composition melt that forms as a result of the dewetting of nanometric thin films. We also present a kinetic model that shows how this nano-porous single-crystalline structure can be obtained, and which allows the potential size of the porous single crystal to be predicted. Retaining their single-crystalline nature is due to the fact that the full crystallization process is faster than the average period between two subsequent nucleation events. Our findings clearly demonstrate that it is possible to form single-crystalline nano porous metal crystals in a controlled manner. PMID:26554856

Video-Growing Salt Crystals Onboard the International Space Station (ISS)

NASA Technical Reports Server (NTRS)

2003-01-01

Saturday Morning Science, the science of opportunity series of applied experiments and demonstrations, performed aboard the International Space Station (ISS) by Expedition 6 astronaut Dr. Don Pettit, revealed some remarkable findings. Growing salt crystals in a bottle of water is a favorite science activity for kids. In space, Dr. Pettit grew salt crystals in stretched films of water so that the salt water only fed the crystals around the edges rather than from all sides, as happens in a glass of water. This video of his demonstration shows that surface tension plays a surprisingly dominant role in the crystal formation and convection is more active that one might expect.

Ultrasound assisted crystallization of mefenamic acid: Effect of operating parameters and comparison with conventional approach.

PubMed

Iyer, Sneha R; Gogate, Parag R

2017-01-01

The current work investigates the application of low intensity ultrasonic irradiation for improving the cooling crystallization of Mefenamic Acid for the first time. The crystal shape and size has been analyzed with the help of optical microscope and image analysis software respectively. The effect of ultrasonic irradiation on crystal size, particle size distribution (PSD) and yield has been investigated, also establishing the comparison with conventional approach. It has been observed that application of ultrasound not only enhances the yield but also reduces the induction time for crystallization as compared to conventional cooling crystallization technique. In the presence of ultrasound, the maximum yield was obtained at optimum conditions of power dissipation of 30W and ultrasonic irradiation time of 10min. The yield was further improved by application of ultrasound in cycles where the formed crystals are allowed to grow in the absence of ultrasonic irradiation. It was also observed that the desired crystal morphology was obtained for the ultrasound assisted crystallization. The conventionally obtained needle shaped crystals transformed into plate shaped crystals for the ultrasound assisted crystallization. The particle size distribution was analyzed using statistical means on the basis of skewness and kurtosis values. It was observed that the skewness and excess kurtosis value for ultrasound assisted crystallization was significantly lower as compared to the conventional approach. XRD analysis also revealed better crystal properties for the processed mefenamic acid using ultrasound assisted approach. The overall process intensification benefits of mefenamic acid crystallization using the ultrasound assisted approach were reduced particle size, increase in the yield and uniform PSD coupled with desired morphology. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

Protein crystal growth in microgravity: Temperature induced large scale crystallization of insulin

NASA Technical Reports Server (NTRS)

Long, Marianna M.; Delucas, Larry J.; Smith, C.; Carson, M.; Moore, K.; Harrington, Michael D.; Pillion, D. J.; Bishop, S. P.; Rosenblum, W. M.; Naumann, R. J.

1994-01-01

One of the major stumbling blocks that prevents rapid structure determination using x-ray crystallography is macro-molecular crystal growth. There are many examples where crystallization takes longer than structure determination. In some cases, it is impossible to grow useful crystals on earth. Recent experiments conducted in conjuction with NASA on various Space Shuttle missions have demonstrated that protein crystals often grow larger and display better internal molecular order than their earth-grown counterparts. This paper reports results from three Shuttle flights using the Protein Crystallization Facility (PCF). The PCF hardware produced large, high-quality insulin crystals by using a temperature change as the sole means to affect protein solubility and thus, crystallization. The facility consists of cylinders/containers with volumes of 500, 200, 100, and 50 ml. Data from the three Shuttle flights demonstrated that larger, higher resolution crystals (as evidenced by x-ray diffraction data) were obtained from the microgravity experiments when compared to earth-grown crystals.

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.

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.

Nonlinear Optical Phenomena in Solids

DTIC Science & Technology

1981-02-01

December 1980, organized according to research objectives: a. Objective: Grow five crystals of Hg].Cdx.Te by the modified Bridgman (quench/anneal) method...objectives of the contract are listed below: a. Grow five 2rystals of Hgl _ ,Cd T e by the modified Bridgman (quench/anneal) method. b. Determine the...composicinn and purity profiles of the crystals . c. Prepare spin-flip Raman laser cavities from selected sections of the crystals . d. Evaluate the utility of

Protein Crystals Grow Purer in Space: Physics of Phenomena

NASA Technical Reports Server (NTRS)

Chernov, Alex A.

2000-01-01

This presentation will summarize the quantitative experimental and theoretical results obtained by B.R. Thomas, P.G. Vekilov, D.C. Carter, A.M. Holmes, W.K. Widierow and the Author, the team with expertise in physics, biochemistry, crystallography and engineering. Impurities inhomogeneously trapped by a growing crystal - e.g., producing sectorial structure and/or striations - may induce macroscopic internal stress in it if an impurity molecule has slightly (less than 10%) different shape or volume than the regular one(s) they replace. We tested for the first time plasticity and measured Young modulus E of the triclinic, not cross-linked lysozyme by triple point bending technique. Triclinic lysozyme crystals are purely elastic with E similar or equal to 1/5 (raised dot) 10 (exp 9) partial derivative yn/sq cm. The strength limit, sigma (sub c) similar or equal to 10 (exp -3)E similar or equal to Epsilon (sub c), where sigma (sub c) and epsilon (sub c) are critical stress and strain, respectively. Scaling E and sigma (sub c) with the lattice spacing suggests similar binding stiffness in inorganic and biomolecular crystals. The inhomogeneous internal stress may be resolved in these brittle crystals either by cracking or by creation of misoriented mosaic blocks during, not after growth. If each impurity molecule induces in the lattice elementary strain epsilon (sub 0) similar or equal to 3 (raised dot) 10 (exp -2) (this is maximal elementary strain that can arise at the supersaturation DELTA mu/kT similar or equal to 2 and macroscopic molecular concentration difference between subsequent macrolayers or growth sectors is partial derivativeC similar or equal to 5 (raised dot) 10 (exp -3), the internal strain epsilon similar or equal to epsilon (sub 0) partial derivative C similar or equal to 10 (exp -4). Mosaic misorientation resolving such strain is approximately 30 arcsec. Tenfold increase of impurity concentration may cause cracking. Estimates of stress in an isometric sectorial crystal show that lysozyme crystals can tolerate the stress till the size of 0.5mm. Dissolving mosaic lysozyme crystal shows that the mosaicity, indeed, is absent below that size.

Protein Crystallization

NASA Technical Reports Server (NTRS)

Chernov, Alexander A.

2005-01-01

Nucleation, growth and perfection of protein crystals will be overviewed along with crystal mechanical properties. The knowledge is based on experiments using optical and force crystals behave similar to inorganic crystals, though with a difference in orders of magnitude in growing parameters. For example, the low incorporation rate of large biomolecules requires up to 100 times larger supersaturation to grow protein, rather than inorganic crystals. Nucleation is often poorly reproducible, partly because of turbulence accompanying the mixing of precipitant with protein solution. Light scattering reveals fluctuations of molecular cluster size, its growth, surface energies and increased clustering as protein ages. Growth most often occurs layer-by-layer resulting in faceted crystals. New molecular layer on crystal face is terminated by a step where molecular incorporation occurs. Quantitative data on the incorporation rate will be discussed. Rounded crystals with molecularly disordered interfaces will be explained. Defects in crystals compromise the x-ray diffraction resolution crucially needed to find the 3D atomic structure of biomolecules. The defects are immobile so that birth defects stay forever. All lattice defects known for inorganics are revealed in protein crystals. Contribution of molecular conformations to lattice disorder is important, but not studied. This contribution may be enhanced by stress field from other defects. Homologous impurities (e.g., dimers, acetylated molecules) are trapped more willingly by a growing crystal than foreign protein impurities. The trapped impurities induce internal stress eliminated in crystals exceeding a critical size (part of mni for ferritin, lysozyme). Lesser impurities are trapped from stagnant, as compared to the flowing, solution. Freezing may induce much more defects unless quickly amorphysizing intracrystalline water.

Formation of curved micrometer-sized single crystals.

PubMed

Koifman Khristosov, Maria; Kabalah-Amitai, Lee; Burghammer, Manfred; Katsman, Alex; Pokroy, Boaz

2014-05-27

Crystals in nature often demonstrate curved morphologies rather than classical faceted surfaces. Inspired by biogenic curved single crystals, we demonstrate that gold single crystals exhibiting curved surfaces can be grown with no need of any fabrication steps. These single crystals grow from the confined volume of a droplet of a eutectic composition melt that forms via the dewetting of nanometric thin films. We can control their curvature by controlling the environment in which the process is carried out, including several parameters, such as the contact angle and the curvature of the drops, by changing the surface tension of the liquid drop during crystal growth. Here we present an energetic model that explains this phenomenon and predicts why and under what conditions crystals will be forced to grow with the curvature of the microdroplet even though the energetic state of a curved single crystal is very high.

Microgravity

NASA Image and Video Library

1998-01-05

The Interferometer Protein Crystal Growth (IPCG) experiment was designed to measure details of how protein molecules move through a fluid. It was flown on the STS-86 mission for use aboard Russian Space Station Mir in 1998. It studied aspects of how crystals grow - and what conditions lead to the best crystals, details that remain a mystery. IPCG produces interference patterns by spilitting then recombining laser light. This let scientists see how fluid densities - and molecular diffusion - change around a crystal as it grows in microgravity. The heart of the IPCG apparatus is the interferometer cell comprising the optical bench, microscope, other optics, and video camera. IPCG experiment cells are made of optical glass and silvered on one side to serve as a mirror in the interferometer system that visuzlizes crystals and conditions around them as they grow inside the cell. This diagram shows the optical layout. The principal investigator was Dr. Alexander McPherson of University of California, Irvine. Co-investigators are William Witherow and Dr. Marc Pusey of NASA's Marshall Space Flight Center (MSFC).

Microgravity

NASA Image and Video Library

1998-01-05

The Interferometer Protein Crystal Growth (IPCG) experiment was designed to measure details of how protein molecules move through a fluid. It was flown on the STS-86 mission for use aboard Russian Space Station Mir in 1998. It studied aspects of how crystals grow - and what conditions lead to the best crystals, details that remain a mystery. IPCG produces interference patterns by spilitting then recombining laser light. This let scientists see how fluid densities - and molecular diffusion - change around a crystal as it grows in microgravity. The heart of the IPCG apparatus is the interferometer cell comprising the optical bench, microscope, other optics, and video camera. IPCG experiment cells are made of optical glass and silvered on one side to serve as a mirror in the interferometer system that visuzlizes crystals and conditions around them as they grow inside the cell. This view shows interferograms produced in ground tests. The principal investigator was Dr. Alexander McPherson of University of California, Irvine. Co-investigators are William Witherow and Dr. Marc Pusey of NASA's Marshall Space Flight Center (MSFC).

Microgravity

NASA Image and Video Library

1998-01-05

The Interferometer Protein Crystal Growth (IPCG) experiment was designed to measure details of how protein molecules move through a fluid. It was flown on the STS-86 mission for use aboard Russian Space Station Mir in 1998. It studied aspects of how crystals grow - and what conditions lead to the best crystals, details that remain a mystery. IPCG produces interference patterns by spilitting then recombining laser light. This let scientists see how fluid densities - and molecular diffusion - change around a crystal as it grows in microgravity. The heart of the IPCG apparatus is the interferometer cell comprising the optical bench, microscope, other optics, and video camera. IPCG experiment cells are made of optical glass and silvered on one side to serve as a mirror in the interferometer system that visuzlizes crystals and conditions around them as they grow inside the cell. This diagram shows the growth cells. The principal investigator was Dr. Alexander McPherson of University of California, Irvine. Co-investigators are William Witherow and Dr. Marc Pusey of NASA's Marshall Space Flight Center (MSFC).

Microgravity

NASA Image and Video Library

1998-01-05

The Interferometer Protein Crystal Growth (IPCG) experiment was designed to measure details of how protein molecules move through a fluid. It was flown on the STS-86 mission for use aboard Russian Space Station Mir in 1998. It studied aspects of how crystals grow - and what conditions lead to the best crystals, details that remain a mystery. IPCG produces interference patterns by spilitting then recombining laser light. This let scientists see how fluid densities - and molecular diffusion - change around a crystal as it grows in microgravity. The heart of the IPCG apparatus is the interferometer cell comprising the optical bench, microscope, other optics, and video camera. IPCG experiment cells are made of optical glass and silvered on one side to serve as a mirror in the interferometer system that visuzlizes crystals and conditions around them as they grow inside the cell. This view shows a large growth cell. The principal investigator was Dr. Alexander McPherson of University of California, Irvine. Co-investigators are William Witherow and Dr. Marc Pusey of NASA's Marshall Space Flight Center (MSFC).

Crystal face temperature determination means

DOEpatents

Nason, Donald O.; Burger, Arnold

1994-01-01

An optically transparent furnace (10) having a detection apparatus (29) with a pedestal (12) enclosed in an evacuated ampule (16) for growing a crystal (14) thereon. Temperature differential is provided by a source heater (20), a base heater (24) and a cold finger (26) such that material migrates from a polycrystalline source material (18) to grow the crystal (14). A quartz halogen lamp (32) projects a collimated beam (30) onto the crystal (14) and a reflected beam (34) is analyzed by a double monochromator and photomultiplier detection spectrometer (40) and the detected peak position (48) in the reflected energy spectrum (44) of the reflected beam (34) is interpreted to determine surface temperature of the crystal (14).

The Commercial Vapor Diffusion Apparatus (CVDA) STS-95

NASA Technical Reports Server (NTRS)

2004-01-01

The Commercial Vapor Diffusion Apparatus will be used to perform 128 individual crystal growth investigations for commercial and science research. These experiments will grow crystals of several different proteins, including HIV-1 Protease Inhibitor, Glycogen Phosphorylase A, and NAD Synthetase. The Commercial Vapor Diffusion Apparatus supports multiple commercial investigations within a controlled environment. The goal of the Commercial Protein Crystal Growth payload on STS-95 is to grow large, high-quality crystals of several different proteins of interest to industry, and to continue to refine the technology and procedures used in microgravity for this important commercial research.

Convection Induced by Traveling Magnetic Fields in Semiconductor Melts

NASA Technical Reports Server (NTRS)

Konstantin, Mazuruk

2000-01-01

Axisymmetric traveling magnetic fields (TMF) can be beneficial for crystal growth applications. such as the vertical Bridgman, float zone or traveling heater methods. TMF induces a basic flow in the form of a single roll. This type of flow can enhance mass and heat transfer to the growing crystal. More importantly, the TMF Lorentz body force induced in the system can counterbalance the buoyancy forces, so the resulting convection can be much smaller and even the direction of it can be changed. In this presentation, we display basic features of this novel technique. In particular, numerical calculations of the Lorentz force for arbitrary frequencies will be presented along with induced steady-state fluid flow profiles. Also, numerical modeling of the TMF counter-balancing natural convection in vertical Bridgman systems will be demonstrated.

Compressive auto-indexing in femtosecond nanocrystallography

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

Maia, Filipe; Yang, Chao; Marchesini, Stefano

2010-09-20

Ultrafast nanocrystallography has the potential to revolutionize biology by enabling structural elucidation of proteins for which it is possible to grow crystals with 10 or fewer unit cells. The success of nanocrystallography depends on robust orientation-determination procedures that allow us to average diffraction data from multiple nanocrystals to produce a 3D diffraction data volume with a high signal-to-noise ratio. Such a 3D diffraction volume can then be phased using standard crystallographic techniques."Indexing" algorithms used in crystallography enable orientation determination of a diffraction data from a single crystal when a relatively large number of reflections are recorded. Here we show thatmore » it is possible to obtain the exact lattice geometry from a smaller number of measurements than standard approaches using a basis pursuit solver.« less

Growth and lasing of single crystal YAG fibers with different Ho3+ concentrations

NASA Astrophysics Data System (ADS)

Bera, Subhabrata; Nie, Craig D.; Soskind, Michael G.; Li, Yuan; Harrington, James A.; Johnson, Eric G.

2018-01-01

A method to grow single crystal (SC) yttrium aluminum garnet (YAG) fibers with varied rare-earth ion dopant concentration has been proposed. Crystalline holmium aluminum garnet (HoAG), prepared via sol-gel process, was dip-coated on to previously grown SC YAG fibers. The HoAG coated SC YAG fiber preforms were re-grown to a smaller diameter using the laser heated pedestal growth (LHPG) technique. The final dopant concentration of the re-grown SC fiber was varied by changing the number of HoAG coatings on the preform. 120 μm diameter SC Ho:YAG fibers with four different dopant concentrations were grown. Lasing was demonstrated at 2.09 μm for these fibers. A maximum of 58.5% optical-to-optical slope efficiency was obtained.

Thermal analysis of a growing crystal in an aqueous solution

NASA Astrophysics Data System (ADS)

Shiomi, Yuji; Kuroda, Toshio; Ogawa, Tomoya

1980-10-01

The temperature profiles around growing crystals in aqueous solutions of Rochelle salt were measured with accuracy of 0.005°C in a two-dimensional cell which was used for elimination of thermal convection current in the cell. The temperature distribution became stationary after 2 h from injection of the mother liquid, but the concentration distribution did not become stationary because the diffusion constant of solute in the solution was much smaller than the thermal diffusivity of the solution. The growth rate was linearly proportional to the temperature gradient at every growing interface. Since crystal growth is a typical interaction process between thermal and material flow, the experimental results were analysed by such an interaction model. The analysis confirms that the material flow is limited by diffusion within a layer width of about a few hundreds micrometers on the growing interface.

Anisotropic high-harmonic generation in bulk crystals

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

You, Yong Sing; Reis, David A.; Ghimire, Shambhu

2016-11-21

The microscopic valence electron density determines the optical, electronic, structural and thermal properties of materials. However, current techniques for measuring this electron charge density are limited: for example, scanning tunnelling microscopy is confined to investigations at the surface, and electron diffraction requires very thin samples to avoid multiple scattering. Therefore, an optical method is desirable for measuring the valence charge density of bulk materials. Since the discovery of high-harmonic generation (HHG) in solids, there has been growing interest in using HHG to probe the electronic structure of solids. Here, using single-crystal MgO, we demonstrate that high-harmonic generation in solids ismore » sensitive to interatomic bonding. We find that harmonic efficiency is enhanced (diminished) for semi-classical electron trajectories that connect (avoid) neighbouring atomic sites in the crystal. Finally, these results indicate the possibility of using materials’ own electrons for retrieving the interatomic potential and thus the valence electron density, and perhaps even wavefunctions, in an all-optical setting.« less

Crystal settling and crystal growth caused by Ostwald Ripening in a terrestrial magma ocean under rotation

NASA Astrophysics Data System (ADS)

Maas, C.; Moeller, A.; Hansen, U.

2013-12-01

About 4.5 billion years ago the earth was covered by a heavily convecting and rotating global magma ocean which was caused by an impact of a mars-sized impactor in a later stage of the earth's accretion. After the separation of metal and silicate (see A. Möller, U. Hansen (2013)) and the formation of the earth's core it began to crystallize. Small silicate crystals emerge and grow by Ostwald Ripening when the fluid is supersaturated. This process results in shrinking of small crystals and growing of large crystals on behalf of the smaller ones. This leads to an altering of the crystal settling time. One question which is still under great debate is whether fractional or equilibrium crystallization occurred in the magma ocean. Fractional crystallization means that different mineral fractions settle one after the other which would lead to a strongly differentiated mantle after solidification of the magma ocean. In contrast to that equilibrium crystallization would result in a well mixed mantle. Whether fractional or equilibrium crystallization occurred is for example important for the starting model of plate tectonics or the understanding of the mantle development until today. To study the change of crystal radius in a convecting and rotating magma ocean we employed a 3D numerical model. Due to the low viscosity and strong rotation the influence of rotation on the early magma Ocean cannot be neglected. In the model the crystals are able to influence each other and the fluid flow. They are able to grow, shrink, vanish and form and gravitational, Coriolis and drag forces due to the fluid act on them. In our present work we study the crystal settling depending on different rotation rates and rotation axes with two configurations. For the polar setting the rotation axis is parallel, at the equator it is perpendicular to gravity. Low rotation at the pole leads to a large fraction of suspended crystals. With increasing rotation the crystals settle and form a thick layer at the bottom of the magma ocean. At the equator we find three regimes (see A. Möller, U. Hansen (2013)) depending on the rotation strength. At low rotation a high fraction of silicate crystals settle at the bottom. At higher rotation the crystals form a thick layer in the bottom 1/3 of box. At high rotation all crystals are suspended and we observe a ribbon structure in the middle of the box. With a second model we investigate growing and shrinking of crystals by Ostwald Ripening and include formation and melting. In general we observe the same behaviour and regimes as described above, however due to Ostwald Ripening the evolution of crystal radius with time depends on the strength of rotation and on the orientation of the rotation axis. Very first results show that at the pole the growth of the silicate crystals is limited. The resulting small radius leads to a slow crystal settling. At the equator the crystals are able to grow larger than at the pole and therefore settle faster. This could lead to an asymmetrical crystallization of the magma ocean. In an extreme case due to the different settling times this could lead to a well mixed mantle at the pole whereas at the equator the mantle could be strongly differentiated after the solidification of the magma ocean.

Calcium pyrophosphate dihydrate gout and other crystal deposition diseases.

PubMed

Reginato, A J

1991-08-01

The number of crystal or birefringent particles associated with arthritis is increasing, and a uniform taxonomy is needed. The term gout has been proposed as a generic term for these diseases based on historical, clinical, and crystallographic reasons. Calcium pyrophosphate dihydrate gout follows monosodium urate gout in frequency, and its spectrum of clinical manifestations continues to grow. Familial calcium pyrophosphate dihydrate gout was described for the first time in kindreds studied in England and Tunisia; new Jewish and Spanish kindreds were also reported. Type I collagen was shown to nucleate nativelike calcium pyrophosphate dihydrate crystals, and pyrophosphate elaboration was explored in cartilage explants in an attempt to reproduce the in vivo metabolic or endocrine disorders associated with calcium pyrophosphate dihydrate gout. The effect of pyrophosphatase and different cofactors such as magnesium in dissolving calcium pyrophosphate dihydrate crystals was investigated. High-resolution electron microscopy was used to study the interrelation between apatite and other basic calcium phosphate crystals in apatite gout. Raman microscopy was applied for the first time to identify crystals in biologic specimens. A simple and specific technique for basic calcium phosphate crystal identification is necessary to understand the relationship between different calcium phosphate crystals and osteoarthritis. Several reports about children and young patients with primary oxalate gout described the effect of oxalate on eyes, periodontal tissues, and bone. Multicenter studies showed poor results of renal transplantation, but favored combined liver and renal transplantation.(ABSTRACT TRUNCATED AT 250 WORDS)

Bibliography of Soviet Laser Developments, Number 85, September - October 1986.

DTIC Science & Technology

1987-11-01

Ultrashort Pulse Generation, Laser Crystal Growing, Free Electron Lasers , Laser Theory, Laser Biological Effects, Laser Communications, Laser ...liquid, gas, and chemical lasers ; components; nonlinear optics; spectroscopy of laser materials; ultrashort pulse generation; crystal growing; theoretical...30 5. Self-focusing 30 6. Acoustic Interaction ................ 30 G. Spectroscopy of Laser Materials ......... 33 H. Ultrashort

Method for Growing Low-Defect Single Crystal Heteroepitaxial Films

NASA Technical Reports Server (NTRS)

Powell, J. Anthony (Inventor); Neudeck, Philip G. (Inventor)

2002-01-01

A method is disclosed for growing high-quality low-defect crystal films heteroepitaxially on substrates that are different than the crystal films. The growth of the first two heteroepitaxial bilayers is performed on a first two-dimensional nucleate island before a second growth of two-dimensional nucleation is allowed to start. The method is particularly suited for the growth of 3C-SiC, 2H-AlN, or 2H-GaN on 6H-SiC, 4H-SiC, or silicon substrates.

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

Generation of Protein Crystals Using a Solution-Stirring Technique

NASA Astrophysics Data System (ADS)

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

2004-06-01

Crystals of bovine adenosine deaminase (ADA) were grown over a two week period in the presence of an inhibitor, whereas ADA crystals did not form using conventional crystallization methods when the inhibitor was excluded. To obtain ADA crystals in the absence of the inhibitor, a solution-stirring technique was used. The crystals obtained using this technique were found to be of high quality and were shown to have high structural resolution for X-ray diffraction analysis. The results of this study indicate that the stirring technique is a useful method for obtaining crystals of proteins that do not crystallize using conventional techniques.

Drilling technique for crystals

NASA Technical Reports Server (NTRS)

Hunter, T.; Miyagawa, I.

1977-01-01

Hole-drilling technique uses special crystal driller in which drill bit rotates at fixed position at speed of 30 rpm while crystal slowly advances toward drill. Technique has been successfully applied to crystal of Rochell salt, Triglycine sulfate, and N-acetyglycine. Technique limits heat buildup and reduces strain on crystal.

Effect of local structures on crystallization in deeply undercooled metallic glass-forming liquids

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

Jiang, S. Q.; Li, M. Z., E-mail: maozhili@ruc.edu.cn; Wu, Z. W.

2016-04-21

The crystallization mechanism in deeply undercooled ZrCu metallic glass-forming liquids was investigated via molecular dynamics simulations. It was found that the crystallization process is mainly controlled by the growth of crystal nuclei formed by the BCC-like atomic clusters, consistent with experimental speculations. The crystallization rate is found to relate to the number of growing crystal nuclei in the crystallization process. The crystallization rate in systems with more crystal nuclei is significantly hindered by the larger surface fractions of crystal nuclei and their different crystalline orientations. It is further revealed that in the crystallization in deeply undercooled regions, the BCC-like crystalmore » nuclei are formed from the inside of the precursors formed by the FCC-like atomic clusters, and growing at the expense of the precursors. Meanwhile, the precursors are expanding at the expense of the outside atomic clusters. This process is consistent with the so-called Ostwald step rule. The atomic structures of metallic glasses are found to have significant impact on the subsequent crystallization process. In the Zr{sub 85}Cu{sub 15} system, the stronger spatial correlation of Cu atoms could hinder the crystallization processes in deeply undercooled regions.« less

Modeling solute clustering in the diffusion layer around a growing crystal.

PubMed

Shiau, Lie-Ding; Lu, Yung-Fang

2009-03-07

The mechanism of crystal growth from solution is often thought to consist of a mass transfer diffusion step followed by a surface reaction step. Solute molecules might form clusters in the diffusion step before incorporating into the crystal lattice. A model is proposed in this work to simulate the evolution of the cluster size distribution due to the simultaneous aggregation and breakage of solute molecules in the diffusion layer around a growing crystal in the stirred solution. The crystallization of KAl(SO(4))(2)12H(2)O from aqueous solution is studied to illustrate the effect of supersaturation and diffusion layer thickness on the number-average degree of clustering and the size distribution of solute clusters in the diffusion layer.

Split and sealing of dislocated pipes at the front of a growing crystal

NASA Astrophysics Data System (ADS)

Gutkin, M. Yu.; Sheinerman, A. G.

2004-07-01

A model is suggested for the split of dislocated pipes at the front a growing crystal. Within the model, the pipe split occurs through the generation of a dislocation semi-loop at the pipe and crystal surfaces and its subsequent expansion into the crystal interior. The strain energy of such a dislocation semi-loop as well as the stress field of a dislocated pipe perpendicular to a flat crystal surface are calculated. The parameter regions are determined at which the expansion of the dislocation semi-loop is energetically favorable and, thus, the pipe split becomes irreversible. A mechanism is proposed for the formation of a stable semi-loop resulting in the split and possible subsequent overgrowth of the dislocated pipe.

Phase transition and epitaxies between hydrated orthorhombic and anhydrous monoclinic uric acid crystals

NASA Astrophysics Data System (ADS)

Boistelle, R.; Rinaudo, C.

1981-05-01

Anhydrous monoclinic and hydrated orthorhombic uric acid crystals can be nucleated and grown from pure water solutions either separately or together with epitaxial relationships. When crystals of one modification exist in the solution they can act as nucleation substrate for the crystals of the other modification. In both cases the new phase grows epitaxially on the substrate; the mutual orientations are the same but the contact planes are different. In addition, the anhydrous modification grows into the hydrated one which undergoes a phase transition by a dissolution-recrystallization process. It is likely that the same processes occur in human stones made up of uric acids.

Spiral crystal growth of potassium dichromate in gelatin

NASA Astrophysics Data System (ADS)

Suda, Jun-Ichiro; Matsushita, Mitsugu

1995-02-01

Huge spiral crystals of potassium dichromate (K2Cr2O7) have been found to grow three-dimensionally in a gelatin medium when gelatin containing K2Cr2O7 was dried slowly in a test tube at a low temperature. These spirals were all right-handed, and their widths, axial pitches and lengths were 2-3 mm, 5-6 mm and 20-25 mm, repectively. When the gelatin concentration in the medium was decreased, ordinary plate-like crystals were observed to grow, instead of the spiral crystals. To the best of our knowledge, inorganic compounds such as K2Cr2O7 have so far not been reported to form such huge spiral crystals. It is conjectured that collagen molecules, which compose the gelatin medium and have right-handed triple helix structure lead to the growth of spiral crystals.

Effect of the Inhomogeneity of Ice Crystals on Retrieving Ice Cloud Optical Thickness and Effective Particle Size

NASA Technical Reports Server (NTRS)

Xie, Yu; Minnis, Patrick; Hu, Yong X.; Kattawar, George W.; Yang, Ping

2008-01-01

Spherical or spheroidal air bubbles are generally trapped in the formation of rapidly growing ice crystals. In this study the single-scattering properties of inhomogeneous ice crystals containing air bubbles are investigated. Specifically, a computational model based on an improved geometric-optics method (IGOM) has been developed to simulate the scattering of light by randomly oriented hexagonal ice crystals containing spherical or spheroidal air bubbles. A combination of the ray-tracing technique and the Monte Carlo method is used. The effect of the air bubbles within ice crystals is to smooth the phase functions, diminish the 22deg and 46deg halo peaks, and substantially reduce the backscatter relative to bubble-free particles. These features vary with the number, sizes, locations and shapes of the air bubbles within ice crystals. Moreover, the asymmetry factors of inhomogeneous ice crystals decrease as the volume of air bubbles increases. Cloud reflectance lookup tables were generated at wavelengths 0.65 m and 2.13 m with different air-bubble conditions to examine the impact of the bubbles on retrieving ice cloud optical thickness and effective particle size. The reflectances simulated for inhomogeneous ice crystals are slightly larger than those computed for homogenous ice crystals at a wavelength of 0.65 microns. Thus, the retrieved cloud optical thicknesses are reduced by employing inhomogeneous ice cloud models. At a wavelength of 2.13 microns, including air bubbles in ice cloud models may also increase the reflectance. This effect implies that the retrieved effective particle sizes for inhomogeneous ice crystals are larger than those retrieved for homogeneous ice crystals, particularly, in the case of large air bubbles.

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.

Macromolecular crystal growing system

NASA Technical Reports Server (NTRS)

Snyder, Robert S. (Inventor); Herren, Blair J. (Inventor); Carter, Daniel C. (Inventor); Yost, Vaughn H. (Inventor); Bugg, Charles E. (Inventor); Delucas, Lawrence J. (Inventor); Suddath, Fred L. (Inventor)

1991-01-01

A macromolecular crystal growing system especially designed for growing crystals in the low gravity of space as well as the gravity of earth includes at least one tray assembly, a carrier assembly which receives the tray, and a refrigeration-incubation module in which the carrier assembly is received. The tray assembly includes a plurality of sealed chambers with a plastic syringe and a plug means for the double tip of the syringe provided therein. Ganging mechanisms operate the syringes and plugs simultaneously in a precise and smooth operation. Preferably, the tray assemblies are mounted on ball bearing slides for smooth operation in inserting and removing the tray assemblies into the carrier assembly. The plugging mechanism also includes a loading control mechanism. A mechanism for leaving a syringe unplugged is also provided.

New Scintillator Materials (K2CeBr5) and (Cs2CeBr5)

NASA Technical Reports Server (NTRS)

Hawrami, R.; Volz, M. P.; Batra, A. K.; Aggarwal, M. D.; Roy, U. N.; Groza, M.; Burger, A.; Cherepy, Nerine; Niedermayr, Thomas; Payne, Stephen A.

2008-01-01

Cesium cerium bromide (Cs2CeBr5) and potassium cerium bromide (K2CeBr5) are new scintillator materials for X-ray and gamma ray detector applications. Recently halide scintillator materials, such as Ce doped lanthanum bromide has been proved to be very important material for the same purpose. These materials are highly hygroscopic; a search for high light yield non-hygroscopic materials was highly desirable to advance the scintillator technology. In this paper, we are reporting the crystal growth of novel scintillator materials, cesium cerium bromide (Cs2CeBr5) and potassium cerium bromide (K2CeBr5). Crystals were successfully grown from the melt using the vertical Bridgman-Stockbarger technique, in a comparison with the high performance LaBr3 or LaCl3 crystals, cerium based alkali halides crystals, (Cs2CeBr5) and (K2CeBr5) have similar scintillation properties, while being much less hygroscopic. Furthermore, cesium based compounds will not suffer from the self-activity present in potassium and lanthanum compounds. However the Cs2CeBr5 crystals did not grow properly probably due to non-congruent melting or to some phase transition during cooling. Keywords." Scintillator materials; Ce3+; Energy resolution; Light yield; K2CeBr5

Understanding the crystallization behavior of as-deposited Ti-Sb-Te alloys through real-time radial distribution functions.

PubMed

Zhu, Min; Xia, Mengjiao; Song, Zhitang; Cheng, Yan; Wu, Liangcai; Rao, Feng; Song, Sannian; Wang, Miao; Lu, Yegang; Feng, Songlin

2015-06-07

Phase change materials, successfully used in optical data-storage and non-volatile electronic memory, are well-known for their ultrafast crystallization speed. However, the fundamental understanding of their crystallization behavior, especially the nucleation process, is limited by present experimental techniques. Here, real-time radial distribution functions (RDFs), derived from the selected area electron diffractions, are employed as structural probes to comprehensively study both nucleation and subsequent growth stages of Ti-doped Sb2Te3 (TST) materials in the electron-irradiation crystallization process. It can be found that the incorporation of Ti atoms in Sb2Te3 forms wrong bonds such as Ti-Te, Ti-Sb, breaks the originally ordered atomic arrangement and diminishes the initial nucleus size of the as-deposited films, which results in better thermal stability. But these nuclei hardly grow until their sizes exceed a critical value, and then a rapid growth period starts. This means that an extended nucleation time is required to form the supercritical nuclei of TST alloys with higher concentration. Also, the increasing formation of four-membered rings, which served as nucleation sites, after doping excessive Ti is responsible for the change of the crystallization behavior from growth-dominated to nucleation-dominated.

Leakage current analysis for dislocations in Na-flux GaN bulk single crystals by conductive atomic force microscopy

NASA Astrophysics Data System (ADS)

Hamachi, T.; Takeuchi, S.; Tohei, T.; Imanishi, M.; Imade, M.; Mori, Y.; Sakai, A.

2018-04-01

The mechanisms associated with electrical conduction through individual threading dislocations (TDs) in a Na-flux GaN crystal grown with a multipoint-seed-GaN technique were investigated by conductive atomic force microscopy (C-AFM). To focus on individual TDs, dislocation-related etch pits (DREPs) were formed on the Na-flux GaN surface by wet chemical etching, after which microscopic Pt electrodes were locally fabricated on the DREPs to form conformal contacts to the Na-flux GaN crystal, using electron beam assisted deposition. The C-AFM data clearly demonstrate that the leakage current flows through the individual TD sites. It is also evident that the leakage current and the electrical conduction mechanism vary significantly based on the area within the Na-flux GaN crystal where the TDs are formed. These regions include the c-growth sector (cGS) in which the GaN grows in the [0001 ] direction on top of the point-seed with a c-plane growth front, the facet-growth sector (FGS) in which the GaN grows with {10 1 ¯ 1 } facets on the side of the cGS, the boundary region between the cGS and FGS (BR), and the coalescence boundary region between FGSs (CBR). The local current-voltage (I-V) characteristics of the specimen demonstrate space charge limited current conduction and conduction related to band-like trap states associated with TDs in the FGS, BR, and CBR. A detailed analysis of the I-V data indicates that the electrical conduction through TDs in the cGS may proceed via the Poole-Frenkel emission mechanism.

Improving the growth of CZT crystals for radiation detectors: a modeling perspective

NASA Astrophysics Data System (ADS)

Derby, Jeffrey J.; Zhang, Nan; Yeckel, Andrew

2012-10-01

The availability of large, single crystals of cadmium zinc telluride (CZT) with uniform properties is key to improving the performance of gamma radiation detectors fabricated from them. Towards this goal, we discuss results obtained by computational models that provide a deeper understanding of crystal growth processes and how the growth of CZT can be improved. In particular, we discuss methods that may be implemented to lessen the deleterious interactions between the ampoule wall and the growing crystal via engineering a convex solidification interface. For vertical Bridgman growth, a novel, bell-curve furnace temperature profile is predicted to achieve macroscopically convex solid-liquid interface shapes during melt growth of CZT in a multiple-zone furnace. This approach represents a significant advance over traditional gradient-freeze profiles, which always yield concave interface shapes, and static heat transfer designs, such as pedestal design, that achieve convex interfaces over only a small portion of the growth run. Importantly, this strategy may be applied to any Bridgman configuration that utilizes multiple, controllable heating zones. Realizing a convex solidification interface via this adaptive bell-curve furnace profile is postulated to result in better crystallinity and higher yields than conventional CZT growth techniques.

An effective approach to synthesize monolayer tungsten disulphide crystals using tungsten halide precursor

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

Thangaraja, Amutha; Shinde, Sachin M.; Kalita, Golap, E-mail: kalita.golap@nitech.ac.jp

2016-02-01

The synthesis of large-area monolayer tungsten disulphide (WS{sub 2}) single crystal is critical for realistic application in electronic and optical devices. Here, we demonstrate an effective approach to synthesize monolayer WS{sub 2} crystals using tungsten hexachloride (WCl{sub 6}) as a solid precursor in atmospheric chemical vapor deposition process. In this technique, 0.05M solution of WCl{sub 6} in ethanol was drop-casted on SiO{sub 2}/Si substrate to create an even distribution of the precursor, which was reduced and sulfurized at 750 °C in Ar atmosphere. We observed growth of triangular, star-shaped, as well as dendritic WS{sub 2} crystals on the substrate. The crystalmore » geometry evolves with the shape and size of the nuclei as observed from the dendritic structures. These results show that controlling the initial nucleation and growth process, large WS{sub 2} single crystalline monolayer can be grown using the WCl{sub 6} precursor. Our finding shows an easier and effective approach to grow WS{sub 2} monolayer using tungsten halide solution-casting, rather than evaporating the precursor for gas phase reaction.« less

Method For Growth of Crystal Surfaces and Growth of Heteroepitaxial Single Crystal Films Thereon

NASA Technical Reports Server (NTRS)

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

2000-01-01

A method of growing atomically-flat surfaces and high quality low-defect crystal films of semiconductor materials and fabricating improved devices thereon is discussed. The method is also suitable for growing films heteroepitaxially on substrates that are different than the film. The method is particularly suited for growth of elemental semiconductors (such as Si), compounds of Groups III and V elements of the Periodic Table (such as GaN), and compounds and alloys of Group IV elements of the Periodic Table (such as SiC).

Morphological Diversity in Crystal Growth of l-Ascorbic Acid Dissolved in Methanol

NASA Astrophysics Data System (ADS)

Ito, Miho; Izui, Machiko; Yamazaki, Yoshihiro; Matsushita, Mitsugu

2003-06-01

Morphological diagram with respect to crystal growth of l-ascorbic acid (C6H8O6; so-called vitamin C) from methanol solution on a flat glass dish is presented. Varying humidity and initial concentration of l-ascorbic acid in methanol solution, the following three distinct kinds of growing patterns have been observed: homogeneous disk, concentric ring and dendrite. In addition, in higher concentration clearly faceted small single crystals grow in any humidity less than 90%. Crossovers from one pattern to another were observed, too.

Method of synthesizing and growing copper-indium-diselenide (CuInSe.sub.2) crystals

DOEpatents

Ciszek, Theodore F.

1987-01-01

A process for preparing CuInSe.sub.2 crystals includes melting a sufficient quantity of B.sub.2 O.sub.3 along with stoichiometric quantities of Cu, In, and Se in a crucible in a high pressure atmosphere of inert gas to encapsulate the CuInSe.sub.2 melt and confine the Se to the crucible. Additional Se in the range of 1.8 to 2.2 percent over the stoichiometric quantity is preferred to make up for small amounts of Se lost in the process. The crystal is grown by inserting a seed crystal through the B.sub.2 O.sub.3 encapsulate into contact with the CuInSe.sub.2 melt and withdrawing the seed upwardly to grow the crystal thereon from the melt.

Crystallization kinetics in Si-1 at%Sn during rapid solidification in undercooled melt

NASA Astrophysics Data System (ADS)

Kuribayashi, K.; Ozawa, S.; Nagayama, K.; Inatomi, Y.

2017-06-01

In order to elucidate the cause of the morphological transition of crystals growing in an undercooled melt of semiconducting materials, we carried out the containerless solidification of undoped Si and Si-1 at%Sn using a CO2 laser-equipped electromagnetic levitator (EML). The crystallization of these materials was successfully achieved under controlled undercooling. The relation between the shape of growing crystals and the degree of undercooling in Si-1 at%Sn was similar to that in undoped Si; that is, plate-like needle crystals were observed at low undercooling, whereas at medium and high undercooling the shape of growing crystals changed to massive dendrites. The grain-size of as-solidified samples of Si-1 at%Sn was remarkably small compared with that of undoped Si. The surface morphologies of samples solidified by dropping the melt onto a chill plate of mirror-polished silicon consisted of typical twin-related <110> dendrites. On the other hand, samples that were dropped from the undercooled state consisted of twin-free <100> dendrites. The nucleation rate of two-dimensional nuclei calculated on the basis of two mechanisms, which are the twin-plane re-entrant edge mechanism and the twin-free mechanism, suggested that the morphological transition to twin-free <100> dendrites from twin-related <110> dendrites occurs when the degree of undercooling becomes larger than the critical value. These results indicate that the cause of the morphological transition of Si growing in the undercooled melt is not the roughening transition of the crystal-melt interface but the transition of the nucleation kinetics to the twin-free mechanism from the twin-related mechanism.

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.

Crystal Growth, Characterization and Fabrication of Cadmium Zinc Telluride-based Nuclear Detectors

NASA Astrophysics Data System (ADS)

Krishna, Ramesh M.

In today's world, nuclear radiation is seeing more and more use by humanity as time goes on. Nuclear power plants are being built to supply humanity's energy needs, nuclear medical imaging is becoming more popular for diagnosing cancer and other diseases, and control of weapons-grade nuclear materials is becoming more and more important for national security. All of these needs require high-performance nuclear radiation detectors which can accurately measure the type and amount of radiation being used. However, most current radiation detection materials available commercially require extensive cooling, or simply do not function adequately for high-energy gamma-ray emitting nuclear materials such as uranium and plutonium. One of the most promising semiconductor materials being considered to create a convenient, field-deployable nuclear detector is cadmium zinc telluride (CdZnTe, or CZT). CZT is a ternary semiconductor compound which can detect high-energy gamma-rays at room temperature. It offers high resistivity (≥ 1010 O-cm), a high band gap (1.55 eV), and good electron transport properties, all of which are required for a nuclear radiation detector. However, one significant issue with CZT is that there is considerable difficulty in growing large, homogeneous, defect-free single crystals of CZT. This significantly increases the cost of producing CZT detectors, making CZT less than ideal for mass-production. Furthermore, CZT suffers from poor hole transport properties, which creates significant problems when using it as a high-energy gamma-ray detector. In this dissertation, a comprehensive investigation is undertaken using a successful growth method for CZT developed at the University of South Carolina. This method, called the solvent-growth technique, reduces the complexity required to grow detector-grade CZT single crystals. It utilizes a lower growth temperature than traditional growth methods by using Te as a solvent, while maintaining the advantages of crystal homogeneity of other modern CZT growth techniques. However, information about crystals grown with this method has not been undertaken in a comprehensive way thus far. In this work, Cd0.9Zn0.1Te is grown using the solvent-growth method using zone-refined precursor materials loaded into carbon-coated quartz ampoules. Ampoules were sealed and crystal growth was performed using crystal growth furnaces built in-house at USC. Ingots 1-2" in diameter produced using the solvent-growth method were wafered, processed, and polished for characterization. Semiconductor characterization is performed on the CZT crystals to determine band gap, elemental stoichiometry, and electrical resistivity. Surface modification studies were undertaken to determine if surface leakage current can be reduced using sulfur passivation. XPS studies were used to confirm the effects of passivation on the surface states, and electrical characterization was performed to measure the effects of passivation on the CZT crystals. Deep-level and surface defect studies were conducted on the CZT samples to determine the type and intensity of defects present in the crystals which may affect detector performance. Finally, nuclear detectors were fabricated and characterized using analog and digital radiation detection systems to measure their performance and energy resolution.

Kyropoulos method for growth of nonlinear optical organic crystal ABP (4-aminobenzophenone) from the melt

NASA Astrophysics Data System (ADS)

Pan, Shoukui; Okano, Y.; Tsunekawa, S.; Fukuda, T.

1993-03-01

The Kyropoulus method was used to grow nonlinear optical organic crystals ABP (4-aminobenzophenone). The crystals were characterized by nonlinear optical measurements and had a large effect of frequency doubling.

Method of synthesizing and growing copper-indium-diselenide (CuInSe/sub 2/) crystals

DOEpatents

Ciszek, T.F.

1984-11-29

A process for preparing CuInSe/sub 2/ crystals includes melting a sufficient quantity of B/sub 2/O/sub 2/ along with stochiometric quantities of Cu, In, and Se in a crucible in a high-pressure atmosphere of inert gas to encapsulate the CuInSe/sub 2/ melt and confine the Se to the crucible. Additional Se in the range of 1.8 to 2.2% over the stochiometric quantity is preferred to make up for small amounts of Se lost in the process. The melt can then be cooled slowly to form the crystal as direct solidification, or the crystal can be grown by inserting a seed crystal through the B/sub 2/O/sub 3/ encapsulate into contact with the CuInSe/sub 2/ melt and withdrawing the seed upwardly to grow the crystal thereon from the melt.

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.

Determining Kinetic Parameters for Isothermal Crystallization of Glasses

NASA Technical Reports Server (NTRS)

Ray, C. S.; Zhang, T.; Reis, S. T.; Brow, R. K.

2006-01-01

Non-isothermal crystallization techniques are frequently used to determine the kinetic parameters for crystallization in glasses. These techniques are experimentally simple and quick compared to the isothermal techniques. However, the analytical models used for non-isothermal data analysis, originally developed for describing isothermal transformation kinetics, are fundamentally flawed. The present paper describes a technique for determining the kinetic parameters for isothermal crystallization in glasses, which eliminates most of the common problems that generally make the studies of isothermal crystallization laborious and time consuming. In this technique, the volume fraction of glass that is crystallized as a function of time during an isothermal hold was determined using differential thermal analysis (DTA). The crystallization parameters for the lithium-disilicate (Li2O.2SiO2) model glass were first determined and compared to the same parameters determined by other techniques to establish the accuracy and usefulness of the present technique. This technique was then used to describe the crystallization kinetics of a complex Ca-Sr-Zn-silicate glass developed for sealing solid oxide fuel cells.

Wafer-scale synthesis of monolayer and few-layer MoS2 via thermal vapor sulfurization

NASA Astrophysics Data System (ADS)

Robertson, John; Liu, Xue; Yue, Chunlei; Escarra, Matthew; Wei, Jiang

2017-12-01

Monolayer molybdenum disulfide (MoS2) is an atomically thin, direct bandgap semiconductor crystal potentially capable of miniaturizing optoelectronic devices to an atomic scale. However, the development of 2D MoS2-based optoelectronic devices depends upon the existence of a high optical quality and large-area monolayer MoS2 synthesis technique. To address this need, we present a thermal vapor sulfurization (TVS) technique that uses powder MoS2 as a sulfur vapor source. The technique reduces and stabilizes the flow of sulfur vapor, enabling monolayer wafer-scale MoS2 growth. MoS2 thickness is also controlled with great precision; we demonstrate the ability to synthesize MoS2 sheets between 1 and 4 layers thick, while also showing the ability to create films with average thickness intermediate between integer layer numbers. The films exhibit wafer-scale coverage and uniformity, with electrical quality varying depending on the final thickness of the grown MoS2. The direct bandgap of grown monolayer MoS2 is analyzed using internal and external photoluminescence quantum efficiency. The photoluminescence quantum efficiency is shown to be competitive with untreated exfoliated MoS2 monolayer crystals. The ability to consistently grow wafer-scale monolayer MoS2 with high optical quality makes this technique a valuable tool for the development of 2D optoelectronic devices such as photovoltaics, detectors, and light emitters.

On the role of convective motion during dendrite growth: Experiments under variable gravity, revised

NASA Technical Reports Server (NTRS)

Hallett, J.; Cho, N.; Harrison, K.; Lord, A.; Wedum, E.; Purcell, R.; Saunders, C. P. R.

1987-01-01

Experiments show the effect of self induced convection on individual dendrite growth in uniformly supercooled samples and solidification of the resulting mush under conditions of high and low g. Convection is visualized by a Schlieren optical system or a Mach Zender interferometer. For ice crystals growing from the vapor in air, a slight reduction in linear growth rate occur under low g. For ice crystals growing from NaCl solution, dendrite tip velocities are unchanged, but subsequent mush solidification is enhanced through drainage channels under higher g. By contrast, sodium sulfate decahydrate dendrites growing from solution produce convective plumes which lead to higher tip growth rate only as the crystal growth direction approaches that of gravity. Convective plumes are laminar for small crystals under conditions of these experiments; the rise velocity of such plumes is greater than individual vortex rings under identical conditions. Convection effects are only present in solution under a critical supercooling less than about 5 C for sodium sulfate and 2 C for ice in NaCl since at higher supercooling the crystallization velocity, proportional to the square of the supercooling, exceeds the convective velocity, proportional to the square root of the supercooling. The role of convective velocity in bulk solidification is to give a large scale flow which under extreme cases may lead to extensive secondary crystal production, which alters the resulting crystal texture of the completely solidified melt.

A Fiber Optic Probe for Monitoring Protein Aggregation, Nucleation, and Crystallization

NASA Technical Reports Server (NTRS)

Ansari, Rafat R.; Suh, Kwang I.; Arabshahi, Alireza; Wilson, William W.; Bray, Terry L.; DeLucas, Lawrence J.

1996-01-01

Protein crystals are experimentally grown in hanging drops in microgravity experiments on-board the Space Shuttle orbiter. The technique of dynamic light scattering (DLS) can be used to monitor crystal growth process in hanging droplets (approx. 30 (L)) in microgravity experiments, but elaborate instrumentation and optical alignment problems have made in-situ applications difficult. In this paper we demonstrate that such experiments are now feasible. We apply a newly developed fiber optic probe to various earth and space (micro- gravity) bound protein crystallization system configurations to test its capability. These include conventional batch (cuvette or capillary) systems, hanging drop method in a six-pack hanging drop vapor diffusion apparatus (HDVDA), a modified HDVDA for temperature- induced nucleation and aggregation studies, and a newly envisioned dynamically controlled vapor diffusion system (DCVDS) configuration. Our compact system exploits the principles of DLS and offers a fast (within a few seconds) means of quantitatively and non-invasively monitoring the various growth stages of protein crystallization. In addition to DLS capability, the probe can also be used for performing single-angle static light scattering measurements. It utilizes extremely low levels of laser power (approx. few (W)) without a need of having any optical alignment and vibration isolation. The compact probe is also equipped with a miniaturized microscope for visualization of macroscopic protein crystals. This new optical diagnostic system opens up enormous opportunity for exploring new ways to grow good quality crystals suitable for x-ray crystallographic analysis and may help develop a concrete scientific basis for understanding the process of crystallization.

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.

Microgravity

NASA Image and Video Library

1998-01-05

The Interferometer Protein Crstal Growth (IPCG) experiment was designed to measure details of how protein molecules move through a fluid. It was flown on the STS-86 mission for use aboard Russin Space Station Mir in 1998. It studied aspects of how crystals grow - and what conditions lead to the best crystals, details that remain a mystery. IPCG produces interference patterns by splitting then recombining laser light. This let scientists see how fluid densities - and molecular diffusion - change around a crystal as it grows in microgravity. The heart of the IPCG apparatus is the interferometer cell comprising the optical bench, microscope, other optics, and video camera. IPCG experiment cells are made of optical glass and silvered on one side to serve as a mirror in the interferometer system that visualizes crystals and conditions around them as they grow inside the cell. This view shows the complete apparatus. The principal investigator was Dr. Alexander McPherson of the University of California, Irvin. Co-investigators are William Witherow and Dr. Marc Pusey of NASA's Marshall Space Flight Center

Crystallization techniques in wastewater treatment: An overview of applications.

PubMed

Lu, Haijiao; Wang, Jingkang; Wang, Ting; Wang, Na; Bao, Ying; Hao, Hongxun

2017-04-01

As a by-product of industrial or domestic activities, wastewater of different compositions has caused serious environmental problems all over the world. Facing the challenge of wastewater treatment, researchers have begun to make use of crystallization techniques in wastewater treatment. Crystallization techniques have many advantages, such as high efficiency, energy saving, low costs, less space occupation and so on. In recent decades, crystallization is considered as one of promising techniques for wastewater treatment, especially for desalination, water and salt recovery. It has been widely used in engineering applications all over the world. In this paper, various crystallization techniques in wastewater treatment are summarized, mainly including evaporation crystallization, cooling crystallization, reaction crystallization, drowning-out crystallization and membrane distillation crystallization. Overall, they are mainly used for desalination, water and salt recovery. Their applications, advantages and disadvantages were compared and discussed in detail. Copyright © 2017 Elsevier Ltd. All rights reserved.

Impact of interaction range and curvature on crystal growth of particles confined to spherical surfaces.

PubMed

Paquay, Stefan; Both, Gert-Jan; van der Schoot, Paul

2017-07-01

When colloidal particles form a crystal phase on a spherical template, their packing is governed by the effective interaction between them and the elastic strain of bending the growing crystal. For example, if growth commences under appropriate conditions, and the isotropic crystal that forms reaches a critical size, growth continues via the incorporation of defects to alleviate elastic strain. Recently, it was experimentally found that, if defect formation is somehow not possible, the crystal instead continues growing in ribbons that protrude from the original crystal. Here we report on computer simulations in which we observe both the formation of ribbons at short interaction ranges and packings that incorporate defects if the interaction is longer-ranged. The ribbons only form above some critical crystal size, below which the nucleus is disk-shaped. We find that the scaling of the critical crystal size differs slightly from the one proposed in the literature, and we argue that this is because the actual morphology transition is caused by the competition between line tension and elastic stress, rather than the competition between chemical potential and elastic stress.

Impact of interaction range and curvature on crystal growth of particles confined to spherical surfaces

NASA Astrophysics Data System (ADS)

Paquay, Stefan; Both, Gert-Jan; van der Schoot, Paul

2017-07-01

When colloidal particles form a crystal phase on a spherical template, their packing is governed by the effective interaction between them and the elastic strain of bending the growing crystal. For example, if growth commences under appropriate conditions, and the isotropic crystal that forms reaches a critical size, growth continues via the incorporation of defects to alleviate elastic strain. Recently, it was experimentally found that, if defect formation is somehow not possible, the crystal instead continues growing in ribbons that protrude from the original crystal. Here we report on computer simulations in which we observe both the formation of ribbons at short interaction ranges and packings that incorporate defects if the interaction is longer-ranged. The ribbons only form above some critical crystal size, below which the nucleus is disk-shaped. We find that the scaling of the critical crystal size differs slightly from the one proposed in the literature, and we argue that this is because the actual morphology transition is caused by the competition between line tension and elastic stress, rather than the competition between chemical potential and elastic stress.

Polymer-mediated growth of crystals and mesocrystals.

PubMed

Cölfen, Helmut

2013-01-01

Polymers are important additives for the control of mineralization reactions in both biological and bioinspired mineralization. The reason is that they allow for a number of interactions with the growing crystals and even amorphous minerals. These can substantially influence the way the mineral grows on several levels. Already in the prenucleation phase, polymers can control the formation of prenucleation clusters and subsequently the nucleation event. Also, polymers can control whether the further crystallization follows a classical or nonclassical particle-mediated growth path. In this chapter, the main ways in which polymers can be used to control a crystallization reaction will be highlighted. In addition, polymers that are useful for this purpose and the experimental conditions suitable for directing a crystallization reaction into the desired direction through the use of polymers will be described. © 2013 Elsevier Inc. All rights reserved.

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.

Ames Lab 101: Single Crystal Growth

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

Schlagel, Deborah

2013-09-27

Ames Laboratory scientist Deborah Schlagel talks about the Lab's research in growing single crystals of various metals and alloys. The single crystal samples are vital to researchers' understanding of the characteristics of a materials and what gives these materials their particular properties.

Ames Lab 101: Single Crystal Growth

ScienceCinema

Schlagel, Deborah

2018-01-16

Ames Laboratory scientist Deborah Schlagel talks about the Lab's research in growing single crystals of various metals and alloys. The single crystal samples are vital to researchers' understanding of the characteristics of a materials and what gives these materials their particular properties.

A Simple, Inexpensive Chamber for Growing Snow Crystals in the Classroom

NASA Astrophysics Data System (ADS)

Hiramatsu, Kazuhiko; Sturm, Matthew

2005-09-01

The creation of artificial snow crystals for scientific study usually requires patience, hard work, and fairly elaborate and expensive equipment that almost always includes a cold room. Here we describe an inexpensive and easy-to-build apparatus that can produce artificial snow crystals in the classroom. The apparatus, which can operate as both a diffusion and cloud chamber, was developed in Japan in 1996 and has been in use in schools there for several years, where it has also been reported on in scientific journals, the newspapers, and television.1,2 The apparatus allows students and teachers to actually watch snow crystals grow. While it has been demonstrated in the United States,3 we are not aware that it has seen much use here.

High-quality EuO thin films the easy way via topotactic transformation

DOE PAGES

Mairoser, Thomas; Mundy, Julia A.; Melville, Alexander; ...

2015-07-16

Epitaxy is widely employed to create highly oriented crystalline films. A less appreciated, but nonetheless powerful means of creating such films is via topotactic transformation, in which a chemical reaction transforms a single crystal of one phase into a single crystal of a different phase, which inherits its orientation from the original crystal. Topotactic reactions may be applied to epitactic films to substitute, add or remove ions to yield epitactic films of different phases. Here we exploit a topotactic reduction reaction to provide a non-ultra-high vacuum (UHV) means of growing highly oriented single crystalline thin films of the easily over-oxidizedmore » half-metallic semiconductor europium monoxide (EuO) with a perfection rivalling that of the best films of the same material grown by molecular-beam epitaxy or UHV pulsed-laser deposition. Lastly, as the technique only requires high-vacuum deposition equipment, it has the potential to drastically improve the accessibility of high-quality single crystalline films of EuO as well as other difficult-to-synthesize compounds.« less

Rastering strategy for screening and centring of microcrystal samples of human membrane proteins with a sub-10 µm size X-ray synchrotron beam

PubMed Central

Cherezov, Vadim; Hanson, Michael A.; Griffith, Mark T.; Hilgart, Mark C.; Sanishvili, Ruslan; Nagarajan, Venugopalan; Stepanov, Sergey; Fischetti, Robert F.; Kuhn, Peter; Stevens, Raymond C.

2009-01-01

Crystallization of human membrane proteins in lipidic cubic phase often results in very small but highly ordered crystals. Advent of the sub-10 µm minibeam at the APS GM/CA CAT has enabled the collection of high quality diffraction data from such microcrystals. Herein we describe the challenges and solutions related to growing, manipulating and collecting data from optically invisible microcrystals embedded in an opaque frozen in meso material. Of critical importance is the use of the intense and small synchrotron beam to raster through and locate the crystal sample in an efficient and reliable manner. The resulting diffraction patterns have a significant reduction in background, with strong intensity and improvement in diffraction resolution compared with larger beam sizes. Three high-resolution structures of human G protein-coupled receptors serve as evidence of the utility of these techniques that will likely be useful for future structural determination efforts. We anticipate that further innovations of the technologies applied to microcrystallography will enable the solving of structures of ever more challenging targets. PMID:19535414

Preparation of high magneto-optical performance and crystalline quality Ce1Gd2Fe5-xGaxO12 films on CLNGG substrate crystal

NASA Astrophysics Data System (ADS)

Fu, Qiu-ping; Zheng, Ze-yuan; Lin, Nan-xi; Liu, Xiao-feng; Hong, Can-huang; Hu, Xiao-lin; Zhuang, Nai-feng; Chen, Jian-zhong

2016-11-01

Thin films of Ce1Gd2Fe5-xGaxO12 (Ce,Ga:GIG) were prepared on Gd3Ga5O12 (GGG) and Ca2.90Li0.30Nb1.93Ga2.76O12 (CLNGG) substrates by using radio frequency magnetron sputtering technique. The phase, grain orientation, surface morphology, transmittance, magnetism and magnetic circular dichroism (MCD) properties of films were analyzed. And the effects of lattice mismatch and non-magnetic Ga3+-doping were discussed. The results show that the films with higher crystallized quality and lower stress can be obtained by growing on CLNGG than on GGG. Moreover, the coercive force, magnetization, magneto-optical effect intensity and orientation of film can be effectively regulated by adjusting Ga3+-doped concentration.

Optimization of chemical displacement deposition of copper on porous silicon.

PubMed

Bandarenka, Hanna; Redko, Sergey; Nenzi, Paolo; Balucani, Marco; Bondarenko, Vitaly

2012-11-01

Copper (II) sulfate was used as a source of copper to achieve uniform distribution of Cu particles deposited on porous silicon. Layers of the porous silicon were formed by electrochemical anodization of Si wafers in a mixture of HF, C3H7OH and deionized water. The well-known chemical displacement technique was modified to grow the copper particles of specific sizes. SEM and XRD analysis revealed that the outer surface of the porous silicon was covered with copper particles of the crystal orientation inherited from the planes of porous silicon skeleton. The copper crystals were found to have the cubic face centering elementary cell. In addition, the traces of Cu2O cubic primitive crystalline phases were identified. The dimensions of Cu particles were determined by the Feret's analysis of the SEM images. The sizes of the particles varied widely from a few to hundreds of nanometers. A phenomenological model of copper deposition was proposed.

Growth of potassium sulfate crystals in the presence of organic dyes: in situ characterization by atomic force microscopy

NASA Astrophysics Data System (ADS)

Mauri, Andrea; Moret, Massimo

2000-01-01

In situ atomic force microscopy (AFM) has been used to observe potassium sulfate crystals growing in the presence of acid fuchsin and pyranine. These polysulfonated dyes are well known for their ability to adsorb onto the {1 1 0} and {0 1 0} (pyranine only) crystal faces. Using AFM, we analyzed the changes in surface micromorphology induced by the additives on advancing steps for the {1 1 0} and {0 1 0} surfaces. In situ AFM showed that layers grow by step flow at pre-existing steps by the addition of growth units at the step edges. It has been found that dye concentrations as low as ˜2×10 -6 M for pyranine and ˜4×10 -4 M for acid fuchsin produce significant changes in the step morphology and growth rates. The additive molecules attach to the terraces and pin the growing front. As a consequence, the edges of the growing steps become jagged as the dye molecules are adsorbed onto the crystal surface. At critical dye concentrations crystal growth is heavily hampered or even stopped along certain crystallographic directions producing, on a macroscopic scale, strong habit modifications. The formation of dye inclusions by means of macrosteps overgrowing the poisoned surface was also imaged. Interestingly, comparison of the in situ AFM experiments with previous habit modification studies showed acid fuchsin is also able to enter the {0 1 0} surfaces, a previously unnoticed phenomenon.

Crystallization and preliminary X-ray diffraction analysis of recombinant phosphoribosylpyrophosphate synthetase from the Thermophilic thermus thermophilus strain HB27

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

Abramchik, Yu. A.; Timofeev, V. I., E-mail: tostars@mail.ru; Muravieva, T. I.

2017-01-15

Phosphoribosylpyrophosphate synthetases (PRPP synthetases) are among the key enzymes essential for vital functions of organisms and are involved in the biosynthesis of purine and pyrimidine nucleotides, coenzymes, and the amino acids histidine and tryptophan. These enzymes are used in biotechnology for the combined chemoenzymatic synthesis of natural nucleotide analogs. Recombinant phosphoribosylpyrophosphate synthetase I from the thermophilic strain HB27 of the bacterium Thermus thermophilus (T. th HB27) has high thermal stability and shows maximum activity at 75°Ð¡, due to which this enzyme holds promise for biotechnological applications. In order to grow crystals and study them by X-ray crystallography, an enzyme sample,more » which was produced using a highly efficient producer strain, was purified by affinity and gel-filtration chromatography. The screening of crystallization conditions was performed by the vapor-diffusion technique. The crystals of the enzyme suitable for X-ray diffraction were grown by the counter-diffusion method through a gel layer. These crystals were used to collect the X-ray diffraction data set at the SPring-8 synchrotron radiation facility (Japan) to 3-Å resolution. The crystals belong to sp. gr. P2{sub 1} and have the following unitcell parameters: a = 107.7 Å, b = 112.6 Å, c = 110.2 Å, α = γ = 90°, β = 116.6°. The X-ray diffraction data set is suitable for determining the three-dimensional structure of the enzyme at 3.0-Å resolution.« less

Crystallization and preliminary X-ray diffraction analysis of recombinant phosphoribosylpyrophosphate synthetase from the Thermophilic thermus thermophilus strain HB27

NASA Astrophysics Data System (ADS)

Abramchik, Yu. A.; Timofeev, V. I.; Muravieva, T. I.; Sinitsyna, E. V.; Esipov, R. S.; Kuranova, I. P.

2017-01-01

Phosphoribosylpyrophosphate synthetases (PRPP synthetases) are among the key enzymes essential for vital functions of organisms and are involved in the biosynthesis of purine and pyrimidine nucleotides, coenzymes, and the amino acids histidine and tryptophan. These enzymes are used in biotechnology for the combined chemoenzymatic synthesis of natural nucleotide analogs. Recombinant phosphoribosylpyrophosphate synthetase I from the thermophilic strain HB27 of the bacterium Thermus thermophilus ( T. th HB27) has high thermal stability and shows maximum activity at 75°C, due to which this enzyme holds promise for biotechnological applications. In order to grow crystals and study them by X-ray crystallography, an enzyme sample, which was produced using a highly efficient producer strain, was purified by affinity and gel-filtration chromatography. The screening of crystallization conditions was performed by the vapor-diffusion technique. The crystals of the enzyme suitable for X-ray diffraction were grown by the counter-diffusion method through a gel layer. These crystals were used to collect the X-ray diffraction data set at the SPring-8 synchrotron radiation facility (Japan) to 3-Å resolution. The crystals belong to sp. gr. P21 and have the following unitcell parameters: a = 107.7 Å, b = 112.6 Å, c = 110.2 Å, α = γ = 90°, β = 116.6°. The X-ray diffraction data set is suitable for determining the three-dimensional structure of the enzyme at 3.0-Å resolution.

Noninvasive in situ observation of the crystallization kinetics of biological macromolecules by confocal laser scanning microscopy.

PubMed

Mühlig, P; Klupsch, Th; Kaulmann, U; Hilgenfeld, R

2003-04-01

High-resolution confocal laser scanning microscopy (CLSM) is a powerful tool for in situ observation and analysis of protein crystal growth kinetics. Because the resolution of CLSM is not diffraction-limited by the object, it is possible to visualize, under certain conditions, objects in molecular dimensions. A modified batch technique is applied which allows the growth kinetics of sufficiently small crystallites fixed at the lower side of a cover glass, within a hanging drop, to be studied in reflected light near the total reflection angle. A gap, or cavity, filled with solution is formed between the cover glass and the upper crystal face, which acts to fix small crystallites by hydrodynamic friction forces. The cavity height enables the propagation of molecular steps across the upper crystal face without constraint, so that the propagation velocity and geometrical parameters can be measured by CLSM. The layer growth kinetics of monoclinic crystallites of a long-acting insulin derivative (Insulin Glargine) is investigated. For a twofold supersaturation of the solution, the growth is governed by 2D nucleation at the edges of the crystallites followed by a spreading of molecular steps. The layer growth kinetics are well fitted by the simple cubic kinetic lattice model. We find that only about one of a thousand solute (protein) molecules which push a kink place due to their Brownian motion becomes really incorporated into the growing crystal.

Thermoelectric Properties of Highly-Crystallized Ge-Te-Se Glasses Doped with Cu/Bi.

PubMed

Srinivasan, Bhuvanesh; Boussard-Pledel, Catherine; Dorcet, Vincent; Samanta, Manisha; Biswas, Kanishka; Lefèvre, Robin; Gascoin, Franck; Cheviré, François; Tricot, Sylvain; Reece, Michael; Bureau, Bruno

2017-03-23

Chalcogenide semiconducting systems are of growing interest for mid-temperature range (~500 K) thermoelectric applications. In this work, Ge 20 Te 77 Se₃ glasses were intentionally crystallized by doping with Cu and Bi. These effectively-crystallized materials of composition (Ge 20 Te 77 Se₃) 100- x M x (M = Cu or Bi; x = 5, 10, 15), obtained by vacuum-melting and quenching techniques, were found to have multiple crystalline phases and exhibit increased electrical conductivity due to excess hole concentration. These materials also have ultra-low thermal conductivity, especially the heavily-doped (Ge 20 Te 77 Se₃) 100- x Bi x ( x = 10, 15) samples, which possess lattice thermal conductivity of ~0.7 Wm -1 K -1 at 525 K due to the assumable formation of nano-precipitates rich in Bi, which are effective phonon scatterers. Owing to their high metallic behavior, Cu-doped samples did not manifest as low thermal conductivity as Bi-doped samples. The exceptionally low thermal conductivity of the Bi-doped materials did not, alone, significantly enhance the thermoelectric figure of merit, zT. The attempt to improve the thermoelectric properties by crystallizing the chalcogenide glass compositions by excess doping did not yield power factors comparable with the state of the art thermoelectric materials, as these highly electrically conductive crystallized materials could not retain the characteristic high Seebeck coefficient values of semiconducting telluride glasses.

Thermoelectric Properties of Highly-Crystallized Ge-Te-Se Glasses Doped with Cu/Bi

PubMed Central

Srinivasan, Bhuvanesh; Boussard-Pledel, Catherine; Dorcet, Vincent; Samanta, Manisha; Biswas, Kanishka; Lefèvre, Robin; Gascoin, Franck; Cheviré, François; Tricot, Sylvain; Reece, Michael; Bureau, Bruno

2017-01-01

Chalcogenide semiconducting systems are of growing interest for mid-temperature range (~500 K) thermoelectric applications. In this work, Ge20Te77Se3 glasses were intentionally crystallized by doping with Cu and Bi. These effectively-crystallized materials of composition (Ge20Te77Se3)100−xMx (M = Cu or Bi; x = 5, 10, 15), obtained by vacuum-melting and quenching techniques, were found to have multiple crystalline phases and exhibit increased electrical conductivity due to excess hole concentration. These materials also have ultra-low thermal conductivity, especially the heavily-doped (Ge20Te77Se3)100−xBix (x = 10, 15) samples, which possess lattice thermal conductivity of ~0.7 Wm−1 K−1 at 525 K due to the assumable formation of nano-precipitates rich in Bi, which are effective phonon scatterers. Owing to their high metallic behavior, Cu-doped samples did not manifest as low thermal conductivity as Bi-doped samples. The exceptionally low thermal conductivity of the Bi-doped materials did not, alone, significantly enhance the thermoelectric figure of merit, zT. The attempt to improve the thermoelectric properties by crystallizing the chalcogenide glass compositions by excess doping did not yield power factors comparable with the state of the art thermoelectric materials, as these highly electrically conductive crystallized materials could not retain the characteristic high Seebeck coefficient values of semiconducting telluride glasses. PMID:28772687

Application of the windowed-Fourier-transform-based fringe analysis technique for investigating temperature and concentration fields in fluids.

PubMed

Mohanan, Sharika; Srivastava, Atul

2014-04-10

The present work is concerned with the development and application of a novel fringe analysis technique based on the principles of the windowed-Fourier-transform (WFT) for the determination of temperature and concentration fields from interferometric images for a range of heat and mass transfer applications. Based on the extent of the noise level associated with the experimental data, the technique has been coupled with two different phase unwrapping methods: the Itoh algorithm and the quality guided phase unwrapping technique for phase extraction. In order to generate the experimental data, a range of experiments have been carried out which include cooling of a vertical flat plate in free convection conditions, combustion of mono-propellant flames, and growth of organic as well as inorganic crystals from their aqueous solutions. The flat plate and combustion experiments are modeled as heat transfer applications wherein the interest is to determine the whole-field temperature distribution. Aqueous-solution-based crystal growth experiments are performed to simulate the mass transfer phenomena and the interest is to determine the two-dimensional solute concentration field around the growing crystal. A Mach-Zehnder interferometer has been employed to record the path-integrated quantity of interest (temperature and/or concentration) in the form of interferometric images in the experiments. The potential of the WFT method has also been demonstrated on numerically simulated phase data for varying noise levels, and the accuracy in phase extraction have been quantified in terms of the root mean square errors. Three levels of noise, i.e., 0%, 10%, and 20% have been considered. Results of the present study show that the WFT technique allows an accurate extraction of phase values that can subsequently be converted into two-dimensional temperature and/or concentration distribution fields. Moreover, since WFT is a local processing technique, speckle patterns and the inherent noise in the interferometric data do not affect the resultant phase values. Brief comparisons of the accuracy of the WFT with other standard techniques such as conventional Fourier-filtering methods are also presented.

Protein crystal growth in microgravity

NASA Technical Reports Server (NTRS)

Carter, Daniel

1992-01-01

The overall scientific goals and rationale for growing protein crystals in microgravity are discussed. Data on the growth of human serum albumin crystals which were produced during the First International Microgravity Laboratory (IML-1) are presented. Potential scientific advantages of the utilization of Space Station Freedom are discussed.

Plant ice-binding (antifreeze) proteins

USDA-ARS?s Scientific Manuscript database

Proteins that determine the temperature at which ice crystals will form in water-based solutions in cells and tissues, that bind to growing ice crystals, thus affecting their size, and that impact ice re-crystallization have been widely-documented and studied in many plant, bacterial, fungal, insect...

Growth of single crystals of mercuric iodide (HgI/sub 2/) in spacelab III

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

Van Den Berg, L.; Schnepple, W.F.

1981-01-01

Continued development of a system designed to grow crystals by physical vapor transport in the environment of Spacelab III will be described, with special emphasis on simulation of expected space conditions, adjustment of crystal growth parameters, and on board observation and control of the experiment by crew members and ground personnel. A critical factor in the use of mercuric iodide for semiconductor detectors of x-rays and gamma-rays is the crystalline quality of the material. The twofold purpose of the Spacelab III experiment is therefore to grow single crystals with superior electronic properties as an indirect result of the greatly reducedmore » gravity field during the growth, and to obtain data which will lead to improved understanding of the vapor transport mechanism. The experiments planned to evaluate the space crystals, including gamma-ray diffractometry and measurements of stoichiometry, lattice dimensions, mechanical strength, luminescense, and detector performance are discussed.« less

REE Incorporation into Calcite Individual Crystals as One Time Spike Addition

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

Gabitov, Rinat; Sadekov, Aleksey; Migdisov, Artas

Experiments on the incorporation of trace elements into calcite were performed, and rare earth elements (REE) were used to mark the growth zones of individual crystals. Experiments were conducted at different pH (7.7 to 8.8) and temperatures (2 °C to 24.6 °C) in NH 4Cl + CaCl 2 solutions, where REE were rapidly consumed by growing calcite. LA-ICP-MS line-scans yielded the distribution of (REE/Ca) calcite within individual crystals in a manner consistent with the addition of REE into fluid. A sharp decrease of (REE/Ca) calcite toward the crystal edge suggests the fast depletion of (REE/Ca) fluid due to strong REEmore » consumption by growing calcite. An attempt was made to estimate the lower limit of the partition coefficients between calcite and fluid using selected REE/Ca data within individual calcite crystals and the amount of REE added into fluid.« less

Theory and simulation of buoyancy-driven convection around growing protein crystals in microgravity.

PubMed

Carotenuto, L; Cartwright, J H E; Castagnolo, D; Garcia Ruiz, J M; Otalora, F

2002-01-01

We present an order-of-magnitude analysis of the Navier-Stokes equations in a time-dependent, incompressible and Boussinesq formulation. The hypothesis employed of two different length scales allows one to determine the different flow regimes on the basis of the geometrical and thermodynamical parameters alone, without solving the Navier-Stokes equations. The order-of-magnitude analysis is then applied to the field of protein crystallization, and to the flow field around a crystal, where the driving forces are solutal buoyancy-driven convection, from density dependence on species concentration, and sedimentation caused by the different densities of the crystal and the protein solution. The main result of this paper is to provide predictions of the conditions in which a crystal is growing in a convective regime, rather than in the ideal diffusive state, even under the typical microgravity conditions of space platforms.

Utilisation of adsorption and desorption for simultaneously improving protein crystallisation success rate and crystal quality

NASA Astrophysics Data System (ADS)

Guo, Yun-Zhu; Sun, Li-Hua; Oberthuer, Dominik; Zhang, Chen-Yan; Shi, Jian-Yu; di, Jiang-Lei; Zhang, Bao-Liang; Cao, Hui-Ling; Liu, Yong-Ming; Li, Jian; Wang, Qian; Huang, Huan-Huan; Liu, Jun; Schulz, Jan-Mirco; Zhang, Qiu-Yu; Zhao, Jian-Lin; Betzel, Christian; He, Jian-Hua; Yin, Da-Chuan

2014-12-01

High-quality protein crystals of suitable size are an important prerequisite for applying X-ray crystallography to determine the 3-dimensional structure of proteins. However, it is often difficult to obtain protein crystals of appropriate size and quality because nucleation and growth processes can be unsuccessful. Here, we show that by adsorbing proteins onto porous polystyrene-divinylbenzene microspheres (SDB) floating on the surface of the crystallisation solution, a localised high supersaturation region at the surface of the microspheres and a low supersaturation region below the microspheres can coexist in a single solution. The crystals will easily nucleate in the region of high supersaturation, but when they grow to a certain size, they will sediment to the region of low supersaturation and continue to grow. In this way, the probability of crystallisation and crystal quality can be simultaneously increased in a single solution without changing other crystallisation parameters.

Identification and control of a multizone crystal growth furnace

NASA Technical Reports Server (NTRS)

Batur, C.; Sharpless, R. B.; Duval, W. M. B.; Rosenthal, B. N.; Singh, N. B.

1992-01-01

This paper presents an intelligent adaptive control system for the control of a solid-liquid interface of a crystal while it is growing via directional solidification inside a multizone transparent furnace. The task of the process controller is to establish a user-specified axial temperature profile and to maintain a desirable interface shape. Both single-input-single-output and multi-input-multi-output adaptive pole placement algorithms have been used to control the temperature. Also described is an intelligent measurement system to assess the shape of the crystal while it is growing. A color video imaging system observes the crystal in real time and determines the position and the shape of the interface. This information is used to evaluate the crystal growth rate, and to analyze the effects of translational velocity and temperature profiles on the shape of the interface. Creation of this knowledge base is the first step to incorporate image processing into furnace control.

REE Incorporation into Calcite Individual Crystals as One Time Spike Addition

DOE PAGES

Gabitov, Rinat; Sadekov, Aleksey; Migdisov, Artas

2017-10-26

Experiments on the incorporation of trace elements into calcite were performed, and rare earth elements (REE) were used to mark the growth zones of individual crystals. Experiments were conducted at different pH (7.7 to 8.8) and temperatures (2 °C to 24.6 °C) in NH 4Cl + CaCl 2 solutions, where REE were rapidly consumed by growing calcite. LA-ICP-MS line-scans yielded the distribution of (REE/Ca) calcite within individual crystals in a manner consistent with the addition of REE into fluid. A sharp decrease of (REE/Ca) calcite toward the crystal edge suggests the fast depletion of (REE/Ca) fluid due to strong REEmore » consumption by growing calcite. An attempt was made to estimate the lower limit of the partition coefficients between calcite and fluid using selected REE/Ca data within individual calcite crystals and the amount of REE added into fluid.« less

Liquid Crystal Colloids

NASA Astrophysics Data System (ADS)

Smalyukh, Ivan I.

2018-03-01

Colloids are abundant in nature, science, and technology, with examples ranging from milk to quantum dots and the colloidal atom paradigm. Similarly, liquid crystal ordering is important in contexts ranging from biological membranes to laboratory models of cosmic strings and liquid crystal displays in consumer devices. Some of the most exciting recent developments in both of these soft matter fields emerge at their interface, in the fast-growing research arena of liquid crystal colloids. Mesoscale self-assembly in such systems may lead to artificial materials and to structures with emergent physical behavior arising from patterning of molecular order and nano- or microparticles into precisely controlled configurations. Liquid crystal colloids show exceptional promise for new discovery that may impinge on composite material fabrication, low-dimensional topology, photonics, and so on. Starting from physical underpinnings, I review the state of the art in this fast-growing field, with a focus on its scientific and technological potential.

A Technique for Rapidly Deploying a Concentration Gradient with Applications to Microgravity

NASA Technical Reports Server (NTRS)

Leslie, Fred; Ramachandran, Narayanan

2000-01-01

The latter half of the last century has seen rapid advancements in semiconductor crystal growth powered by the demand for high performance electronics in myriad applications. The reduced gravity environment of space has also been used for crystal growth tests, especially in instances where terrestrial growth has largely been unsuccessful. While reduced gravity crystal growth affords some control of the gravity parameter, many crystals grown in space, to date, have structural flaws believed to result from convective motions during the growth phase. The character of these instabilities is not well understood but is associated with thermal and solutal density variations near the solidification interface in the presence of residual gravity and g-jitter. In order to study these instabilities in a separate, controlled space experiment, a concentration gradient would first have to be artificially established in a timely manner as an initial condition. This is generally difficult to accomplish in a microgravity environment because the momentum of the fluid injected into a test cell tends to swirl around and mix in the absence of a restoring force. The use of magnetic fields to control the motion and position of liquids has received growing interest in recent times. The possibility of using the force exerted by a non-uniform magnetic field on a ferrofluid to not only achieve fluid manipulation but also to actively control fluid motion makes it an attractive candidate for space applications. This paper describes a technique for quickly establishing a linear or exponential fluid concentration gradient using a magnetic field in place of gravity to stabilize the deployment. Also discussed is a photometric technique for measuring the concentration profile using light attenuation. Results of the ground-based experiments indicate that the concentration distribution is within 3% of the predicted value. Although any range of concentations can be realized, photometric constraints are discussed which impose some limitations on measurements.

Assessment of gadolinium calcium oxoborate (GdCOB) for laser applications

NASA Astrophysics Data System (ADS)

Bajor, A. L.; Kisielewski, J.; Kłos, A.; Kopczyński, K.; Łukasiewicz, T.; Mierczyk, J.; Młyńczak, J.

2011-12-01

Increasing demand for growing high quality laser crystals puts a question about their most important parameters that one should concentrate on to get a desired product which will exhibit best properties in practical use. And by no means, this is a simple question. Apart of the usual lasing properties associated with a special dopant in the host material itself, one needs to consider another two lasing phenomena, namely second (SHG) and higher harmonic generation, and self-frequency doubling (SFD). Not necessarily all of these three can meet altogether in the same host material to yield in its best appearance in every case. We have made a review of basic properties of gadolinium oxoborate GdCa4O(BO3)3 (GdCOB) crystal and came to the conclusion that, currently, as a host material this is probably the best in all of its lasing applications. Although GdCOB has low thermal conductivity, which requires a suitable cooling, on the other hand it has got small thermo-optic coefficients which govern good operation in SHG and SFD experiments. Two inch dia. Nd-doped crystals were grown by the Czochralski technique. Since a large discrepancy in the literature exists on exact values of nonlinear coefficients, one is never sure about this whether theoretically predicted phase-matching angles (PMA) are those that are really optimal. Besides, none has yet measured the values of nonlinear coefficients as a function of doping concentration. Therefore we have not decided to cut numerous differently oriented samples for generation of different wavelengths in SHG and SFD, but rather tried to generate different wavelengths from the same samples. We have also not paid special attention to get highest possible conversion efficiencies. However, we have concentrated our attention on potential use of the core region in laser technique. Unlike in YAG crystals, when the core is by all means a parasitic structure, we discovered that the core region in GdCOB, that majority of investigators are even not aware of its presence in the crystal, can be also useful in laser technique. According to our best knowledge, a SHG of red light in this work is the second reported case in the world-wide literature.

Redox process catalysed by growing crystal-strengite, FePO4,2H2O, crystallizing from solution with iron(II) and hydroxylamine

NASA Astrophysics Data System (ADS)

Lundager Madsen, Hans Erik

2014-09-01

In an attempt to grow pure crystals of the iron(II) phosphate vivianite, Fe3(PO4)2,8H2O, from a solution of Mohr's salt, Fe(NH4)2(SO4)2,6H2O, added to a solution of ammonium phosphate, hydroxylammonium chloride, NH3OHCl, was added to the iron(II) stock solution to eliminate oxidation of iron(II) by oxygen from the air. However, the effect turned out to be the opposite of the expected: whereas hydroxylamine reduces iron(III) in bulk solution, it acted as a strong oxidant in the presence of growing iron phosphate crystals, causing the crystallization of the iron(III) phosphate strengite, FePO4,2H2O, as the only solid phase. Evidently the crystal surface catalyses oxidation of iron(II) by hydroxylamine. The usual composite kinetics of spiral growth and surface nucleation was found. The surface-nucleation part yielded edge free energy λ in the range 12-45 pJ/m, virtually independent of temperature and in the range typical for phosphates of divalent metals. The scatter of values for λ presumably arises from contributions from different crystal forms to the overall growth rate. The low mean value points to strong adsorption of iron(II), which is subsequently oxidized at the crystal surface, forming strengite. The state of the system did not tend to thermodynamic equilibrium, but to a metastable state, presumably controlled by the iron(II) rich surface layer of the crystal. In addition to crystal growth, it was possible to measure nucleation kinetics by light scattering (turbidimetry). A point of transition from heterogeneous to homogeneous nucleation was found, and from the results for the homogeneous domain a rather precise value of crystal surface free energy γ=55 mJ/m2 was found. This is a relatively low value as well, indicating that the redox process plays a role already at the nucleation stage.

Scanning electron microscope view of iron crystal

NASA Technical Reports Server (NTRS)

1972-01-01

A scanning electron microscope photograph of iron crystals which grow in a small vug or cavity in a recrystallized breccia (fragmented rock) from the Apollo 15 Hadley-Apennino lunar landing site. The largest crystal is three microns across. Perfectly developed crystals such as these indicate slow formation from a hot vapor as the rock was cooling. The crystals are resting on an interlocking lattice of pyroxene (calsium-magnesium-iron silicate).

Scanning electron microscope view of iron crystal

NASA Image and Video Library

1972-11-10

A scanning electron microscope photograph of iron crystals which grow in a small vug or cavity in a recrystallized breccia (fragmented rock) from the Apollo 15 Hadley-Apennino lunar landing site. The largest crystal is three microns across. Perfectly developed crystals such as these indicate slow formation from a hot vapor as the rock was cooling. The crystals are resting on an interlocking lattice of pyroxene (calsium-magnesium-iron silicate).

Crystals Out of "Thin Air".

ERIC Educational Resources Information Center

Vollmer, John J.

2000-01-01

Describes how to grow crystals of para-dichlorobenzene beginning with household mothballs. The crystals form through sublimation (solid to gas) and deposition (gas to solid). Also discusses demonstrations of evaporation and condensation and odor perception, which can support a study of the kinetic theory and phases of matter. (WRM)

Characteristics of biogenic calcite in the prismatic layer of a pearl oyster, Pinctada fucata.

PubMed

Okumura, Taiga; Suzuki, Michio; Nagasawa, Hiromichi; Kogure, Toshihiro

2010-10-01

The fine structure of the calcite prism in the outer layer of a pearl oyster, Pinctada fucata, has been investigated using various electron beam techniques, in order to understand its characteristics and growth mechanism including the role of intracrystalline organic substances. As the calcite prismatic layer grows thicker, sinuous boundaries develop to divide the prism into a number of domains. The crystal misorientation between the adjacent domains is several to more than ten degrees. The component of the misorientation is mainly the rotation about the c-axis. There is no continuous organic membrane at the boundaries. Furthermore, the crystal orientation inside the domains changes gradually, as indicated by the electron back-scattered diffraction (EBSD) in a scanning electron microscope (SEM). Transmission electron microscopy (TEM) examination revealed that the domain consists of sub-grains of a few hundred nanometers divided by small-angle grain boundaries, which are probably the origin of the gradual change of the crystal orientation inside the domains. Spherular Fresnel contrasts were often observed at the small-angle grain boundaries, in defocused TEM images. Electron energy-loss spectroscopy (EELS) indicated the spherules are organic macromolecules, suggesting that incorporation of organic macromolecules during the crystal growth forms the sub-grain structure of the calcite prism.

Sizing of colloidal particle and protein molecules in a hanging fluid drop

NASA Technical Reports Server (NTRS)

Ansari, Rafat R.; Suh, Kwang I.

1995-01-01

We report non-invasive particle size measurements of polystyrene latex colloidal particles and bovine serum albumin (BSA) protein molecules suspended in tiny hanging fluid drops of 30 micro-Liter volume using a newly designed fiber optic probe. The probe is based upon the principles of the technique of dynamic light scattering (DLS). The motivation for this work comes from growing protein crystals in outer space. Protein crystals have been grown previously in hanging drops in microgravity experiments on-board the space shuttle orbiter. However, obtaining quantitative information on nucleation and growth of the protein crystals in real time has always been a desired goal, but hitherto not achieved. Several protein researchers have shown interest in using DLS to monitor crystal growth process in a droplet, but elaborate instrumentation and optical alignment problems have made in-situ applications difficult. We demonstrate that such an experiment is now possible. Our system offers fast (5 seconds) determination of particle size, utilize safe levels of very low laser power (less than or equal to 0.2 mW), a small scattering volume (approximately 2 x 10(exp -5) cu mm) and high spatial coherence (Beta) values. This is a major step forward when compared to currently available DLS systems.

Urate Oxidase Purification by Salting-in Crystallization: Towards an Alternative to Chromatography

PubMed Central

Giffard, Marion; Ferté, Natalie; Ragot, François; El Hajji, Mohamed; Castro, Bertrand; Bonneté, Françoise

2011-01-01

Background Rasburicase (Fasturtec® or Elitek®, Sanofi-Aventis), the recombinant form of urate oxidase from Aspergillus flavus, is a therapeutic enzyme used to prevent or decrease the high levels of uric acid in blood that can occur as a result of chemotherapy. It is produced by Sanofi-Aventis and currently purified via several standard steps of chromatography. This work explores the feasibility of replacing one or more chromatography steps in the downstream process by a crystallization step. It compares the efficacy of two crystallization techniques that have proven successful on pure urate oxidase, testing them on impure urate oxidase solutions. Methodology/Principal Findings Here we investigate the possibility of purifying urate oxidase directly by crystallization from the fermentation broth. Based on attractive interaction potentials which are known to drive urate oxidase crystallization, two crystallization routes are compared: a) by increased polymer concentration, which induces a depletion attraction and b) by decreased salt concentration, which induces attractive interactions via a salting-in effect. We observe that adding polymer, a very efficient way to crystallize pure urate oxidase through the depletion effect, is not an efficient way to grow crystals from impure solution. On the other hand, we show that dialysis, which decreases salt concentration through its strong salting-in effect, makes purification of urate oxidase from the fermentation broth possible. Conclusions The aim of this study is to compare purification efficacy of two crystallization methods. Our findings show that crystallization of urate oxidase from the fermentation broth provides purity comparable to what can be achieved with one chromatography step. This suggests that, in the case of urate oxidase, crystallization could be implemented not only for polishing or concentration during the last steps of purification, but also as an initial capture step, with minimal changes to the current process. PMID:21589929

Crystal growth furnace with trap doors

DOEpatents

Sachs, Emanual M.; Mackintosh, Brian H.

1982-06-15

An improved furnace is provided for growing crystalline bodies from a melt. The improved furnace is characterized by a door assembly which is remotely controlled and is arranged so as to selectively shut off or permit communication between an access port in the furnace enclosure and a hot zone within that enclosure. The invention is especially adapted to facilitate use of crystal growing cartridges of the type disclosed in U.S. Pat. No. 4,118,197.

Crystal growth furnace with trap doors

NASA Technical Reports Server (NTRS)

Sachs, Emanual M. (Inventor); Mackintosh, Brian H. (Inventor)

1982-01-01

An improved furnace is provided for growing crystalline bodies from a melt. The improved furnace is characterized by a door assembly which is remotely controlled and is arranged so as to selectively shut off or permit communication between an access port in the furnace enclosure and a hot zone within that enclosure. The invention is especially adapted to facilitate use of crystal growing cartridges of the type disclosed in U.S. Pat. No. 4,118,197.

A Physical Chemistry Experiment in Polymer Crystallization Kinetics

ERIC Educational Resources Information Center

Singfield, Kathy L.; Chisholm, Roderick A.; King, Thomas L.

2012-01-01

A laboratory experiment currently used in an undergraduate physical chemistry lab to investigate the rates of crystallization of a polymer is described. Specifically, the radial growth rates of typical disc-shaped crystals, called spherulites, growing between microscope glass slides are measured and the data are treated according to polymer…

Crystallization of steroids in gels

NASA Astrophysics Data System (ADS)

Kalkura, S. Narayana; Devanarayanan, S.

1991-03-01

The crystal growth and characterization of certain steriods, viz., cholesterol, cholesteryl acetate, β-sitosterol, progesterone and testosterone, in a silica gel medium is discussed. The present study shows that the single test tube diffusion method can be used to grow crystals of steroids in a silica gel medium by the reduction of steroid solubility.

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.

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.

Structure, morphology and Raman and optical spectroscopic analysis of In1-xCuxP thin films grown by MOCVD technique for solar cell applications

NASA Astrophysics Data System (ADS)

Alshahrie, Ahmed; Juodkazis, S.; Al-Ghamdi, A. A.; Hafez, M.; Bronstein, L. M.

2017-10-01

Nanocrystalline In1-xCuxP thin films (0 ≤ x ≤ 0.5) have been deposited on quartz substrates by a Metal-Organic Chemical Vapor Deposition (MOCVD) technique. The effect of the copper ion content on the structural crystal lattice, morphology and optical behavior of the InP thin films was assessed using X-ray diffraction, scanning electron microscopy, atomic force microscopy, Raman spectroscopy and spectrophotometry. All films exhibited a crystalline cubic zinc blende structure, inferring the solubility of the Cu atoms in the InP crystal structure. The XRD patterns demonstrated that the inclusion of Cu atoms into the InP films forced the nanoparticles in the films to grow along the (1 1 1) direction. The AFM topography showed that the Cu ions reduce the surface roughness of deposited films. The Raman spectra of the deposited films contain the first and second order anti-stoke ΓTO, ΓLO, ΧLO + ΧTO, 2ΓTO, and ΓLO + ΓTO bands which are characteristic of the InP crystalline structure. The intensities of these bands decreased with increasing the content of the Cu atoms in the InP crystals implying the creation of a stacking fault density in the InP crystal structure. The In1-xCuxP thin films have shown high optical transparency of 90%. An increase of the optical band gap from 1.38 eV to 1.6 eV was assigned to the increase of the amount of Cu ions in the InP films. The In0.5Cu0.5P thin film exhibited remarkable optical conductivity with very low dissipation factor which makes it a promising buffer window for solar energy applications.

Spherulitic Growth of Coral Skeletons and Synthetic Aragonite: Nature’s Three-Dimensional Printing

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

Sun, Chang-Yu; Marcus, Matthew A.; Frazier, Matthew J.

Coral skeletons were long assumed to have a spherulitic structure, that is, a radial distribution of acicular aragonite (CaCO 3) crystals with their c-axes radiating from series of points, termed centers of calcification (CoCs). This assumption was based on morphology alone, not on crystallography. In this paper, we measure the orientation of crystals and nanocrystals and confirm that corals grow their skeletons in bundles of aragonite crystals, with their c-axes and long axes oriented radially and at an angle from the CoCs, thus precisely as expected for feather-like or “plumose” spherulites. Furthermore, we find that in both synthetic and coralmore » aragonite spherulites at the nanoscale adjacent crystals have similar but not identical orientations, thus demonstrating by direct observation that even at nanoscale the mechanism of spherulite formation is non-crystallographic branching (NCB), as predicted by theory. Finally, synthetic aragonite spherulites and coral skeletons have similar angle spreads, and angular distances of adjacent crystals, further confirming that coral skeletons are spherulites. This is important because aragonite grows anisotropically, 10 times faster along the c-axis than along the a-axis direction, and spherulites fill space with crystals growing almost exclusively along the c-axis, thus they can fill space faster than any other aragonite growth geometry, and create isotropic materials from anisotropic crystals. Greater space filling rate and isotropic mechanical behavior are key to the skeleton’s supporting function and therefore to its evolutionary success. Finally, in this sense, spherulitic growth is Nature’s 3D printing.« less

Spherulitic Growth of Coral Skeletons and Synthetic Aragonite: Nature’s Three-Dimensional Printing

DOE PAGES

Sun, Chang-Yu; Marcus, Matthew A.; Frazier, Matthew J.; ...

2017-05-31

Coral skeletons were long assumed to have a spherulitic structure, that is, a radial distribution of acicular aragonite (CaCO 3) crystals with their c-axes radiating from series of points, termed centers of calcification (CoCs). This assumption was based on morphology alone, not on crystallography. In this paper, we measure the orientation of crystals and nanocrystals and confirm that corals grow their skeletons in bundles of aragonite crystals, with their c-axes and long axes oriented radially and at an angle from the CoCs, thus precisely as expected for feather-like or “plumose” spherulites. Furthermore, we find that in both synthetic and coralmore » aragonite spherulites at the nanoscale adjacent crystals have similar but not identical orientations, thus demonstrating by direct observation that even at nanoscale the mechanism of spherulite formation is non-crystallographic branching (NCB), as predicted by theory. Finally, synthetic aragonite spherulites and coral skeletons have similar angle spreads, and angular distances of adjacent crystals, further confirming that coral skeletons are spherulites. This is important because aragonite grows anisotropically, 10 times faster along the c-axis than along the a-axis direction, and spherulites fill space with crystals growing almost exclusively along the c-axis, thus they can fill space faster than any other aragonite growth geometry, and create isotropic materials from anisotropic crystals. Greater space filling rate and isotropic mechanical behavior are key to the skeleton’s supporting function and therefore to its evolutionary success. Finally, in this sense, spherulitic growth is Nature’s 3D printing.« less

Dy uniform film morphologies on graphene studied with SPA-LEED and STM

DOE PAGES

McDougall, D.; Hattab, H.; Hershberger, M. T.; ...

2016-07-01

The use of graphene for microelectronics and spintronic applications requires strategies for metals to wet graphene and to grow layer-by-layer. This is especially important when metals will be used as electrical contacts or as spin filters. Extensive work in the literature so far has shown that this is very challenging, since practically all metals grow 3D, with multi-height islands forming easily. Reasons for the 3D morphology are the much weaker metal carbon bond when compared to the metal cohesive energy and the role of Coulomb repulsion of the poorly screened charges at the metal graphene interface. We employed the complementarymore » techniques of SPA-LEED and STM to study the growth of Dy on graphene. It was found that under kinetic limitations it is possible to fully cover graphene with a bilayer Dy film, by growing well below room temperature in stepwise deposition experiments. Lastly, the Dy film, however, is amorphous but ways to crystallize it within the 2D morphology are possible, since long range order improves at higher growth temperature.« less

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; Curreri, Peter A. (Technical Monitor)

2002-01-01

Experimental evidence indicates a dominant role of solution phase interactions in nucleating and growing tetragonal lysozyme crystals. These interactions are extensive, even at saturation, and may be a primary cause of misoriented regions in crystals grown on Earth. Microgravity, by limiting interfacial concentrations to diffusion-controlled levels, may benefit crystal quality by also reducing the extent of associated species present at the interface.

Determination of a Definition of Solar Grade Silicon

NASA Technical Reports Server (NTRS)

Hill, D. E.; Gutsche, H. W.

1975-01-01

A definition of solar grade silicon was determined by investigating the singular and the combined effect of the impurities usually found in metallurgical grade silicon on solar cell device performance. The impurity matrix was defined by Jet Propulsion Laboratory Technical Direction Memorandum. The initial work was focussed on standardizing the solar cell process and test procedure, growing baseline crystals, growing crystals contaminated with carbon, iron, nickel, zirconium, aluminum and vanadium, solar blank preparation, and material characterization.

Interfacial wave theory for dendritic structure of a growing needle crystal. I - Local instability mechanism. II - Wave-emission mechanism at the turning point

NASA Technical Reports Server (NTRS)

Xu, Jian-Jun

1989-01-01

The complicated dendritic structure of a growing needle crystal is studied on the basis of global interfacial wave theory. The local dispersion relation for normal modes is derived in a paraboloidal coordinate system using the multiple-variable-expansion method. It is shown that the global solution in a dendrite growth process incorporates the morphological instability factor and the traveling wave factor.

Towards true 3D textural analysis; using your crystal mush wisely.

NASA Astrophysics Data System (ADS)

Jerram, D. A.; Morgan, D. J.; Pankhurst, M. J.

2014-12-01

The crystal cargo that is found in volcanic and plutonic rocks contains a wealth of information about magmatic mush processes, crystallisation history, crystal entrainment and recycling. Phenocryst populations predominantly record episodes of growth/nucleation and bulk geochemical changes within an evolving crystal-melt body. Ante- and xeno-crysts provide useful clues to the nature of mush interaction with wall rock and with principal magma(s). Furthermore, crystal evolutions (core to rim) record pathways through pressure, temperature and compositional space. These can often illustrate complex recycling within systems, describing the plumbing architecture. Understanding this architecture underpins our knowledge of how igneous systems can interact with the crust, grow, freeze, re-mobilise and prime for eruption. Initially, 2D studies produced corrected 3D crystal size distributions to help provide information about nucleation and residence times. It immediately became clear that crystal shape is an important factor in determining the confidence placed upon 3D reconstructions of 2D data. Additionally studies utilised serial sections of medium- to coarse-grain-size populations which allowed 3D reconstruction using modelling software to be improved, since size and shape etc. can be directly constrained. Finally the advent of textural studies using X-ray tomography has revolutionised the way in which we can inspect the crystal cargo in mushy systems, allowing us to image in great detail crystal packing arrangements, 3D CSDs, shapes and orientations etc. The latest most innovative studies use X-ray micro-computed tomography to rapidly characterise chemical populations within the crystal cargo, adding a further dimension to this approach, and implies the ability to untangle magmatic chemical components to better understand their individual and combined evolution. In this contribution key examples of the different types of textural analysis techniques in 2D and 3D, including texture movie animations, are used from both plutonic and volcanic systems to highlight the roll of this approach towards a goal of true 3D textural analysis.

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.

Formation of Large (Approximately 100 micrometers) Ice Crystals Near the Tropical Tropopause

NASA Technical Reports Server (NTRS)

Jensen, E. J.; Pfister, L.; Bui, T. V.; Lawson, P.; Baker, B.; Mo, Q.; Baumgardner, D.; Weinstock, E. M.; Smith, J. B.; Moyer, E. J.;

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

Sornadurai, D.; Ravindran, T. R.; Paul, V. Thomas

Synthesis parameters are optimized in order to grow single crystals of multiferroic BiFeO{sub 3}. 2 to 3 mm size pyramid (tetrahedron) shaped single crystals were successfully obtained by solvothermal method. Scanning electron microscopy with EDAX confirmed the phase formation. Raman scattering spectra of bulk BiFeO3 single crystals have been measured which match well with reported spectra.

A photoluminescence, thermoluminescence and electron paramagnetic resonance study of EFG grown europium doped lithium fluoride (LiF) crystals

NASA Astrophysics Data System (ADS)

Seth, Pooja; Swati, G.; Haranath, D.; Rao, S. M. D.; Aggarwal, Shruti

2018-07-01

Europium (Eu) doped LiF crystals have been grown by the Edge-defined film fed growth (EFG) technique. The designing and installation of the furnace used for the growth of the crystals have been discussed in detail. In the present study, Eu (Eu2O3) has been doped in LiF in different concentration (0.02-0.2 wt %). X-ray diffractometry (XRD) and Energy Dispersive X-ray (EDX) spectroscopy confirms the incorporation of Eu in LiF. The influence of Eu on LiF has been investigated through photoluminescence (PL), thermoluminescence (TL) and electron paramagnetic resonance (EPR) in as-grown and annealed crystals. PL emission spectra shows the presence of both Eu3+ and Eu2+ form in the as-grown crystals which is confirmed by EPR results. Whereas, in annealed crystals, Eu is present predominantly as Eu2+ form. This suggests that growing crystals at high temperature (∼900 °C) in argon gas atmosphere through EFG technique favours the reduction of Eu3+ → Eu2+. This reduction phenomenon has been explained on the basis of charge compensation model. TL study of the LiF: Eu (0.02-0.2 wt %) crystals has been done after irradiation with Co60 gamma rays. In this study, it has been observed that the TL intensity as well as glow curve structure of LiF: Eu crystals are a strong function of Eu concentration. The maximum TL is observed at Eu concentration of 0.05 wt% at which a well defined glow curve structure with a prominent peak at 185 °C and a small peak at 253 °C. Beyond this concentration (0.05 wt %), TL intensity decreases due to aggregation of defects in the host. The peak at 185 °C in LiF: Eu (0.05 wt %) is certainly due to the presence of Eu2+ associated defects which is also supported by the PL spectra. It has been observed that Eu doping have a key role in creation of more defect levels which lead to the increased number of electron and hole traps. Further, trapping parameters are analysed using glow curve deconvolution method to have an insight study of TL phenomena. Further, TL glow curve structure of as-grown and annealed crystal are distinct which may be attributed to the nature of defect traps formed inside the LiF.

Semiconducting icosahedral boron arsenide crystal growth for neutron detection

NASA Astrophysics Data System (ADS)

Whiteley, C. E.; Zhang, Y.; Gong, Y.; Bakalova, S.; Mayo, A.; Edgar, J. H.; Kuball, M.

2011-03-01

Semiconducting icosahedral boron arsenide, B12As2, is an excellent candidate for neutron detectors, thermoelectric converters, and radioisotope batteries, for which high quality single crystals are required. Thus, the present study was undertaken to grow B12As2 crystals by precipitation from metal solutions (nickel) saturated with elemental boron (or B12As2 powder) and arsenic in a sealed quartz ampoule. B12As2 crystals of 10-15 mm were produced when a homogeneous mixture of the three elements was held at 1150 °C for 48-72 h and slowly cooled (3.5 °C/h). The crystals varied in color and transparency from black and opaque to clear and transparent. X-ray topography (XRT), and elemental analysis by energy dispersive X-ray spectroscopy (EDS) confirmed that the crystals had the expected rhombohedral structure and chemical stoichiometry. The concentrations of residual impurities (nickel, carbon, etc.) were low, as measured by Raman spectroscopy and secondary ion mass spectrometry (SIMS). Additionally, low etch-pit densities (4.4×107 cm-2) were observed after etching in molten KOH at 500 °C. Thus, the flux growth method is viable for growing large, high-quality B12As2 crystals.

Diamond Lattice Colloidal Crystals from Binary DNA-grafted Microspheres

NASA Astrophysics Data System (ADS)

Crocker, John; Wang, Yifan; Jenkins, Ian; McGinley, James; Sinno, Talid

Future optical materials promise to do for photonics what semiconductors did for electronics, but the challenge has long been in creating the structure they require regular, three-dimensional array of transparent microspheres arranged like the atoms in a diamond crystal. Here we demonstrate a simple approach for spontaneously growing double-diamond (or B32) crystals from a binary suspension of sub-micron polymer microspheres with synthetic DNA grafted to their surfaces. While diamond symmetry crystals have previously been grown from much smaller nanoparticles, none of those methods appear workable for the larger particles needed for photonic applications, whose size must be comparable to the wavelength of visible light. Intriguingly, matched simulations fail to nucleate or grow B32 crystals from suspension; nor have they been predicted on the basis of theoretical arguments. We conjecture that the B32 crystals may form via transformation from a precursor with a different lattice structure in the bulk or on its surface. The feasibility of converting our self-assembled crystals into diamond-symmetry photonic templates will be discussed. This finding suggests that still other unexpected microstructures may be accessible using this approach. US National Science Foundation, CBET- 1403237.

Modeling dislocation generation in high pressure Czochralski growth of indium phosphide single crystals

NASA Astrophysics Data System (ADS)

Pendurti, Srinivas

InP is an important material for opto-electronic and high speed electronics applications. Its main use today is as the substrate material for epitaxy to produce GaInAsP lasers. The present technology for growing bulk InP is the high pressure Czochralski process. Bulk InP grown through this technique suffers from presence of a high density of line defects or dislocations, which are produced by thermal stresses the material goes through during its growth in the high temperature furnace. Modeling of these thermal stresses and the resulting plastic deformation, giving rise to dislocation densities, entails simulation of the entire thermal history of the crystal during its growth in the furnace, and studying the deformation of the crystal through suitable visco-plastic constitutive equations. Accordingly, a suitable visco-plastic model for deformation of InP was constructed, integrated with the ABAQUS finite element code, and verified through experimental data for uniaxial constant strain rate deformation tests available in literature. This was then coupled with a computation fluid dynamics model, predicting the entire temperature history in the furnace during crystal growth, to study the plastic deformation and dislocation density evolution in the crystal during growth. Growth in a variety of conditions was simulated and those conditions that generate minimum dislocation density identified. Macroscopic controllable parameters that affect the dislocation densities the most, have also been delineated. It was found that the strength of gas convection in the Czochralski furnace has the strongest effect on the dislocation densities in the fully grown crystal. Comparison of the simulated dislocation densities on wafers, with experimentally recorded etch pit profiles on as-grown crystals was reasonable. Finally some limitations in the work are discussed and avenues for future work identified.

Mercury-cadmium-telluride - Technical significance and microgravity relevance related to crystal growth

NASA Astrophysics Data System (ADS)

Walcher, H.; Diehl, R.; Baars, J.

The technical importance of the mixed-crystal system Hg(1-x)Cd(x)Te (MCT) is related to a growing interest in detector devices for the infrared spectral ranges of the two atmospheric 'windows'. Applications are not restricted to the military sector, but are also related to astronomy, archeology, medicine, construction engineering, fire fighting, and the determination of pollutants in the atmosphere. It is found that MCT is uniquely qualified for the considered applications, because no other material combines, in the same way, all the required characteristics. However, problems arise in connection with the need for pure, homogeneous, single crystals of adequate size, which are free of any defects. The best results in attempts to grow such crystals have been obtained in experiments utilizing the traveling heater method (THM). Remaining difficulties are caused by effects of gravity. It is, therefore, expected that the crystals needed can be produced under conditions of microgravity. Suitable experiments for exploring this possibility are discussed.

Evolutionary selection growth of two-dimensional materials on polycrystalline substrates

NASA Astrophysics Data System (ADS)

Vlassiouk, Ivan V.; Stehle, Yijing; Pudasaini, Pushpa Raj; Unocic, Raymond R.; Rack, Philip D.; Baddorf, Arthur P.; Ivanov, Ilia N.; Lavrik, Nickolay V.; List, Frederick; Gupta, Nitant; Bets, Ksenia V.; Yakobson, Boris I.; Smirnov, Sergei N.

2018-03-01

There is a demand for the manufacture of two-dimensional (2D) materials with high-quality single crystals of large size. Usually, epitaxial growth is considered the method of choice1 in preparing single-crystalline thin films, but it requires single-crystal substrates for deposition. Here we present a different approach and report the synthesis of single-crystal-like monolayer graphene films on polycrystalline substrates. The technological realization of the proposed method resembles the Czochralski process and is based on the evolutionary selection2 approach, which is now realized in 2D geometry. The method relies on `self-selection' of the fastest-growing domain orientation, which eventually overwhelms the slower-growing domains and yields a single-crystal continuous 2D film. Here we have used it to synthesize foot-long graphene films at rates up to 2.5 cm h-1 that possess the quality of a single crystal. We anticipate that the proposed approach could be readily adopted for the synthesis of other 2D materials and heterostructures.

Human Recombinant Insulin 1g - ug

NASA Technical Reports Server (NTRS)

2004-01-01

Proteins are the building blocks of our bodies and the living world around us. Within our bodies proteins make it possible for red blood cells to carry oxygen throughout the body. Others help transmit nerve impulses so we can hear, smell and feel the world around us. While others play a crucial role in preventing or causing disease. If the structure of a protein is known, then companies can develop new or improved drugs to fight the disease of which the protein is a part. To determine protein structure, researchers must grow near-perfect crystals of the protein. On Earth convection currents, sedimentation and other gravity-induced phenomena hamper crystal growth efforts. In microgravity researchers can grow near-perfect crystals in an environment free of these effects. Because of the enormous potential for new pharmaceutical products the Center for Macromolecular Crystallography--the NASA Commercial Space Center responsible for commercial protein crystal growth efforts has more than fifty major industry and academic partners. Research on crystals of human insulin could lead to improved treatments for diabetes.

Microgravity

NASA Image and Video Library

2004-04-15

Proteins are the building blocks of our bodies and the living world around us. Within our bodies proteins make it possible for red blood cells to carry oxygen throughout the body. Others help transmit nerve impulses so we can hear, smell and feel the world around us. While others play a crucial role in preventing or causing disease. If the structure of a protein is known, then companies can develop new or improved drugs to fight the disease of which the protein is a part. To determine protein structure, researchers must grow near-perfect crystals of the protein. On Earth convection currents, sedimentation and other gravity-induced phenomena hamper crystal growth efforts. In microgravity researchers can grow near-perfect crystals in an environment free of these effects. Because of the enormous potential for new pharmaceutical products the Center for Macromolecular Crystallography--the NASA Commercial Space Center responsible for commercial protein crystal growth efforts has more than fifty major industry and academic partners. Research on crystals of human insulin could lead to improved treatments for diabetes.

Thermodynamic reactivity, growth and characterization of mercurous halide crystals

NASA Technical Reports Server (NTRS)

Singh, N. B.; Gottlieb, M.; Henningsen, T.; Hopkins, R. H.; Mazelsky, R.; Singh, M.; Glicksman, M. E.; Paradies, C.

1992-01-01

Thermodynamic calculations were carried out for the Hg-X-O system (X = Cl, Br, I) to identify the potential sources of contamination and relative stability of oxides and oxy-halide phases. The effect of excess mercury vapor pressure on the optical quality of mercurous halide crystal was studied by growing several mercurous chloride crystals from mercury-rich composition. The optical quality of crystals was examined by birefringence interferometry and laser scattering studies. Crystals grown in slightly mercury-rich composition showed improved optical quality relative to stoichiometric crystals.

A numerical study of zone-melting process for the thermoelectric material of Bi2Te3

NASA Astrophysics Data System (ADS)

Chen, W. C.; Wu, Y. C.; Hwang, W. S.; Hsieh, H. L.; Huang, J. Y.; Huang, T. K.

2015-06-01

In this study, a numerical model has been established by employing a commercial software; ProCAST, to simulate the variation/distribution of temperature and the subsequent microstructure of Bi2Te3 fabricated by zone-melting technique. Then an experiment is conducted to measure the temperature variation/distribution during the zone-melting process to validate the numerical system. Also, the effects of processing parameters on crystallization microstructure such as moving speed and temperature of heater are numerically evaluated. In the experiment, the Bi2Te3 powder are filled into a 30mm diameter quartz cylinder and the heater is set to 800°C with a moving speed 12.5 mm/hr. A thermocouple is inserted in the Bi2Te3 powder to measure the temperature variation/distribution of the zone-melting process. The temperature variation/distribution measured by experiment is compared to the results of numerical simulation. The results show that our model and the experiment are well matched. Then the model is used to evaluate the crystal formation for Bi2Te3 with a 30mm diameter process. It's found that when the moving speed is slower than 17.5 mm/hr, columnar crystal is obtained. In the end, we use this model to predict the crystal formation of zone-melting process for Bi2Te3 with a 45 mm diameter. The results show that it is difficult to grow columnar crystal when the diameter comes to 45mm.

Crystallization of TiO2 Nanotubes by In Situ Heating TEM

PubMed Central

Casu, Alberto; Lamberti, Andrea

2018-01-01

The thermally-induced crystallization of anodically grown TiO2 amorphous nanotubes has been studied so far under ambient pressure conditions by techniques such as differential scanning calorimetry and in situ X-ray diffraction, then looking at the overall response of several thousands of nanotubes in a carpet arrangement. Here we report a study of this phenomenon based on an in situ transmission electron microscopy approach that uses a twofold strategy. First, a group of some tens of TiO2 amorphous nanotubes was heated looking at their electron diffraction pattern change versus temperature, in order to determine both the initial temperature of crystallization and the corresponding crystalline phases. Second, the experiment was repeated on groups of few nanotubes, imaging their structural evolution in the direct space by spherical aberration-corrected high resolution transmission electron microscopy. These studies showed that, differently from what happens under ambient pressure conditions, under the microscope’s high vacuum (p < 10−5 Pa) the crystallization of TiO2 amorphous nanotubes starts from local small seeds of rutile and brookite, which then grow up with the increasing temperature. Besides, the crystallization started at different temperatures, namely 450 and 380 °C, when the in situ heating was performed irradiating the sample with electron beam energy of 120 or 300 keV, respectively. This difference is due to atomic knock-on effects induced by the electron beam with diverse energy. PMID:29342894

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

NASA Technical Reports Server (NTRS)

Su, Ching-Hua; Brebrick, R. F.; Dudley, M.; Ramachandran, N.; Curreri, Peter A. (Technical Monitor)

2002-01-01

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 buoyance-driven convection and growth interface fluctuations caused by irregular fluid-flows. ZnSe and related ternary compounds, such as ZnSeS and ZnSeTe, were grown by vapor transport technique with real time in-situ non-invasive monitoring techniques. The grown crystals were characterized extensively to correlate the grown crystal properties with the growth conditions. The following are the research progress in the past two years. In-situ monitoring of partial pressure by optical absorption technique and visual observation of the growing crystal were performed during vapor growth of ZnSe. Low-temperature photoluminescence (PL) spectra and glow discharge mass spectroscopy (GDMS) were measured on ZnSe starting materials provided by various vendors and on bulk crystals grown from these starting materials by physical vapor transport (PVT) to study the effects of purification and contamination during crystal growth process. Optical characterization was performed on wafers sliced from the grown crystals of ZnSe, ZnTe and ZnSe(1-x),Te(x), (0

Magnetic spherical cores partly coated with periodic mesoporous organosilica single crystals.

PubMed

Li, Jing; Wei, Yong; Li, Wei; Deng, Yonghui; Zhao, Dongyuan

2012-03-07

Core-shell structured materials are of special significance in various applications. Until now, most reported core-shell structures have polycrystalline or amorphous coatings as their shell layers, with popular morphologies of microspheres or quasi-spheres. However, the single crystals, either mesoscale or atomic ones, are still rarely reported as shell layers. If single crystals can be coated on core materials, it would result in a range of new type core-shell structures with various morphologies, and probably more potential applications. In this work, we demonstrate that periodic mesoporous organosilica (PMO) single crystals can partly grow on magnetic microspheres to form incomplete Fe(3)O(4)@nSiO(2)@PMO core-shell materials in aqueous solution, which indeed is the first illustration that mesoporous single-crystal materials can be used as shell layers for preparation of core-shell materials. The achieved materials have advantages of high specific surface areas, good magnetic responses, embedded functional groups and cubic mesopore channels, which might provide them with various application conveniences. We suppose the partial growth is largely decided by the competition between growing tendency of single crystals and the resistances to this tendency. In principle, other single crystals, including a range of atomic single crystals, such as zeolites, are able to be developed into such core-shell structures.

Silicon web process development

NASA Technical Reports Server (NTRS)

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

1981-01-01

The silicon web process takes advantage of natural crystallographic stabilizing forces to grow long, thin single crystal ribbons directly from liquid silicon. The ribbon, or web, is formed by the solidification of a liquid film supported by surface tension between two silicon filaments, called dendrites, which border the edges of the growing strip. The ribbon can be propagated indefinitely by replenishing the liquid silicon as it is transformed to crystal. The dendritic web process has several advantages for achieving low cost, high efficiency solar cells. These advantages are discussed.

Laser radiation frequency doubling in a single-crystal fibre based on a stoichiometric LiNbO3 crystal

NASA Astrophysics Data System (ADS)

Kashin, V. V.; Nikolaev, D. A.; Rusanov, S. Ya; Tsvetkov, V. B.

2015-01-01

We demonstrate the employment of single-crystal optical fibres based on lithium niobate for doubling the laser radiation frequency. The measured characteristics of the fibre confirm its high quality and spatial homogeneity. Parameters of the frequency doublers for neodymium laser radiation (λ = 1 mm) based on fibre and bulk single crystals are compared. Single crystals are grown by the method of laser-heated pedestal growing with heating by radiation of a CO2 laser (LHPG-method).

Determination of the Contact Angle Based on the Casimir Effect

NASA Technical Reports Server (NTRS)

Mazuruk, Konstantin; Volz, Martin P.

2015-01-01

On a macroscopic scale, a nonreactive liquid partially covering a homogeneous solid surface will intersect the solid at an angle called the contact angle. For molten metals and semiconductors, the contact angle is materially dependent upon both the solid and liquid and typical values fall in the range 80-170 deg, depending on the crucible material. On a microscopic scale, there does not exist a precise and sharp contact angle but rather the liquid and solid surfaces merge smoothly and continuously. Consider the example of the so called detached Bridgman crystal growth process. In this technique, a small gap is formed between the growing crystal and the crucible. At the crystal/melt interface, a meniscus ring is formed. Its width can be in the range of a few micrometers, approaching a microscopic scale. It then becomes questionable to describe the shape of this meniscus by the contact angle. A more advanced treatment of the interface is needed and here we propose such a refined model. The interaction of the liquid surface with the solid can be calculated by considering two forces: a short-range repulsive force and a longer range (up to a few micrometers) Casimir or van der Waals force.

Self-assembly of vertically aligned quantum ring-dot structure by Multiple Droplet Epitaxy

NASA Astrophysics Data System (ADS)

Elborg, Martin; Noda, Takeshi; Mano, Takaaki; Kuroda, Takashi; Yao, Yuanzhao; Sakuma, Yoshiki; Sakoda, Kazuaki

2017-11-01

We successfully grow vertically aligned quantum ring-dot structures by Multiple Droplet Epitaxy technique. The growth is achieved by depositing GaAs quantum rings in a first droplet epitaxy process which are subsequently covered by a thin AlGaAs barrier. In a second droplet epitaxy process, Ga droplets preferentially position in the center indentation of the ring as well as attached to the edge of the ring in [ 1 1 bar 0 ] direction. By designing the ring geometry, full selectivity for the center position of the ring is achieved where we crystallize the droplets into quantum dots. The geometry of the ring and dot as well as barrier layer can be controlled in separate growth steps. This technique offers great potential for creating complex quantum molecules for novel quantum information technologies.

Material electronic quality specifications for polycrystalline silicon wafers

NASA Astrophysics Data System (ADS)

Kalejs, J. P.

1994-06-01

As the use of polycrystalline silicon wafers has expanded in the photovoltaic industry, the need grows for monitoring and qualification techniques for as-grown material that can be used to optimize crystal growth and help predict solar cell performance. Particular needs are for obtaining quantitative measures over full wafer areas of the effects of lifetime limiting defects and of the lifetime upgrading taking place during solar cell processing. We review here the approaches being pursued in programs under way to develop material quality specifications for thin Edge-defined Film-fed Growth (EFG) polycrystalline silicon as-grown wafers. These studies involve collaborations between Mobil Solar, and NREL and university-based laboratories.

Germanium layers grown by zone thermal crystallization from a discrete liquid source

NASA Astrophysics Data System (ADS)

Yatsenko, A. N.; Chebotarev, S. N.; Lozovskii, V. N.; Mohamed, A. A. A.; Erimeev, G. A.; Goncharova, L. M.; Varnavskaya, A. A.

2017-11-01

It is proposed and investigated a method for growing thin uniform germanium layers onto large silicon substrates. The technique uses the hexagonally arranged local sources filled with liquid germanium. Germanium evaporates on very close substrate and in these conditions the residual gases vapor pressure highly reduces. It is shown that to achieve uniformity of the deposited layer better than 97% the critical thickness of the vacuum zone must be equal to l cr = 1.2 mm for a hexagonal arranged system of round local sources with the radius of r = 0.75 mm and the distance between the sources of h = 0.5 mm.

Direct Visualization of an Impurity Depletion Zone

NASA Technical Reports Server (NTRS)

Chernov, Alex A.; Garcia-Ruiz, Juan Ma; Thomas, Bill R.

2000-01-01

When a crystal incorporates more impurity per unit of its volume than the impurity concentration in solution, the solution in vicinity of the growing crystal is depleted with respect to the impurity I,2. With a stagnant solution, e. g. in microgravity or gels, an impurity depletion zone expands as the crystal grows and results in greater purity in most of the outer portion of the crystal than in the core. Crystallization in gel provides an opportunity to mimic microgravity conditions and visualize the impurity depletion zone. Colorless, transparent apoferritin (M congruent to 450 KDa) crystals were grown in the presence of red holoferritin dimer as a microheterogeneous impurity (M congruent to 900 KDa) within agarose gel by counterdiffusion with Cd(2+) precipitant. Preferential trapping of dimers, (distribution coefficient K = 4 (exp 1,2)) results in weaker red color around the crystals grown in the left tube in the figure as compared to the control middle tube without crystals. The left and the middle tubes contain colored ferritin dimers, the right tube contains colored trimers. The meniscus in the left tube separate gel (below) and liquid solution containing Cd(2+) (above). Similar solutions, though without precipitants, were present on top of the middle and right tube allowing diffusion of dimers and trimers. The area of weaker color intensity around crystals directly demonstrates overlapped impurity depletion zones.

Impact of Supramolecular Aggregation on the Crystallization Kinetics of Organic Compounds from the Supercooled Liquid State.

PubMed

Kalra, Arjun; Tishmack, Patrick; Lubach, Joseph W; Munson, Eric J; Taylor, Lynne S; Byrn, Stephen R; Li, Tonglei

2017-06-05

Despite numerous challenges in their theoretical description and practical implementation, amorphous drugs are of growing importance to the pharmaceutical industry. One such challenge is to gain molecular level understanding of the propensity of a molecule to form and remain as a glassy solid. In this study, a series of structurally similar diarylamine compounds was examined to elucidate the role of supramolecular aggregation on crystallization kinetics from supercooled liquid state. The structural similarity of the compounds makes it easier to isolate the molecular features that affect crystallization kinetics and glass forming ability of these compounds. To examine the role of hydrogen-bonded aggregation and motifs on crystallization kinetics, a combination of thermal and spectroscopic techniques was employed. Using variable temperature FTIR, Raman, and solid-state NMR spectroscopies, the presence of hydrogen bonding in the melt and glassy state was examined and correlated with observed phase transition behaviors. Spectroscopic results revealed that the formation of hydrogen-bonded aggregates involving carboxylic acid and pyridine nitrogen (acid-pyridine aggregates) between neighboring molecules in the melt state impedes crystallization, while the presence of carboxylic acid dimers (acid-acid dimers) in the melt favors crystallization. This study suggests that glass formation of small molecules is influenced by the type of intermolecular interactions present in the melt state and the kinetics associated with the molecules to assemble into a crystalline lattice. For the compounds that form acid-pyridine aggregates, the formation of energy degenerate chains, produced due to conformational flexibility of the molecules, presents a kinetic barrier to crystallization. The poor crystallization tendency of these aggregates stems from the highly directional hydrogen-bonding interactions needed to form the acid-pyridine chains. Conversely, for the compounds that form acid-acid dimers, the nondirectional van der Waals forces needed to construct a nucleus promote rapid assembly and crystallization.

Thermal-capillary analysis of small-scale floating zones Steady-state calculations

NASA Technical Reports Server (NTRS)

Duranceau, J. L.; Brown, R. A.

1986-01-01

Galerkin finite element analysis of a thermal-capillary model of the floating zone crystal growth process is used to predict the dependence of molten zone shape on operating conditions for the growth of small silicon boules. The model accounts for conduction-dominated heat transport in the melt, feed rod and growing crystal and for radiation between these phases, the ambient and a heater. Surface tension acting on the shape of the melt/gas meniscus counteracts gravity to set the shape of the molten zone. The maximum diameter of the growing crystal is set by the dewetting of the melt from the feed rod when the crystal radius is large. Calculations with small Bond number show the increased zone lengths possible for growth in a microgravity environment. The sensitivity of the method to the shape and intensity of the applied heating distribution is demonstrated. The calculations are compared with experimental observations.

In vitro growth of flat aragonite crystals between the layers of the insoluble organic matrix of the abalone Haliotis laevigata

NASA Astrophysics Data System (ADS)

Gries, Katharina I.; Heinemann, Fabian; Rosenauer, Andreas; Fritz, Monika

2012-11-01

Nacre of abalone shells consists of aragonite platelets and organic material, the so-called organic matrix. During the growth process of the shell the aragonite platelets grow into a scaffold formed by the organic matrix. In this work we tried to mimic this growth process by placing a piece of the insoluble organic matrix (which is a part of the organic matrix) of the abalone Haliotis laevigata in a crystallization device which was flowed through by CaCl2 and NaHCO3 solutions. Using this setup amongst others flat aragonite crystals grow on the insoluble organic matrix. When investigating these crystals in a transmission electron microscope it is possible to recognize similarities to the structure of nacre, like the formation of mineral bridges and growth between layers of the insoluble organic matrix. These similarities are presented in this paper.

Growth of single crystals from solutions using semi-permeable membranes

NASA Astrophysics Data System (ADS)

Varkey, A. J.; Okeke, C. E.

1983-05-01

A technique suitable for growth of single crystals from solutions using semi-preamble membranes is described. Using this technique single crystals of copper sulphate, potassium bromide and ammonium dihydrogen phosphate have been successfully grown. Advantages of this technique over other methods are discussed.

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.

Commander Bowersox Tends to Zeolite Crystal Samples Aboard Space Station

NASA Technical Reports Server (NTRS)

2003-01-01

Expedition Six Commander Ken Bowersox spins Zeolite Crystal Growth sample tubes to eliminate bubbles that could affect crystal formation in preparation of a 15 day experiment aboard the International Space Station (ISS). Zeolites are hard as rock, yet are able to absorb liquids and gases like a sponge. By using the ISS microgravity environment to grow better, larger crystals, NASA and its commercial partners hope to improve petroleum manufacturing and other processes.

Methods for improved growth of group III nitride buffer layers

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

Melnik, Yurity; Chen, Lu; Kojiri, Hidehiro

Methods are disclosed for growing high crystal quality group III-nitride epitaxial layers with advanced multiple buffer layer techniques. In an embodiment, a method includes forming group III-nitride buffer layers that contain aluminum on suitable substrate in a processing chamber of a hydride vapor phase epitaxy processing system. A hydrogen halide or halogen gas is flowing into the growth zone during deposition of buffer layers to suppress homogeneous particle formation. Some combinations of low temperature buffers that contain aluminum (e.g., AlN, AlGaN) and high temperature buffers that contain aluminum (e.g., AlN, AlGaN) may be used to improve crystal quality and morphologymore » of subsequently grown group III-nitride epitaxial layers. The buffer may be deposited on the substrate, or on the surface of another buffer. The additional buffer layers may be added as interlayers in group III-nitride layers (e.g., GaN, AlGaN, AlN).« less

High compositional homogeneity of CdTe{sub x}Se{sub 1−x} crystals grown by the Bridgman method

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

Roy, U. N.; Bolotnikov, A. E.; Camarda, G. S.

2015-02-01

We obtained high-quality CdTe{sub x}Se{sub 1−x} (CdTeSe) crystals from ingots grown by the vertical Bridgman technique. The compositional uniformity of the ingots was evaluated by X-ray fluorescence at BNL’s National Synchrotron Light Source X27A beam line. The compositional homogeneity was highly uniform throughout the ingot, and the effective segregation coefficient of Se was ∼1.0. This high uniformity offers potential opportunity to enhance the yield of the materials for both infrared substrate and radiation-detector applications, so greatly lowering the cost of production and also offering us the prospect to grow large-diameter ingots for use as large-area substrates and for producing highermore » efficiency gamma-ray detectors. The concentration of secondary phases was found to be much lower, by eight- to ten fold compared to that of conventional Cd{sub x}Zn{sub 1−x}Te (CdZnTe or CZT)« less

High Compositional Homogeneity of CdTe xSe 1-x Crystals Grown by the Bridgman Method

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

Roy, U. N.; Bolotnikov, A. E.; Camarda, G. S.

2015-02-03

We obtained high-quality CdTe xSe 1-x (CdTeSe) crystals from ingots grown by the vertical Bridgman technique. The compositional uniformity of the ingots was evaluated by X-ray fluorescence at BNL’s National Synchrotron Light Source X27A beam line. The resulting compositional homogeneity was highly uniform throughout the ingot, and the effective segregation coefficient of Se was ~1.0. This uniformity offers potential opportunity to enhance the yield of the materials for both infrared substrate and radiation-detector applications, so greatly lowering the cost of production and also offering us the prospect to grow large-diameter ingots for use as large-area substrates and for producing highermore » efficiency gamma-ray detectors. The concentration of secondary phases was found to be much lower, by eight- to ten fold compared to that of conventional Cd xZn 1-xTe (CdZnTe or CZT).« less

Electrooptic crystal growth and properties

NASA Astrophysics Data System (ADS)

1994-02-01

A new member in the tungsten-bronze family of ferroelectric lead potassium niobate (PKN), with general formula Pb(1-x)K(2x)Nb2O6, has been grown as bulk single crystal. Growth of PKN with charge composition x = 0.23 has been achieved using the Czochralski technique of crystal pulling. Large diameter boules were grown in platinum crucibles at temperatures between 1280 and 1300 C. Crystallographic studies were conducted using x ray diffraction techniques. The samples were characterized for ferroelectric properties between 25 and 600 C and for optical absorption. This paper presents the crystal synthesis and the results of ferroelectric and optical characterization. Bulk single crystals of potassium tantalate niobate, KTa(1-x)Nb(x)O3, ferroelectric with different values of Ta/Nb ratios have been grown by temperature gradient transport technique (TGTT). A second attached paper presents the results of the crystal growth experiments, ferroelectric characterization techniques, and properties of potassium tantalate niobate crystals.

Molecule diagram from earth-grown crystals

NASA Technical Reports Server (NTRS)

2004-01-01

Like many chemicals in the body, the three-dimensional structure of insulin is extremely complex. When grown on the ground, insulin crystals do not grow as large or as ordered as researchers desire--obscuring the blueprint of the insulin molecules.

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.

Droplet based microfluidics.

PubMed

Seemann, Ralf; Brinkmann, Martin; Pfohl, Thomas; Herminghaus, Stephan

2012-01-01

Droplet based microfluidics is a rapidly growing interdisciplinary field of research combining soft matter physics, biochemistry and microsystems engineering. Its applications range from fast analytical systems or the synthesis of advanced materials to protein crystallization and biological assays for living cells. Precise control of droplet volumes and reliable manipulation of individual droplets such as coalescence, mixing of their contents, and sorting in combination with fast analysis tools allow us to perform chemical reactions inside the droplets under defined conditions. In this paper, we will review available drop generation and manipulation techniques. The main focus of this review is not to be comprehensive and explain all techniques in great detail but to identify and shed light on similarities and underlying physical principles. Since geometry and wetting properties of the microfluidic channels are crucial factors for droplet generation, we also briefly describe typical device fabrication methods in droplet based microfluidics. Examples of applications and reaction schemes which rely on the discussed manipulation techniques are also presented, such as the fabrication of special materials and biophysical experiments.

Morphology and kinetics of crystals growth in amorphous films of Cr2O3, deposited by laser ablation

NASA Astrophysics Data System (ADS)

Bagmut, Aleksandr

2018-06-01

An electron microscopic investigation was performed on the structure and kinetics of the crystallization of amorphous Cr2O3 films, deposited by pulsed laser sputtering of chromium target in an oxygen atmosphere. The crystallization was initiated by the action of an electron beam on an amorphous film in the column of a transmission electron microscope. The kinetic curves were plotted on the basis of a frame-by-frame analysis of the video recorded during the crystallization of the film. It was found that the amorphous phase - crystal phase transition in Cr2O3 films occurs as a layer polymorphic crystallization and is characterized by the values of the dimensionless relative length unit δ0 ≈ 2000-3100. The action of the electron beam initiates the formation of crystals of two basic morphological forms: disk-shaped and sickle-shaped. Growth of a disk-shaped crystals is characterized by a constant rate v and the quadratic dependence of the fraction of the crystalline phase x on the time t. Sickle-shaped crystal at an initial stage, as it grows, becomes as ring-shaped and disk-shaped crystal. The growth of a sickle-shaped crystal is characterized by normal and tangential velocity components, which depend on the time as ∼√t and as ∼1/√t respectively The end point of the arc at the interface between the amorphous and crystalline phases as the crystal grows describes a curve, which is similar to the Fermat helix. For sickle-shaped, as well as for disk-shaped crystals, the degree of crystallinity x ∼ t2.

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.

Practical physics behind growing crystals of biological macromolecules.

PubMed

Candoni, Nadine; Grossier, Romain; Hammadi, Zoubida; Morin, Roger; Veesler, Stéphane

2012-07-01

The aim of this review is to provide biocrystallographers who intend to tackle protein-crystallization with theory and practical examples. Crystallization involves two separate processes, nucleation and growth, which are rarely completely unconnected. Here we give theoretical background and concrete examples illustrating protein crystallization. We describe the nucleation of a new phase, solid or liquid, and the growth and transformation of existing crystals obtained by primary or secondary nucleation or by seeding. Above all, we believe that a thorough knowledge of the phase diagram is vital to the selection of starting position and path for any crystallization experiment.

van der Waals epitaxy of SnS film on single crystal graphene buffer layer on amorphous SiO2/Si

NASA Astrophysics Data System (ADS)

Xiang, Yu; Yang, Yunbo; Guo, Fawen; Sun, Xin; Lu, Zonghuan; Mohanty, Dibyajyoti; Bhat, Ishwara; Washington, Morris; Lu, Toh-Ming; Wang, Gwo-Ching

2018-03-01

Conventional hetero-epitaxial films are typically grown on lattice and symmetry matched single crystal substrates. We demonstrated the epitaxial growth of orthorhombic SnS film (∼500 nm thick) on single crystal, monolayer graphene that was transferred on the amorphous SiO2/Si substrate. Using X-ray pole figure analysis we examined the structure, quality and epitaxy relationship of the SnS film grown on the single crystal graphene and compared it with the SnS film grown on commercial polycrystalline graphene. We showed that the SnS films grown on both single crystal and polycrystalline graphene have two sets of orientation domains. However, the crystallinity and grain size of the SnS film improve when grown on the single crystal graphene. Reflection high-energy electron diffraction measurements show that the near surface texture has more phases as compared with that of the entire film. The surface texture of a film will influence the growth and quality of film grown on top of it as well as the interface formed. Our result offers an alternative approach to grow a hetero-epitaxial film on an amorphous substrate through a single crystal graphene buffer layer. This strategy of growing high quality epitaxial thin film has potential applications in optoelectronics.

Drop deployment system for crystal growth apparatus

NASA Technical Reports Server (NTRS)

Rhodes, Percy H. (Inventor); Snyder, Robert S. (Inventor); Pusey, Marc L. (Inventor)

1992-01-01

This invention relates to a crystal growth apparatus (10) generally used for growing protein crystals wherein a vapor diffusion method is used for growing the crystals. In this apparatus, a precipitating solution and a solution containing dissolved crystalline material are stored in separate vials (12, 14), each having a resilient diaphragm (28) across one end and an opening (24) with a puncturable septum (26) thereacross at an opposite end. The vials are placed in receptacles (30) having a manifold (41) with a manifold diaphragm (42) in contact with the vial diaphragm at one end of the receptacle and a hollow needle (36) for puncturing the septum at the other end of the manifold. The needles of each vial communicate with a ball mixer (40) that mixes the precipitate and protein solutions and directs the mixed solution to a drop support (64) disposed in a crystal growth chamber (16), the drop support being a tube with an inner bevelled surface (66) that provides more support for the drop (68) than the tubes of the prior art. A sealable storage region (70) intermediate the drop support and mixer provides storage of the drop (68) and the grown crystals.

Growth of binary organic NLO crystals: m.NA-p.NA and m.NA-CNA system

NASA Technical Reports Server (NTRS)

Singh, N. B.; Henningsen, T.; Hopkins, R. H.; Mazelsky, R.

1993-01-01

Experiments were carried out to grow 3.Nitroaniline (m.NA) crystals doped with 4.Nitroaniline (p.NA) and 2.chloro 4.Nitroaniline (CNA). The measured undercooling for m.NA, p.NA, and CNA were 0.21 tm K, 0.23 tm K, and 0.35 tm K respectively, where tm represents the melting temperature of the pure component. Because of the crystals' large heat of fusion and large undercooling, it was not possible to grow good quality crystals with low thermal gradients. In the conventional two-zone Bridgman furnace we had to raise the temperature of the hot zone above the decomposition temperature of CNA, p.NA, and m.NA to achieve the desired thermal gradient. To avoid decomposition, we used an unconventional Bridgman furnace. Two immiscible liquids, silicone oil and ethylene glycol, were used to build a special two-zone Bridgman furnace. A temperature gradient of 18 K/cm was achieved without exceeding the decomposition temperature of the crystal. The binary crystals, m.NA-p.NA and m.NA-CNA, were grown in centimeter size in this furnace. X-ray and optical characterization showed good optical quality.

Gas Atmospheres Improve Silicon-Ribbon Quality

NASA Technical Reports Server (NTRS)

Wald, F. V.; Kalejs, J. P.

1985-01-01

Growing crystal surrounded by gas containing carbon or oxygen. Ribbon of solid silicon, edgewise, grows from pool of molten silicon in die. Gases flowing through orifice ensure longer diffusion length and less contaminiation by carbide particles in product.

ACTIVE MEDIA: BaY2F8 single crystals doped with rare-earth ions as promising up-conversion media for UV and VUV lasers

NASA Astrophysics Data System (ADS)

Pushkar', A. A.; Uvarova, T. V.; Molchanov, V. N.

2008-04-01

BaY2F8 crystals are studied as promising active media for UV and VUV lasers. The up-conversion pumping of rare-earth activators is proposed to solve problems related to the solarisation of the medium and the selection of pump sources. The technology of growing oriented BaY2F8 single crystals is developed and the influence of the crystal orientation on the growth rate and quality of single crystals is determined.

Chemical vapor deposition of high-quality large-sized MoS 2 crystals on silicon dioxide substrates

DOE PAGES

Chen, Jianyi; Tang, Wei; Tian, Bingbing; ...

2016-03-31

Large-sized MoS 2 crystals can be grown on SiO 2/Si substrates via a two-stage chemical vapor deposition method. The maximum size of MoS 2 crystals can be up to about 305 μm. The growth method can be used to grow other transition metal dichalcogenide crystals and lateral heterojunctions. Additionally, the electron mobility of the MoS 2 crystals can reach ≈30 cm 2 V –1 s –1, which is comparable to those of exfoliated flakes.

Chemical Vapor Deposition of High-Quality Large-Sized MoS2 Crystals on Silicon Dioxide Substrates.

PubMed

Chen, Jianyi; Tang, Wei; Tian, Bingbing; Liu, Bo; Zhao, Xiaoxu; Liu, Yanpeng; Ren, Tianhua; Liu, Wei; Geng, Dechao; Jeong, Hu Young; Shin, Hyeon Suk; Zhou, Wu; Loh, Kian Ping

2016-08-01

Large-sized MoS 2 crystals can be grown on SiO 2 /Si substrates via a two-stage chemical vapor deposition method. The maximum size of MoS 2 crystals can be up to about 305 μm. The growth method can be used to grow other transition metal dichalcogenide crystals and lateral heterojunctions. The electron mobility of the MoS 2 crystals can reach ≈30 cm 2 V -1 s -1 , which is comparable to those of exfoliated flakes.

Solution-grown organic single-crystalline p-n junctions with ambipolar charge transport.

PubMed

Fan, Congcheng; Zoombelt, Arjan P; Jiang, Hao; Fu, Weifei; Wu, Jiake; Yuan, Wentao; Wang, Yong; Li, Hanying; Chen, Hongzheng; Bao, Zhenan

2013-10-25

Organic single-crystalline p-n junctions are grown from mixed solutions. First, C60 crystals (n-type) form and, subsequently, C8-BTBT crystals (p-type) nucleate heterogeneously on the C60 crystals. Both crystals continue to grow simultaneously into single-crystalline p-n junctions that exhibit ambipolar charge transport characteristics. This work provides a platform to study organic single-crystalline p-n junctions. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Shape optimization of solid-air porous phononic crystal slabs with widest full 3D bandgap for in-plane acoustic waves

NASA Astrophysics Data System (ADS)

D'Alessandro, Luca; Bahr, Bichoy; Daniel, Luca; Weinstein, Dana; Ardito, Raffaele

2017-09-01

The use of Phononic Crystals (PnCs) as smart materials in structures and microstructures is growing due to their tunable dynamical properties and to the wide range of possible applications. PnCs are periodic structures that exhibit elastic wave scattering for a certain band of frequencies (called bandgap), depending on the geometric and material properties of the fundamental unit cell of the crystal. PnCs slabs can be represented by plane-extruded structures composed of a single material with periodic perforations. Such a configuration is very interesting, especially in Micro Electro-Mechanical Systems industry, due to the easy fabrication procedure. A lot of topologies can be found in the literature for PnCs with square-symmetric unit cell that exhibit complete 2D bandgaps; however, due to the application demand, it is desirable to find the best topologies in order to guarantee full bandgaps referred to in-plane wave propagation in the complete 3D structure. In this work, by means of a novel and fast implementation of the Bidirectional Evolutionary Structural Optimization technique, shape optimization is conducted on the hole shape obtaining several topologies, also with non-square-symmetric unit cell, endowed with complete 3D full bandgaps for in-plane waves. Model order reduction technique is adopted to reduce the computational time in the wave dispersion analysis. The 3D features of the PnC unit cell endowed with the widest full bandgap are then completely analyzed, paying attention to engineering design issues.

In Situ Determination of Thermal Profiles during Czochralski Silicon Crystal Growth by an Eddy Current Technique.

NASA Astrophysics Data System (ADS)

Choe, Kwang Su.

An eddy current testing method was developed to continuously monitor crystal growth process and determine thermal profiles in situ during Czochralski silicon crystal growth. The work was motivated by the need to improve the quality of the crystal by controlling thermal gradients and annealing history over the growth cycle. The experimental concept is to monitor intrinsic electrical conductivities of the growing crystal and deduce temperature values from them. The experiments were performed in a resistance-heated Czochralski puller with a 203 mm (8 inch) diameter crucible containing 6.5 kg melt. The silicon crystals being grown were about 80 mm in diameter and monitored by an encircling sensor operating at three different test frequencies (86, 53 and 19 kHz). A one-dimensional analytical solution was employed to translate the detected signals into electrical conductivities. In terms of experiments, the effects of changes in growth condition, which is defined by crystal and crucible rotation rates, crucible position, pull rate, and hot-zone configuration, were investigated. Under a given steady-state condition, the thermal profile was usually stable over the entire length of crystal growth. The profile shifted significantly, however, when the crucible rotation rate was kept too high. As a direct evidence to the effects of melt flow on heat transfer process, a thermal gradient minimum was observed about the crystal/crucible rotation combination of 20/-10 rpm cw. The thermal gradient reduction was still most pronounced when the pull rate or the radiant heat loss to the environment was decreased: a nearly flat axial thermal gradient was achieved when either the pull rate was halved or the height of the exposed crucible wall was effectively doubled. Under these conditions, the average axial thermal gradient along the surface of the crystal was about 4-5 ^{rm o}C/mm. Regardless of growth condition, the three-frequency data revealed radial thermal gradients much larger than what were predicted by existing theoretical models. This discrepancy seems to indicate that optical effects, which are neglected in theoretical modeling, play a major role in the internal heat transfer of the crystal.

Evolutionary selection growth of two-dimensional materials on polycrystalline substrates

DOE PAGES

Vlassiouk, Ivan V.; Stehle, Yijing; Pudasaini, Pushpa Raj; ...

2018-03-12

There is a demand for the manufacture of two-dimensional (2D) materials with high-quality single crystals of large size. Usually, epitaxial growth is considered the method of choice in preparing single-crystalline thin films, but it requires single-crystal substrates for deposition. Here in this paper we present a different approach and report the synthesis of single-crystal-like monolayer graphene films on polycrystalline substrates. The technological realization of the proposed method resembles the Czochralski process and is based on the evolutionary selection approach, which is now realized in 2D geometry. The method relies on ‘self-selection’ of the fastest-growing domain orientation, which eventually overwhelms themore » slower-growing domains and yields a single-crystal continuous 2D film. Here we have used it to synthesize foot-long graphene films at rates up to 2.5 cm h -1 that possess the quality of a single crystal. We anticipate that the proposed approach could be readily adopted for the synthesis of other 2D materials and heterostructures.« less

Solid Xenon Project

NASA Astrophysics Data System (ADS)

Balakishiyeva, Durdana N.; Mahapatra, Rupak; Saab, Tarek; Yoo, Jonghee

2010-08-01

Crystals like Germanium and Silicon need to be grown in specialized facilities which is time and money costly. It takes many runs to test the detector once it's manufactured and mishaps are very probable. It is of a great challenge to grow big germanium crystals and that's why stacking them up in a tower is the only way at the moment to increase testing mass. Liquid Noble gas experiments experiencing contamination problems, their predicted energy resolution at 10 keV and lower energy range is not as good as predicted. Every experiment is targeting one specific purpose, looking for one thing. Why not to design an experiment that is diverse and build a detector that can search for Dark Matter, Solar Axions, Neutrinoless Double Beta decay, etc. Solid Xenon detector is such detector. We designed a simple Xenon crystal growing chamber that was put together at Fermi National Accelerator Laboratory. The first phase of this experiment was to demonstrate that a good, crack free Xenon crystal can be grown (regardless of many failed attempts by various groups) and our first goal, 1 kg crystal, was successful.

Influence of convection on free growth of dendrite crystals from solution

NASA Technical Reports Server (NTRS)

Hallett, J.; Wedum, E.

1979-01-01

The free growth of dendrites in a uniformly supercooled solution was examined using cine photography with a Schlieren optical system. Crystals were grown in the bulk of the solution from a centrally located capillary tube, nucleated at the interface with a liquid nitrogen cooled wire. Crystals propagated along the tube, the slower growing orientations eliminated, and emerged at the tip, usually growing parallel to the tube direction. For both sodium sulfate decahydrate from its solution and ice from sodium chloride solution, growth rate and fineness of dendrites increased with supercooling. In sodium sulfate, upward convection of the less dense depleted solution occurs; downward convection was observed for the rejected, more concentrated sodium chloride solution. In both cases, there was a spatial and temporal delay in the release of the convective plume from the moving dendrite tip. The role of this convection on the growth characteristics and the production of secondary crystals is examined. A proposed low-g experiment to examine differences in growth rate, crystal texture, and secondary nucleation in a reduced convective regime where molecular diffusion is the dominant transfer process is discussed.

Evolutionary selection growth of two-dimensional materials on polycrystalline substrates

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

Vlassiouk, Ivan V.; Stehle, Yijing; Pudasaini, Pushpa Raj

There is a demand for the manufacture of two-dimensional (2D) materials with high-quality single crystals of large size. Usually, epitaxial growth is considered the method of choice in preparing single-crystalline thin films, but it requires single-crystal substrates for deposition. Here in this paper we present a different approach and report the synthesis of single-crystal-like monolayer graphene films on polycrystalline substrates. The technological realization of the proposed method resembles the Czochralski process and is based on the evolutionary selection approach, which is now realized in 2D geometry. The method relies on ‘self-selection’ of the fastest-growing domain orientation, which eventually overwhelms themore » slower-growing domains and yields a single-crystal continuous 2D film. Here we have used it to synthesize foot-long graphene films at rates up to 2.5 cm h -1 that possess the quality of a single crystal. We anticipate that the proposed approach could be readily adopted for the synthesis of other 2D materials and heterostructures.« less

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.

Steady distribution structure of point defects near crystal-melt interface under pulling stop of CZ Si crystal

NASA Astrophysics Data System (ADS)

Abe, T.; Takahashi, T.; Shirai, K.

2017-02-01

In order to reveal a steady distribution structure of point defects of no growing Si on the solid-liquid interface, the crystals were grown at a high pulling rate, which Vs becomes predominant, and the pulling was suddenly stopped. After restoring the variations of the crystal by the pulling-stop, the crystals were then left in prolonged contact with the melt. Finally, the crystals were detached and rapidly cooled to freeze point defects and then a distribution of the point defects of the as-grown crystals was observed. As a result, a dislocation loop (DL) region, which is formed by the aggregation of interstitials (Is), was formed over the solid-liquid interface and was surrounded with a Vs-and-Is-free recombination region (Rc-region), although the entire crystals had been Vs rich in the beginning. It was also revealed that the crystal on the solid-liquid interface after the prolonged contact with the melt can partially have a Rc-region to be directly in contact with the melt, unlike a defect distribution of a solid-liquid interface that has been growing. This experimental result contradicts a hypothesis of Voronkov's diffusion model, which always assumes the equilibrium concentrations of Vs and Is as the boundary condition for distribution of point defects on the growth interface. The results were disscussed from a qualitative point of view of temperature distribution and thermal stress by the pulling-stop.

Interface and facet control during Czochralski growth of (111) InSb crystals for cost reduction and yield improvement of IR focal plane array substrates

NASA Astrophysics Data System (ADS)

Gray, Nathan W.; Perez-Rubio, Victor; Bolke, Joseph G.; Alexander, W. B.

2014-10-01

Focal plane arrays (FPAs) made on InSb wafers are the key cost-driving component in IR imaging systems. The electronic and crystallographic properties of the wafer directly determine the imaging device performance. The "facet effect" describes the non-uniform electronic properties of crystals resulting from anisotropic dopant segregation during bulk growth. When the segregation coefficient of dopant impurities changes notably across the melt/solid interface of a growing crystal the result is non-uniform electronic properties across wafers made from these crystals. The effect is more pronounced in InSb crystals grown on the (111) axis compared with other orientations and crystal systems. FPA devices made on these wafers suffer costly yield hits due to inconsistent device response and performance. Historically, InSb crystal growers have grown approximately 9-19 degree off-axis from the (111) to avoid the facet effect and produced wafers with improved uniformity of electronic properties. It has been shown by researchers in the 1960s that control of the facet effect can produce uniform small diameter crystals. In this paper, we share results employing a process that controls the facet effect when growing large diameter crystals from which 4, 5, and 6" wafers can be manufactured. The process change resulted in an increase in wafers yielded per crystal by several times, all with high crystal quality and uniform electronic properties. Since the crystals are grown on the (111) axis, manufacturing (111) oriented wafers is straightforward with standard semiconductor equipment and processes common to the high-volume silicon wafer industry. These benefits result in significant manufacturing cost savings and increased value to our customers.

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.

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.

Crystallography of metal–organic frameworks

PubMed Central

Gándara, Felipe; Bennett, Thomas D.

2014-01-01

Metal–organic frameworks (MOFs) are one of the most intensely studied material types in recent times. Their networks, resulting from the formation of strong bonds between inorganic and organic building units, offer unparalled chemical diversity and pore environments of growing complexity. Therefore, advances in single-crystal X-ray diffraction equipment and techniques are required to characterize materials with increasingly larger surface areas, and more complex linkers. In addition, whilst structure solution from powder diffraction data is possible, the area is much less populated and we detail the current efforts going on here. We also review the growing number of reports on diffraction under non-ambient conditions, including the response of MOF structures to very high pressures. Such experiments are important due to the expected presence of stresses in proposed applications of MOFs – evidence suggesting rich and complex behaviour. Given the entwined and inseparable nature of their structure, properties and applications, it is essential that the field of structural elucidation is able to continue growing and advancing, so as not to provide a rate-limiting step on characterization of their properties and incorporation into devices and applications. This review has been prepared with this in mind. PMID:25485136

Meniscus Imaging for Crystal-Growth Control

NASA Technical Reports Server (NTRS)

Sachs, E. M.

1983-01-01

Silicon crystal growth monitored by new video system reduces operator stress and improves conditions for observation and control of growing process. System optics produce greater magnification vertically than horizontally, so entire meniscus and melt is viewed with high resolution in both width and height dimensions.

Modeling Calculation and Synthesis of Alumina Whiskers Based on the Vapor Deposition Process.

PubMed

Gong, Wei; Li, Xiangcheng; Zhu, Boquan

2017-10-17

This study simulated the bulk structure and surface energy of Al₂O₃ based on the density of states (DOS) and studied the synthesis and microstructure of one-dimensional Al₂O₃ whiskers. The simulation results indicate that the (001) surface has a higher surface energy than the others. The growth mechanism of Al₂O₃ whiskers follows vapor-solid (VS) growth. For the (001) surface with the higher surface energy, the driving force of crystal growth would be more intense in the (001) plane, and the alumina crystal would tend to grow preferentially along the direction of the (001) plane from the tip of the crystal. The Al₂O₃ grows to the shape of whisker with [001] orientation, which is proved both through modeling and experimentation.

Laminar mixing in a small floating zone

NASA Technical Reports Server (NTRS)

Harriott, George M.

1987-01-01

The relationship between the flow and solute fields during steady mass transfer of a dilute component is analyzed for multi-cellular rotating flows in the floating zone process of semiconductor growth. When the recirculating flows are weak in relation to the rate of crystal growth, a closed-form solution clearly shows the link between the convection pattern in the melt and the solute distribution across the surface of the growing solid. In the limit of strong convection, finite element calculations demonstrate the tendency of the composition to become uniform over the majority of the melt. The solute segregation in the product crystal is greatest when the recirculating motion is comparable to the rate of crystal growth, and points to the danger in attempting to grow compositionally uniform materials from a nearly convectionless melt.

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.

Drop deployment system for crystal growth apparatus

NASA Technical Reports Server (NTRS)

Rhodes, Percy (Inventor); Snyder, Robert S. (Inventor); Pusey, Marc L. (Inventor)

1990-01-01

A crystal growth apparatus is presented. It utilizes a vapor diffusion method for growing protein crystals, and particularly such an apparatus wherein a ball mixer is used to mix the fluids that form a drop within which crystals are grown. Particular novelty of this invention lies in utilizing a ball mixer to completely mix the precipitate and protein solutions prior to forming the drop. Additional novelty lies in details of construction of the vials, the fluid deployment system, and the fluid storage system of the preferred embodiment.

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.

Growth and characterization of pure and Cadmium chloride doped KDP Crystals grown by gel medium

NASA Astrophysics Data System (ADS)

Kalaivani, M. S.; Asaithambi, T.

2016-10-01

Crystal growth technology provides an important basis for many industrial branches. Crystals are the unrecognized pillars of modern technology. Without crystals, there is no electronic industry, no photonic industry, and no fiber optic communications. Single crystals play a major role and form the strongest base for the fast growing field of engineering, science and technology. Crystal growth is an interdisciplinary subject covering physics, chemistry, material science, chemical engineering, metallurgy, crystallography, mineralogy, etc. In past few decades, there has been a keen interest on crystal growth processes, particularly in view of the increasing demand of materials for technological applications. Optically good quality pure and metal doped KDP crystals have been grown by gel method at room temperature and their characterization have been studied. Gel method is a much uncomplicated method and can be utilized to synthesize crystals which are having low solubility. Potassium dihydrogen orthophosphate KH2PO4 (KDP) continues to be an interesting material both academically and industrially. KDP is a representative of hydrogen bonded materials which possess very good electro - optic and nonlinear optical properties in addition to interesting electrical properties. Due to this interesting properties, we made an attempt to grow pure and cadmium chloride doped KDP crystals in various concentrations (0.002, 0.004, 0.006, 0.008 and 0.010) using gel method. The grown crystals were collected after 20 days. We get crystals with good quality and shaped. The dc electrical conductivity (resistance, capacitance and dielectric constant) values were measured at frequencies in the range of 1 KHZ and 100 HZ of pure and cadmium chloride added crystal with a temperature range of 400C to 1300C using simple two probe setup with Q band digital LCR meter present in our lab. The electrical conductivity increases with increase of temperature. The dielectric constants of metal doped KDP crystals were slightly decreased compared to pure KDP crystals.

Growth of zeolite crystals in the microgravity environment of space

NASA Technical Reports Server (NTRS)

Sacco, A., Jr.; Sand, L. B.; Collette, D.; Dieselman, K.; Crowley, J.; Feitelberg, A.

1986-01-01

Zeolites are hydrated, crystalline aluminosilicates with alkali and alkaling earth metals substituted into cation vacancies. Typically zeolite crystals are 3 to 8 microns. Larger cyrstals are desirable. Large zeolite crystals were produced (100 to 200 microns); however, they have taken restrictively long times to grow. It was proposed if the rate of nucleation or in some other way the number of nuclei can be lowered, fewer, larger crystals will be formed. The microgravity environment of space may provide an ideal condition to achieve rapid growth of large zeolite crystals. The objective of the project is to establish if large zeolite crystals can be formed rapidly in space.

100-Fold Enhancement of Charge Transport in Uniaxially Oriented Mesoporous Anatase TiO 2 Films

DOE PAGES

Li, Ke; Liu, Jie; Sheng, Xia; ...

2017-12-04

Mesoporous semiconductor films are of considerable interest for applications in photoelectrochemical devices, however, despite intensive research till now, their charge transport properties remain significantly lower than their single-crystal counterparts. Herein, we report a novel low-temperature template-free technique for growing high surface area mesoporous anatase TiO2 films with a preferred [001] crystalline-orientation on FTO-coated glass substrate. Compared to mesoporous films that comprised of randomly oriented crystallites, the uniaxial orientation enables a 100-fold increase in the rate of electron transport. The uniaxially oriented mesoporous anatase TiO2 films exhibit should greatly facilitate the development and application of photoelectrochemical and electrochemical devices.

Comparative analysis of quantitative methodologies for Vibrionaceae biofilms.

PubMed

Chavez-Dozal, Alba A; Nourabadi, Neda; Erken, Martina; McDougald, Diane; Nishiguchi, Michele K

2016-11-01

Multiple symbiotic and free-living Vibrio spp. grow as a form of microbial community known as a biofilm. In the laboratory, methods to quantify Vibrio biofilm mass include crystal violet staining, direct colony-forming unit (CFU) counting, dry biofilm cell mass measurement, and observation of development of wrinkled colonies. Another approach for bacterial biofilms also involves the use of tetrazolium (XTT) assays (used widely in studies of fungi) that are an appropriate measure of metabolic activity and vitality of cells within the biofilm matrix. This study systematically tested five techniques, among which the XTT assay and wrinkled colony measurement provided the most reproducible, accurate, and efficient methods for the quantitative estimation of Vibrionaceae biofilms.

A Robust and Engineerable Self-Assembling Protein Template for the Synthesis and Patterning of Ordered Nanoparticle Arrays

NASA Technical Reports Server (NTRS)

McMillan, R. Andrew; Howard, Jeanie; Zaluzec, Nestor J.; Kagawa, Hiromi K.; Li, Yi-Fen; Paavola, Chad D.; Trent, Jonathan D.

2004-01-01

Self-assembling biomolecules that form highly ordered structures have attracted interest as potential alternatives to conventional lithographic processes for patterning materials. Here we introduce a general technique for patterning materials on the nanoscale using genetically modified protein cage structures called chaperonins that self-assemble into crystalline templates. Constrained chemical synthesis of transition metal nanoparticles is specific to templates genetically functionalized with poly-Histidine sequences. These arrays of materials are ordered by the nanoscale structure of the crystallized protein. This system may be easily adapted to pattern a variety of materials given the rapidly growing list of peptide sequences selected by screening for specificity for inorganic materials.

Medium-range structure and glass forming ability in Zr–Cu–Al bulk metallic glasses

DOE PAGES

Zhang, Pei; Maldonis, Jason J.; Besser, M. F.; ...

2016-03-05

Fluctuation electron microscopy experiments combined with hybrid reverse Monte Carlo modeling show a correlation between medium-range structure at the nanometer scale and glass forming ability in two Zr–Cu–Al bulk metallic glass (BMG) alloys. Both Zr 50Cu 35Al 15 and Zr 50Cu 45Al 5 exhibit two nanoscale structure types, one icosahedral and the other more crystal-like. In Zr 50Cu 35Al 15, the poorer glass former, the crystal-like structure is more stable under annealing below the glass transition temperature, T g, than in Zr 50Cu 45Al 5. Variable resolution fluctuation microscopy of the MRO clusters show that in Zr 50Cu 35Al 15more » on sub-Tg annealing, the crystal-like clusters shrink even as they grow more ordered, while icosahedral-like clusters grow. Furthermore, the results suggest that achieving better glass forming ability in this alloy system may depend more on destabilizing crystal-like structures than enhancing non-crystalline structures.« less

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

Zhang, Pei; Maldonis, Jason J.; Besser, M. F.

Fluctuation electron microscopy experiments combined with hybrid reverse Monte Carlo modeling show a correlation between medium-range structure at the nanometer scale and glass forming ability in two Zr–Cu–Al bulk metallic glass (BMG) alloys. Both Zr 50Cu 35Al 15 and Zr 50Cu 45Al 5 exhibit two nanoscale structure types, one icosahedral and the other more crystal-like. In Zr 50Cu 35Al 15, the poorer glass former, the crystal-like structure is more stable under annealing below the glass transition temperature, T g, than in Zr 50Cu 45Al 5. Variable resolution fluctuation microscopy of the MRO clusters show that in Zr 50Cu 35Al 15more » on sub-Tg annealing, the crystal-like clusters shrink even as they grow more ordered, while icosahedral-like clusters grow. Furthermore, the results suggest that achieving better glass forming ability in this alloy system may depend more on destabilizing crystal-like structures than enhancing non-crystalline structures.« less

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.

Synthesis, crystal growth and characterization of a phase matchable nonlinear optical single crystal: p-chloro dibenzylideneacetone

NASA Astrophysics Data System (ADS)

Ravindra, H. J.; John Kiran, A.; Nooji, Satheesha Rai; Dharmaprakash, S. M.; Chandrasekharan, K.; Kalluraya, Balakrishna; Rotermund, Fabian

2008-05-01

Good quality single crystals of p-chloro dibenzylideneacetone (CDBA) of size 13 mm×8 mm×2 mm were grown by slow evaporation solution growth technique. The grown crystals were confirmed by elemental analysis, Fourier transform infrared (FTIR) analysis and single crystal X-ray diffraction techniques. From the thermo gravimetric/differential thermal (TG/DT) analysis, the CDBA was found to be thermally stable up to 250 °C. The mechanical stability of the crystal is comparable with that of the other reported chalcones. The lower optical cut-off wavelength for this crystal was observed at 440 nm. The laser damage threshold of the crystal was 0.6 GW/cm 2 at 532 nm. The second harmonic generation conversion efficiency of the powder sample of CDBA was found to be 4.5 times greater than that of urea. We also demonstrate the existence of the phase matching property in this crystal using Kurtz powder technique.

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).

Phase boundaries, nucleation rates and speed of crystal growth of the water-to-ice transition under an electric field: a simulation study

NASA Astrophysics Data System (ADS)

Zaragoza, Alberto; Espinosa, Jorge R.; Ramos, Regina; Cobos, José Antonio; Aragones, Juan Luis; Vega, Carlos; Sanz, Eduardo; Ramírez, Jorge; Valeriani, Chantal

2018-05-01

We investigate with computer simulations the effect of applying an electric field on the water-to-ice transition. We use a combination of state-of-the-art simulation techniques to obtain phase boundaries and crystal growth rates (direct coexistence), nucleation rates (seeding) and interfacial free energies (seeding and mold integration). First, we consider ice Ih, the most stable polymorph in the absence of a field. Its normal melting temperature, speed of crystal growth and nucleation rate (for a given supercooling) diminish as the intensity of the field goes up. Then, we study polarised cubic ice, or ice Icf, the most stable solid phase under a strong electric field. Its normal melting point goes up with the field and, for a given supercooling, under the studied field (0.3 V nm‑1) ice Icf nucleates and grows at a similar rate as Ih with no field. The net effect of the field would then be that ice nucleates at warmer temperatures, but in the form of ice Icf. The main conclusion of this work is that reasonable electric fields (not strong enough to break water molecules apart) are not relevant in the context of homogeneous ice nucleation at 1 bar.

Phase boundaries, nucleation rates and speed of crystal growth of the water-to-ice transition under an electric field: a simulation study.

PubMed

Zaragoza, Alberto; Espinosa, Jorge R; Ramos, Regina; Antonio Cobos, José; Luis Aragones, Juan; Vega, Carlos; Sanz, Eduardo; Ramírez, Jorge; Valeriani, Chantal

2018-05-02

We investigate with computer simulations the effect of applying an electric field on the water-to-ice transition. We use a combination of state-of-the-art simulation techniques to obtain phase boundaries and crystal growth rates (direct coexistence), nucleation rates (seeding) and interfacial free energies (seeding and mold integration). First, we consider ice Ih, the most stable polymorph in the absence of a field. Its normal melting temperature, speed of crystal growth and nucleation rate (for a given supercooling) diminish as the intensity of the field goes up. Then, we study polarised cubic ice, or ice Icf, the most stable solid phase under a strong electric field. Its normal melting point goes up with the field and, for a given supercooling, under the studied field (0.3 V nm -1 ) ice Icf nucleates and grows at a similar rate as Ih with no field. The net effect of the field would then be that ice nucleates at warmer temperatures, but in the form of ice Icf. The main conclusion of this work is that reasonable electric fields (not strong enough to break water molecules apart) are not relevant in the context of homogeneous ice nucleation at 1 bar.

A microcrystal selection technique in protein crystallization

NASA Astrophysics Data System (ADS)

Han, Qing; Lin, Sheng-Xiang

1996-10-01

The goal of protein crystallization is to obtain high quality single crystals for X-ray diffraction analysis. A new and easy technique was employed to control the number and quality of crystals by eliminating poor microcrystals after the spontaneous nucleation. The process was carried out with two samples: human 17β-hydroxysteroid dehydrogenase (17β-HSD) and hen egg white lysozyme. The present study suggests a useful method for the successful crystal growth of biomacromolecules.

Using in situ synchrotron radiation wide angle X-ray scattering (WAXS) to study CaCO3 scale formation at ambient and elevated temperature.

PubMed

Chen, Tao; Neville, Anne; Sorbie, Ken; Zhong, Zhong

2007-01-01

The formation of calcium carbonate mineral scale is a persistent and expensive problem in oil and gas production, water piping systems, power generator, and batch precipitation. The aim of this paper is to further the understanding of scale formation and inhibition by in situ probing of crystal growth by synchrotron radiation wide angle X-ray scattering (WAXS) at ambient and elevated temperature. This novel technique enables in situ study of mineral scale formation and inhibition and as such, information on the nucleation and growth processes are accessible. This technique studies bulk precipitation and surface deposition in the same system and will be of great benefit to the understanding of an industrial scaling system. It offers an exciting prospect for the study of scaling. It has been shown that the nucleation and growth of various calcareous polymorphs and their individual crystal planes can be followed in real-time and from this the following conclusions are reached. The process of scale deposition on the surface can be divided into an unstable phase and a stable phase. The initial phase of crystallization of calcium carbonate is characterized by instability with individual planes from various vaterite and aragonite polymorphs emerging and subsequently disappearing under the hydrodynamic conditions. After the initial unstable phase, various calcium carbonate crystal planes adhere on the surface and then grow on the surface. At 25 degrees C, the main plane of surface deposit is calcite and a strong (104) peak is detected. The other calcite planes (102), (006), (110) (113) and (202) are hardly detectable under this condition. At 80 degrees C, the main planes in the surface deposit are the (104), (113) and (110) planes of calcite. Stable planes of vaterite and aragonite are also observed. This paper will discuss how surface scale evolves--exploring the power of the synchrotron in situ methodology.

In-plane x-ray diffraction for characterization of monolayer and few-layer transition metal dichalcogenide films

NASA Astrophysics Data System (ADS)

Chubarov, Mikhail; Choudhury, Tanushree H.; Zhang, Xiaotian; Redwing, Joan M.

2018-02-01

There is significant interest in the growth of single crystal monolayer and few-layer films of transition metal dichalcogenides (TMD) and other 2D materials for scientific exploration and potential applications in optics, electronics, sensing, catalysis and others. The characterization of these materials is crucial in determining the properties and hence the applications. The ultra-thin nature of 2D layers presents a challenge to the use of x-ray diffraction (XRD) analysis with conventional Bragg-Brentano geometry in analyzing the crystallinity and epitaxial orientation of 2D films. To circumvent this problem, we demonstrate the use of in-plane XRD employing lab scale equipment which uses a standard Cu x-ray tube for the analysis of the crystallinity of TMD monolayer and few-layer films. The applicability of this technique is demonstrated in several examples for WSe2 and WS2 films grown by chemical vapor deposition on single crystal substrates. In-plane XRD was used to determine the epitaxial relation of WSe2 grown on c-plane sapphire and on SiC with an epitaxial graphene interlayer. The evolution of the crystal structure orientation of WS2 films on sapphire as a function of growth temperature was also examined. Finally, the epitaxial relation of a WS2/WSe2 vertical heterostructure deposited on sapphire substrate was determined. We observed that WSe2 grows epitaxially on both substrates employed in this work under all conditions studied while WS2 exhibits various preferred orientations on sapphire substrate which are temperature dependent. In contrast to the sapphire substrate, WS2 deposited on WSe2 exhibits only one preferred orientation which may provide a route to better control the orientation and crystal quality of WS2. In the case of epitaxial graphene on SiC, no graphene-related peaks were observed in in-plane XRD while its presence was confirmed using Raman spectroscopy. This demonstrates the limitation of the in-plane XRD technique for characterizing low electron density materials.

Synthesis, crystal growth, optical, thermal, and mechanical properties of a nonlinear optical single crystal: ammonium sulfate hydrogen sulphamate (ASHS)

NASA Astrophysics Data System (ADS)

Sudhakar, K.; Nandhini, S.; Muniyappan, S.; Arumanayagam, T.; Vivek, P.; Murugakoothan, P.

2018-04-01

Ammonium sulfate hydrogen sulphamate (ASHS), an inorganic nonlinear optical crystal, was grown from the aqueous solution by slow evaporation solution growth technique. The single-crystal XRD confirms that the grown single crystal belongs to the orthorhombic system with the space group of Pna21. Powder XRD confirms the crystalline nature and the diffraction planes were indexed. Crystalline perfection of grown crystal was analysed by high-resolution X-ray diffraction rocking curve technique. UV-Vis-NIR studies revealed that ASHS crystal has optical transparency 65% and lower cut-off wavelength at 218 nm. The violet light emission of the crystal was identified by photoluminescence studies. The particle size-dependent second-harmonic generation efficiency for ASHS crystal was evaluated by Kurtz-Perry powder technique using Nd:YAG laser which established the existence of phase matching. Surface laser damage threshold value was evaluated using Nd:YAG laser. Optical homogeneity of the crystal was evaluated using modified channel spectrum method through birefringence study. Thermal analysis reveals that ASHS crystal is stable up to 213 °C. The mechanical behaviour of the ASHS crystal was analysed using Vickers microhardness study.

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.

Microgravity

NASA Image and Video Library

1986-06-03

Crystals grown in the hand-held Protein Crystallization Apparatus for Microgravity (PCAM) onboard STS-61C. The PCAM has a pedestal in the center of a circular chamber, the surrounding chamber holds an absorbent reservoir that contains a solution of the precipitant. Vapor pressure differences between the protein solution and the reservoir solution force water to move from the protein solution to the reservoir. As protein concentrations increase, protein crystals begin to nucleate and grow.

Growth of mercuric iodide single crystals from dimethylsulfoxide

DOEpatents

Carlston, Richard C.

1976-07-13

Dimethylsulfoxide is used as a solvent for the growth of red mercuric iodide (HgI.sub.2) crystals for use in radiation detectors. The hygroscopic property of the solvent allows controlled amounts of water to enter into the solvent phase and diminish the large solubility of HgI.sub.2 so that the precipitating solid collects as well-defined euhedral crystals which grow into a volume of several cc.

Cryo-TEM of morphology and kinetics of self-assembled nanostructures

NASA Astrophysics Data System (ADS)

Dong, Jingshan

Cryogenic Transmission Electron Microscopy (Cryo-TEM) is applied to study various structures in solutions and suspensions from micron to nanometer scale. By vitrifying the liquid samples at different moments, sequential stages of a dynamic process can be frozen and the structures occurring from about 30 sec to over 10 min can be imaged. Therefore a picture of how the structures evolve with time in the liquid systems can be established. This method has been proven to be a powerful technique in studying the morphology and kinetics of self-assembled nanostructures. Such a pseudo-in-situ technique is used to "watch" the crystallization process of silver stearate (AgSt) from sodium stearate (NaSt) dispersions. AgSt crystal is produced from a reaction of NaSt and silver nitrate. The reaction, as a AgSt crystallization process, starts from AgSt micelles, which aggregate and grow into hexagonal shaped crystals of about 10 microns. If silver bromide (AgBr) grains are present, the micelles do not prefer to aggregate, but rather deposit on the surface of the AgBr crystalline grains. Variation of the carboxylate chain length does not affect the crystallization process very much, although the morphology of both the reactant and the product is changed. Nanostructure transition in sodium lauryl ether sulfate (SLES) solutions is investigated as well. A micellar network structure can form if equal molar calcium chloride is added to 3 wt% SLES solution. The network can be broken into wormlike micelle segments such as spheres and rods by sonication. After about 10 min, these broken pieces can reassemble and reform the network through wormlike micelle growth and connection. Also by using Cryo-TEM, 100-200 nm casein micelles are observed at 1 wt% casein solution, but aggregated submicelles cannot be distinguished. However, individual submicelles of about 30 nm are indeed captured in a 0.03 wt% solution. By adding acid or EDTA, the casein micelles can be disrupted into small particles, the size of which is close to the estimated radius of gyration of single casein molecules.

Grow Your Own Copper Deposit

ERIC Educational Resources Information Center

Corcoran, Timothy John

2009-01-01

Crystals are beautiful structures--yet they occur naturally in dirty and remote places. In the inquiry-based activity described here, students will enjoy the process of creating their own crystals and using microscopes to examine them. It demonstrates the process of mineral concentration and deposition. Upon completing this activity, students…

Improved spatial resolution in PET scanners using sampling techniques

PubMed Central

Surti, Suleman; Scheuermann, Ryan; Werner, Matthew E.; Karp, Joel S.

2009-01-01

Increased focus towards improved detector spatial resolution in PET has led to the use of smaller crystals in some form of light sharing detector design. In this work we evaluate two sampling techniques that can be applied during calibrations for pixelated detector designs in order to improve the reconstructed spatial resolution. The inter-crystal positioning technique utilizes sub-sampling in the crystal flood map to better sample the Compton scatter events in the detector. The Compton scatter rejection technique, on the other hand, rejects those events that are located further from individual crystal centers in the flood map. We performed Monte Carlo simulations followed by measurements on two whole-body scanners for point source data. The simulations and measurements were performed for scanners using scintillators with Zeff ranging from 46.9 to 63 for LaBr3 and LYSO, respectively. Our results show that near the center of the scanner, inter-crystal positioning technique leads to a gain of about 0.5-mm in reconstructed spatial resolution (FWHM) for both scanner designs. In a small animal LYSO scanner the resolution improves from 1.9-mm to 1.6-mm with the inter-crystal technique. The Compton scatter rejection technique shows higher gains in spatial resolution but at the cost of reduction in scanner sensitivity. The inter-crystal positioning technique represents a modest acquisition software modification for an improvement in spatial resolution, but at a cost of potentially longer data correction and reconstruction times. The Compton scatter rejection technique, while also requiring a modest acquisition software change with no increased data correction and reconstruction times, will be useful in applications where the scanner sensitivity is very high and larger improvements in spatial resolution are desirable. PMID:19779586

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.

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.

Ion channeling study of defects in compound crystals using Monte Carlo simulations

NASA Astrophysics Data System (ADS)

Turos, A.; Jozwik, P.; Nowicki, L.; Sathish, N.

2014-08-01

Ion channeling is a well-established technique for determination of structural properties of crystalline materials. Defect depth profiles have been usually determined basing on the two-beam model developed by Bøgh (1968) [1]. As long as the main research interest was focused on single element crystals it was considered as sufficiently accurate. New challenge emerged with growing technological importance of compound single crystals and epitaxial heterostructures. Overlap of partial spectra due to different sublattices and formation of complicated defect structures makes the two beam method hardly applicable. The solution is provided by Monte Carlo computer simulations. Our paper reviews principal aspects of this approach and the recent developments in the McChasy simulation code. The latter made it possible to distinguish between randomly displaced atoms (RDA) and extended defects (dislocations, loops, etc.). Hence, complex defect structures can be characterized by the relative content of these two components. The next refinement of the code consists of detailed parameterization of dislocations and dislocation loops. Defect profiles for variety of compound crystals (GaN, ZnO, SrTiO3) have been measured and evaluated using the McChasy code. Damage accumulation curves for RDA and extended defects revealed non monotonous defect buildup with some characteristic steps. Transition to each stage is governed by the different driving force. As shown by the complementary high resolution XRD measurements lattice strain plays here the crucial role and can be correlated with the concentration of extended defects.

Decrystallization of Crystals Using Gold “Nano-Bullets” and the Metal-Assisted and Microwave-Accelerated Decrystallization Technique

PubMed Central

Thompson, Nishone; Boone-Kukoyi, Zainab; Shortt, Raquel; Lansiquot, Carisse; Kioko, Bridgit; Bonyi, Enock; Toker, Salih; Ozturk, Birol; Aslan, Kadir

2017-01-01

Gout is caused by the overproduction of uric acid and the inefficient metabolism of dietary purines in humans. Current treatments of gout, which include anti-inflammatory drugs, cyclooxygenase-2 inhibitors, and systemic glucocorticoids, have harmful side-effects. Our research laboratory has recently introduced an innovative approach for the decrystallization of biological and chemical crystals using the Metal-Assisted and Microwave-Accelerated Evaporative Decrystallization (MAMAD) technique. In the MAMAD technique, microwave energy is used to heat and activate gold nanoparticles that behave as “nano-bullets” to rapidly disrupt the crystal structure of biological crystals placed on planar surfaces. In this study, crystals of various sizes and compositions were studied as models for tophaceous gout at different stages (i.e., uric acid as small crystals (~10–100 μm) and L-alanine as medium (~300 μm) and large crystals (~4400 μm). Our results showed that the use of the MAMAD technique resulted in the reduction of the size and number of uric acid and L-alanine crystals up to >40% when exposed to intermittent microwave heating (up to 20 W power at 8 GHz) in the presence of 20 nm gold nanoparticles up to 120 s. This study demonstrates that the MAMAD technique can be potentially used as an alternative therapeutic method for the treatment of gout by effective decrystallization of large crystals, similar in size to those that often occur in gout. PMID:27763557

Growth and microtopographic study of CuInSe{sub 2} single crystals

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

Chauhan, Sanjaysinh M.; Chaki, Sunil, E-mail: sunilchaki@yahoo.co.in; Deshpande, M. P.

2016-05-23

The CuInSe{sub 2} single crystals were grown by chemical vapour transport (CVT) technique using iodine as transporting agent. The elemental composition of the as-grown CuInSe{sub 2} single crystals was determined by energy dispersive analysis of X-ray (EDAX). The unit cell crystal structure and lattice parameters were determined by X-ray diffraction (XRD) technique. The surface microtopographic study of the as-grown CuInSe{sub 2} single crystals surfaces were done to study the defects, growth mechanism, etc. of the CVT grown crystals.

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.

The Crystallization of Canavalin as a Function of pH and NaCl Concentration

NASA Technical Reports Server (NTRS)

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

2004-01-01

We posed the question of what happens to a protein that is known to grow as an n-mer when it is placed in solution conditions where it is monomeric. The trypsin-treated, or cut, form of the protein canavalin (CCAN) has been shown to nucleate and grow crystals as a trimer from neutral to slightly acidic solutions. Under these conditions the solution is composed almost wholly of trimers. The crystalline protein can be readily dissolved by weakly basic solution, which has been proposed to result in a solution that is monomeric. There are three possible outcomes to an attempt at crystallization of the protein under monomeric (high pH) conditions: 1) we will obtain the same crystals as under trimer conditions, but at different protein concentrations governed by the self association equilibria; 2) we will obtain crystals having a different symmetry, based upon a monomeric growth unit; 3) we will not obtain crystals. Obtaining the first result would be indicative that the solution-phase self-association process is critical to the crystal nucleation and growth process. The second result would be less clear, as it may also reflect a pH-dependent shift in the trimer-trimer molecular interactions. The third result, particularly for experiments in the transition pH's between trimeric and monomeric CCAN, would indicate that the monomer does not crystallize, and that solution phase self association is not part of the crystal nucleation and growth path. Results are presented for crystallization experiments of CCAN over the pH 6.4 to 9.6 range. Fluorescence anisotropy, light scattering, and gel filtration experiments show that the solutions are primarily trimers, with association to form larger species occurring as a function of protein concentration.

In meso in situ serial X-ray crystallography of soluble and membrane proteins at cryogenic temperatures

PubMed Central

Huang, Chia-Ying; Olieric, Vincent; Ma, Pikyee; Howe, Nicole; Vogeley, Lutz; Liu, Xiangyu; Warshamanage, Rangana; Weinert, Tobias; Panepucci, Ezequiel; Kobilka, Brian; Diederichs, Kay; Wang, Meitian; Caffrey, Martin

2016-01-01

Here, a method for presenting crystals of soluble and membrane proteins growing in the lipid cubic or sponge phase for in situ diffraction data collection at cryogenic temperatures is introduced. The method dispenses with the need for the technically demanding and inefficient crystal-harvesting step that is an integral part of the lipid cubic phase or in meso method of growing crystals. Crystals are dispersed in a bolus of mesophase sandwiched between thin plastic windows. The bolus contains tens to hundreds of crystals, visible with an in-line microscope at macromolecular crystallography synchrotron beamlines and suitably disposed for conventional or serial crystallographic data collection. Wells containing the crystal-laden boluses are removed individually from hermetically sealed glass plates in which crystallization occurs, affixed to pins on goniometer bases and excess precipitant is removed from around the mesophase. The wells are snap-cooled in liquid nitrogen, stored and shipped in Dewars, and manually or robotically mounted on a goniometer in a cryostream for diffraction data collection at 100 K, as is performed routinely with standard, loop-harvested crystals. The method is a variant on the recently introduced in meso in situ serial crystallography (IMISX) method that enables crystallo­graphic measurements at cryogenic temperatures where crystal lifetimes are enormously enhanced whilst reducing protein consumption dramatically. The new approach has been used to generate high-resolution crystal structures of a G-protein-coupled receptor, α-helical and β-barrel transporters and an enzyme as model integral membrane proteins. Insulin and lysozyme were used as test soluble proteins. The quality of the data that can be generated by this method was attested to by performing sulfur and bromine SAD phasing with two of the test proteins. PMID:26894538

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.

Theoretical study of the impact of stress and interstitial oxygen on the behavior of intrinsic point defects in growing Czochralski Si crystals

NASA Astrophysics Data System (ADS)

Sueoka, K.; Nakamura, K.; Vanhellemont, J.

2017-09-01

For the development of crystal pulling processes for 450 mm-diameter defect-free Si crystals, it is important to evaluate the impact of thermal stress on intrinsic point defect behavior during crystal growth. In a crystal growing from a melt, the melt/solid interface can be considered as being stress-free. Due to that the thermal stress in the growing substrate near the interface is internal plane stress. Previously, we evaluated the impact of (001) planar-isotropic stress on the formation enthalpy (Hf) of the vacancy (V) and the self-interstitial (I) using density functional theory (DFT) calculations, and explained quantitatively the published experimental values of the so-called ;Voronkov criterion;. The thermal stress in a growing crystal is indeed planar but is not isotropic in the plane except for the central region of the crystal. The purpose of the present study is to estimate the impact of planar-anisotropic stress on the formation enthalpy Hf of V and I. It is found that the three stress dependencies of σx: σy=1: 1 (planar-isotropic), 2: 1, 5: 1 (planar-anisotropic) are close to each other, independent of the assumption of isotropic or anisotropic planar stress. This is the reason why the experimental results obtained over the whole radial direction of the crystal are well reproduced by the calculated results assuming planar-isotropic stress. A uniaxial stress dependence which is a good assumption for the crystal peripheral region, leads also to results that are close to those for the planar stress dependence. Also the mechanisms behind the experimentally observed impact of interstitial oxygen (Oi), introduced during Czochralski Si growth, on V and I concentrations are clarified. DFT calculations are performed to obtain the formation energies (Ef) of V and I at all sites within a sphere with 5 Å radius around the Oi atom. Formation (vibration) entropy (Sf) calculations for V and I are also performed. It is found that both EfV and SfV of V in the zigzag-bond (1st, 2nd, 5th) including the Oi atom decrease while EfI of I is not affected by the Oi atom. ;Total V; is defined as the sum of free V and V trapped by the Oi atoms. The total V concentration at the melting point is evaluated by considering the EfV and SfV at each site. The calculated V concentration increases by about 2.9% with 1×1018 Oi cm-3 and agrees well with the experimentally estimated value of a few % increase with 1×1018 Oi cm-3.

Kinetic transition in the order-disorder transformation at a solid/liquid interface

NASA Astrophysics Data System (ADS)

Galenko, P. K.; Nizovtseva, I. G.; Reuther, K.; Rettenmayr, M.

2018-01-01

Phase-field analysis for the kinetic transition in an ordered crystal structure growing from an undercooled liquid is carried out. The results are interpreted on the basis of analytical and numerical solutions of equations describing the dynamics of the phase field, the long-range order parameter as well as the atomic diffusion within the crystal/liquid interface and in the bulk crystal. As an example, the growth of a binary A50B50 crystal is described, and critical undercoolings at characteristic changes of growth velocity and the long-range order parameter are defined. For rapidly growing crystals, analogies and qualitative differences are found in comparison with known non-equilibrium effects, particularly solute trapping and disorder trapping. The results and model predictions are compared qualitatively with results of the theory of kinetic phase transitions (Chernov 1968 Sov. Phys. JETP 26, 1182-1190) and with experimental data obtained for rapid dendritic solidification of congruently melting alloy with order-disorder transition (Hartmann et al. 2009 Europhys. Lett. 87, 40007 (doi:10.1209/0295-5075/87/40007)). This article is part of the theme issue `From atomistic interfaces to dendritic patterns'.

Characterization of the Polycaprolactone Melt Crystallization: Complementary Optical Microscopy, DSC, and AFM Studies

PubMed Central

Speranza, V.; Sorrentino, A.; De Santis, F.; Pantani, R.

2014-01-01

The first stages of the crystallization of polycaprolactone (PCL) were studied using several techniques. The crystallization exotherms measured by differential scanning calorimetry (DSC) were analyzed and compared with results obtained by polarized optical microscopy (POM), rheology, and atomic force microscope (AFM). The experimental results suggest a strong influence of the observation scale. In particular, the AFM, even if limited on time scale, appears to be the most sensitive technique to detect the first stages of crystallization. On the contrary, at least in the case analysed in this work, rheology appears to be the least sensitive technique. DSC and POM provide closer results. This suggests that the definition of induction time in the polymer crystallization is a vague concept that, in any case, requires the definition of the technique used for its characterization. PMID:24523644

Characterization of the polycaprolactone melt crystallization: complementary optical microscopy, DSC, and AFM studies.

PubMed

Speranza, V; Sorrentino, A; De Santis, F; Pantani, R

2014-01-01

The first stages of the crystallization of polycaprolactone (PCL) were studied using several techniques. The crystallization exotherms measured by differential scanning calorimetry (DSC) were analyzed and compared with results obtained by polarized optical microscopy (POM), rheology, and atomic force microscope (AFM). The experimental results suggest a strong influence of the observation scale. In particular, the AFM, even if limited on time scale, appears to be the most sensitive technique to detect the first stages of crystallization. On the contrary, at least in the case analysed in this work, rheology appears to be the least sensitive technique. DSC and POM provide closer results. This suggests that the definition of induction time in the polymer crystallization is a vague concept that, in any case, requires the definition of the technique used for its characterization.

Sodium Flux Growth of Bulk Gallium Nitride

NASA Astrophysics Data System (ADS)

Von Dollen, Paul Martin

This dissertation focused on development of a novel apparatus and techniques for crystal growth of bulk gallium nitride (GaN) using the sodium flux method. Though several methods exist to produce bulk GaN, none have been commercialized on an industrial scale. The sodium flux method offers potentially lower cost production due to relatively mild process conditions while maintaining high crystal quality. But the current equipment and methods for sodium flux growth of bulk GaN are generally not amenable to large-scale crystal growth or in situ investigation of growth processes, which has hampered progress. A key task was to prevent sodium loss or migration from the sodium-gallium growth melt while permitting N2 gas to access the growing crystal, which was accomplished by implementing a reflux condensing stem along with a reusable sealed capsule. The reflux condensing stem also enabled direct monitoring and control of the melt temperature, which has not been previously reported for the sodium flux method. Molybdenum-based materials were identified from a corrosion study as candidates for direct containment of the corrosive sodium-gallium melt. Successful introduction of these materials allowed implementation of a crucible-free containment system, which improved process control and can potentially reduce crystal impurity levels. Using the new growth system, the (0001) Ga face (+c plane) growth rate was >50 mum/hr, which is the highest bulk GaN growth rate reported for the sodium flux method. Omega X-ray rocking curve (?-XRC) measurements indicated the presence of multiple grains, though full width at half maximum (FWHM) values for individual peaks were <100 arcseconds. Oxygen impurity concentrations as measured by secondary ion mass spectroscopy (SIMS) were >1020 atoms/cm3, possibly due to reactor cleaning and handling procedures. This dissertation also introduced an in situ technique to correlate changes in N2 pressure with dissolution of nitrogen and precipitation of GaN from the sodium-gallium melt. Different stages of N2 pressure decay were identified and linked to distinct modes of GaN crystal growth. Based on this analysis, the highest growth rate may have up to 90 mum/hr, and did not appear to be mass-transport limited, in contrast to previous reports. Several refinements and improvements of the novel equipment and methods introduced were also explored, all of which have potential to further advance state of the art sodium flux growth of bulk GaN.

DNA Brick Crystals with Prescribed Depth

PubMed Central

Ke, Yonggang; Ong, Luvena L.; Sun, Wei; Song, Jie; Dong, Mingdong; Shih, William M.; Yin, Peng

2014-01-01

We describe a general framework for constructing two-dimensional crystals with prescribed depth and sophisticated three-dimensional features. These crystals may serve as scaffolds for the precise spatial arrangements of functional materials for diverse applications. The crystals are self-assembled from single-stranded DNA components called DNA bricks. We demonstrate the experimental construction of DNA brick crystals that can grow to micron-size in the lateral dimensions with precisely controlled depth up to 80 nanometers. They can be designed to display user-specified sophisticated three-dimensional nanoscale features, such as continuous or discontinuous cavities and channels, and to pack DNA helices at parallel and perpendicular angles relative to the plane of the crystals. PMID:25343605

Cupric oxide inclusions in cuprous oxide crystals grown by the floating zone method

NASA Astrophysics Data System (ADS)

Frazer, Laszlo; Chang, Kelvin B.; Poeppelmeier, Kenneth R.; Ketterson, John B.

2015-06-01

Phase-pure cuprous oxide (Cu2O) crystals are difficult to grow since cupric oxide can form within the crystal as the crystal is cooled to ambient conditions. Vacancies are the solute which causes precipitation of macroscopic defects. Therefore, even when a mostly phase-pure single crystal is used as a feed rod, cupric oxide inclusions persist in the recrystallized solid. Control of the thermal profile during crystal growth, however, can improve phase-purity; a slow counter-rotation rate of the feed and seed rods results in fewer inclusions. Cupric oxide can be removed by annealing, which produces a factor of 540 ± 70 increase in phase-purity.

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.

Cupric oxide inclusions in cuprous oxide crystals grown by the floating zone method

PubMed Central

Frazer, Laszlo; Chang, Kelvin B; Poeppelmeier, Kenneth R; Ketterson, John B

2015-01-01

Phase-pure cuprous oxide (Cu2O) crystals are difficult to grow since cupric oxide can form within the crystal as the crystal is cooled to ambient conditions. Vacancies are the solute which causes precipitation of macroscopic defects. Therefore, even when a mostly phase-pure single crystal is used as a feed rod, cupric oxide inclusions persist in the recrystallized solid. Control of the thermal profile during crystal growth, however, can improve phase-purity; a slow counter-rotation rate of the feed and seed rods results in fewer inclusions. Cupric oxide can be removed by annealing, which produces a factor of 540 ± 70 increase in phase-purity. PMID:27877798

Method for single crystal growth of photovoltaic perovskite material and devices

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

Huang, Jinsong; Dong, Qingfeng

Systems and methods for perovskite single crystal growth include using a low temperature solution process that employs a temperature gradient in a perovskite solution in a container, also including at least one small perovskite single crystal, and a substrate in the solution upon which substrate a perovskite crystal nucleates and grows, in part due to the temperature gradient in the solution and in part due to a temperature gradient in the substrate. For example, a top portion of the substrate external to the solution may be cooled.

Adaptive temperature profile control of a multizone crystal growth furnace

NASA Technical Reports Server (NTRS)

Batur, C.; Sharpless, R. B.; Duval, W. M. B.; Rosenthal, B. N.

1991-01-01

An intelligent measurement system is described which is used to assess the shape of a crystal while it is growing inside a multizone transparent furnace. A color video imaging system observes the crystal in real time, and determines the position and the shape of the interface. This information is used to evaluate the crystal growth rate, and to analyze the effects of translational velocity and temperature profiles on the shape of the interface. Creation of this knowledge base is the first step to incorporate image processing into furnace control.

Crystal growth, structural, optical, dielectric and thermal studies of an amino acid based organic NLO material: L-Phenylalanine L-phenylalaninium malonate

NASA Astrophysics Data System (ADS)

Prakash, M.; Geetha, D.; Lydia Caroline, M.; Ramesh, P. S.

2011-12-01

Good transparent single crystals of L-phenylalanine L-phenylalaninium malonate (LPPMA) have been grown successfully by slow evaporation technique from aqueous solution. Single crystal X-ray diffractometer was utilized to measure unit cell parameter and to confirm the crystal structure. The chemical structure of compound was established by FT-NMR technique. The vibrational modes of the molecules of elucidated from FTIR spectra. Its optical behaviour has been examined by UV-vis spectral analysis, which shows the absence of absorbance in the visible region. Thermal properties of the LPPMA crystal were carried out by thermo gravimetric analysis (TGA) and differential thermal analysis (DTA) techniques, which indicate that the material does not decompose before melting. The melting point of grown crystal was observed as 180 °C by melting point apparatus. The NLO property was confirmed by the powder technique of Kurtz and Perry. The dielectric behaviour of the sample was also studied for the first time.

Anchoring protein crystals to mounting loops with hydrogel using inkjet technology.

PubMed

Shinoda, Akira; Tanaka, Yoshikazu; Yao, Min; Tanaka, Isao

2014-11-01

X-ray crystallography is an important technique for structure-based drug discovery, mainly because it is the only technique that can reveal whether a ligand binds to the target protein as well as where and how it binds. However, ligand screening by X-ray crystallography involves a crystal-soaking experiment, which is usually performed manually. Thus, the throughput is not satisfactory for screening large numbers of candidate ligands. In this study, a technique to anchor protein crystals to mounting loops by using gel and inkjet technology has been developed; the method allows soaking of the mounted crystals in ligand-containing solution. This new technique may assist in the design of a fully automated drug-screening pipeline.

A synergistic approach to protein crystallization: Combination of a fixed-arm carrier with surface entropy reduction

PubMed Central

Moon, Andrea F; Mueller, Geoffrey A; Zhong, Xuejun; Pedersen, Lars C

2010-01-01

Protein crystallographers are often confronted with recalcitrant proteins not readily crystallizable, or which crystallize in problematic forms. A variety of techniques have been used to surmount such obstacles: crystallization using carrier proteins or antibody complexes, chemical modification, surface entropy reduction, proteolytic digestion, and additive screening. Here we present a synergistic approach for successful crystallization of proteins that do not form diffraction quality crystals using conventional methods. This approach combines favorable aspects of carrier-driven crystallization with surface entropy reduction. We have generated a series of maltose binding protein (MBP) fusion constructs containing different surface mutations designed to reduce surface entropy and encourage crystal lattice formation. The MBP advantageously increases protein expression and solubility, and provides a streamlined purification protocol. Using this technique, we have successfully solved the structures of three unrelated proteins that were previously unattainable. This crystallization technique represents a valuable rescue strategy for protein structure solution when conventional methods fail. PMID:20196072

Supercrystallization of KCl from solution irradiated by soft X-rays

NASA Astrophysics Data System (ADS)

Janavičius, A. J.; Rinkūnas, R.; Purlys, R.

2016-10-01

The X-rays influence on KCl crystallization in a saturated water solution has been investigated for the aim of comparing it with previously considered NaCl crystallization. The rate of crystallization has been measured in the drying drop in the solution activated by the irradiation. We have measured the influence of the irradiation time of the solution on the rates of KCl crystallization as well as the beginning of the crystallization processes on drying drops. For a longer irradiation time of the solution early crystallization in the drops occurs. A saturated water solution of KCl was irradiated with the diffractometer DRON-3M (Russian device) and this had a great influence on the two-step processes of crystallization. The ionization of the solution by soft X-rays can produce ions, metastable radicals in water, excited crystals' seeds and vacancies in growing crystals by Auger's effect. The X-rays generate a very fast crystallization in the drying drop.

Crystal Growth and Characterization of THO2 and UxTh1-xO2

DTIC Science & Technology

2013-03-01

bulk actinide crystals would open up new possibilities for the detection of weapons of mass destruction, the study of the effect of aging on...way of growing bulk actinide materials of optical quality. These refractory oxide single crystals offer potential applications in thorium nuclear...fuel technology, wide-band-gap uranium-based direct-conversion solid state neutron detectors, and understanding how actinide fuels age with time. ThO2

Growth and characterization of 4-chloro-3-nitrobenzophenone single crystals using vertical Bridgman technique

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

Aravinth, K., E-mail: anandcgc@gmail.com; Babu, G. Anandha, E-mail: anandcgc@gmail.com; Ramasamy, P., E-mail: anandcgc@gmail.com

2014-04-24

4-chloro-3-nitrobenzophenone (4C3N) has been grown by using vertical Bridgman technique. The grown crystal was confirmed by Powder X-ray diffraction analysis. The crystalline perfection of the grown crystal was examined by high-resolution X-ray diffraction study. The fluorescence spectra of grown 4C3N single crystals exhibit emission peak at 575 nm. The micro hardness measurements were used to analyze the mechanical property of the grown crystal.

The role of mass transport in protein crystallization.

PubMed

García-Ruiz, Juan Manuel; Otálora, Fermín; García-Caballero, Alfonso

2016-02-01

Mass transport takes place within the mesoscopic to macroscopic scale range and plays a key role in crystal growth that may affect the result of the crystallization experiment. The influence of mass transport is different depending on the crystallization technique employed, essentially because each technique reaches supersaturation in its own unique way. In the case of batch experiments, there are some complex phenomena that take place at the interface between solutions upon mixing. These transport instabilities may drastically affect the reproducibility of crystallization experiments, and different outcomes may be obtained depending on whether or not the drop is homogenized. In diffusion experiments with aqueous solutions, evaporation leads to fascinating transport phenomena. When a drop starts to evaporate, there is an increase in concentration near the interface between the drop and the air until a nucleation event eventually takes place. Upon growth, the weight of the floating crystal overcomes the surface tension and the crystal falls to the bottom of the drop. The very growth of the crystal then triggers convective flow and inhomogeneities in supersaturation values in the drop owing to buoyancy of the lighter concentration-depleted solution surrounding the crystal. Finally, the counter-diffusion technique works if, and only if, diffusive mass transport is assured. The technique relies on the propagation of a supersaturation wave that moves across the elongated protein chamber and is the result of the coupling of reaction (crystallization) and diffusion. The goal of this review is to convince protein crystal growers that in spite of the small volume of the typical protein crystallization setup, transport plays a key role in the crystal quality, size and phase in both screening and optimization experiments.

Local Structure and Anisotropy in the Amorphous Precursor= to Ba-Hexaferrite Thin Films

NASA Astrophysics Data System (ADS)

Snyder, J. E.; Harris, V. G.; Koon, N. C.; Sui, X.; Kryder, M. H.

1996-03-01

Ba-hexaferrite thin-films for recording media applications are commonly fabricated by a two-step process: sputter-deposition of an amorphous precursor, followed by annealing to crystallize the BaFe_12O_19 phase. The magnetic anisotropy of the crystalline films can be either in-plane or perpendicular, depending on the sputtering process used in the first step. However, conventional characterization techniques (x-ray diffraction and TEM) have been unable to observe any structure in the amorphous precursor films. In this study, such films are investigated by PD-EXAFS (polarization-dependent extended x-ray absorption fine structure). An anisotropic local ordered structure is observed around both Fe and Ba atoms in the "amorphous" films. This anisotropic local structure appears to determine the orientation of the fast-growing basal plane directions during crystallization, and thus the directions of the c-axes and the magnetic anisotropy. Results suggest that the structure of the amorphous films consists of networks made up of units of Fe atoms surrounded by their O nearest neighbors, that are connected together. Ba atoms appear to fit into in-between spaces as network-modifiers.

The Stonehenge technique. A method for aligning coherent bremsstrahlung radiators

NASA Astrophysics Data System (ADS)

Livingston, Ken

2009-05-01

This paper describes a technique for the alignment of crystal radiators used to produce high energy, linearly polarized photons via coherent bremsstrahlung scattering at electron beam facilities. In these experiments the crystal is mounted on a goniometer which is used to adjust its orientation relative to the electron beam. The angles and equations which relate the crystal lattice, goniometer and electron beam direction are presented here, and the method of alignment is illustrated with data taken at MAMI (the Mainz microtron). A practical guide to setting up a coherent bremsstrahlung facility and installing new crystals using this technique is also included.

Study of thin film production of ceramic ZrO2 on silicon wafer using second harmonic Nd-Yag laser with pulsed laser deposition technique

NASA Astrophysics Data System (ADS)

Suliyanti, Maria M.; Hidayah, Affi Nur; Kurniawan, K. H.

2012-06-01

Study about thin film production using technique pulsed laser deposition have been done. The Pulsed Laser Deposition (PLD) method has been used for growing thin film of ZrO2 on silicon wafer substrate (111 single crystal, thickness 400μm and diameter 7.5 cm). The target made from Zirconia oxide powder mixing with PVA and press using pressure 100kgN. The laser beam was focused by a lens (f = 100mm) through a quartz window onto the sample surface and the substrate was placed in parallel line with target. The distance between the target and the substrate is about 1 cm. The early results of this synthesis using 75 mJ Nd-YAG second harmonic laser pulse (532 nm Nd-YAG) and low pressure chamber surrounding gas 5 Torr. The irradiation of laser take around 6000 shoots or 10 minutes using frequencies laser 10 Hz. The micro thickness of film can be produced on silicon wafer using this technique. The results of ZrO2 thin film on substrate about 26.92%.

The HB-2D Polarized Neutron Development Beamline at the High Flux Isotope Reactor

NASA Astrophysics Data System (ADS)

Crow, Lowell; Hamilton, WA; Zhao, JK; Robertson, JL

2016-09-01

The Polarized Neutron Development beamline, recently commissioned at the HB-2D position on the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory, provides a tool for development and testing of polarizers, polarized neutron devices, and prototyping of polarized neutron techniques. With available monochromators including pyrolytic graphite and polarizing enriched Fe-57 (Si), the instrument has operated at 4.25 and 2.6 Å wavelengths, using crystal, supermirror, or He-3 polarizers and analyzers in various configurations. The Neutron Optics and Development Team has used the beamline for testing of He-3 polarizers for use at other HFIR and Spallation Neutron Source (SNS) instruments, as well as a variety of flipper devices. Recently, we have acquired new supermirror polarizers which have improved the instrument performance. The team and collaborators also have continuing demonstration experiments of spin-echo focusing techniques, and plans to conduct polarized diffraction measurements. The beamline is also used to support a growing use of polarization techniques at present and future instruments at SNS and HFIR.

Modeling of PCG fluid dynamics: Salient results

NASA Technical Reports Server (NTRS)

Ramachandran, N.

1993-01-01

Materials processing in space-based laboratories has already yielded higher quality crystals during previous space flights, and opportunities for several fluids experiments are anticipated during the extended duration missions planned for the future. Crystal growth in space benefits not only from its reduced gravity environment but also from the absence of the hydrostatic pressure which assists certain crystal growth and refinement methods. Gravity-driven phenomena are thus reduced in strength, and a purely diffusive fluid's behavior can be attained. In addition, past materials science experiments have shown that microgravity can also help produce larger crystals. While gravity-related effects are definitely curtailed in space, they are nevertheless present to some degree due to the acceleration environment onboard the spacecraft. This residual acceleration level is comprised of quasi-steady, oscillatory, and transient components, and is caused by a variety of mechanisms. For example, gravity gradient forces produce low frequency disturbances, and the operation of machinery, control thrusters, solar panels, human activity, etc. contribute to higher frequency accelerations. These disturbances are collectively referred to as g-jitter, and they can be deleterious to certain experiments where the minimization of the acceleration level is important. Advanced vibration isolation techniques can be utilized to actively filter out some of the detrimental frequencies and help in obtaining optimum results. However, the successful application of this technology requires the detailed analysis of candidate fluids experiments to gauge their response to g-jitter and to determine their acceleration sensitivities. Several crystal growth experiments in the Protein Crystal Growth (PCG) area, besides others, are expected to be carried out on future shuttle flights and on Space Station Freedom. The need for vibration isolation systems or components for microgravity science experiments can be expected to grow as experiments and available hardware becomes more complex. This technology will also find increased application as the science community develops an awareness of their specific needs relative to the environment available in manned space missions. Vibration isolation research strives to develop a microgravity environment requirement that defines tolerance limits on the allowable g-level, and provides the required technology to achieve it. This effort will assist in establishing the tolerable acceleration levels for specific fluids experiments. The primary effort is directed towards modeling PCG and the approach undertaken for this investigation is outlined. The objectives of this research are: (1) to computationally determine vibration sensitivity of protein crystal growth experiments; (2) determine if these experiments can benefit from vibration isolation techniques; and (3) provide realistic requirements for vibration isolation technology.

Growth of tourmaline single crystals containing transition metal elements in hydrothermal solutions

NASA Astrophysics Data System (ADS)

Setkova, Tatiana; Shapovalov, Yury; Balitsky, Vladimir

2011-03-01

Interest in the growth of tourmaline single crystals is based on the promising piezoelectric and pyroelectric properties of this material compared to quartz crystals currently in use. Moreover, synthetic tourmaline can be used as a substitute for the natural stone in the jewelry industry similar to other synthetic analogues of gemstones. Single crystals of colored Co-, Ni-, Fe-, (Ni,Cr)-, (Ni,Fe)-, and (Co,Ni,Cr)-containing tourmalines with concentration of transition metal elements up to 16 wt% on a seed have been grown from complex boron-containing hydrothermal solutions at a range of temperatures 400-750 °C and pressures 100 MPa. Experiments were conducted under conditions of a thermal gradient in titanium and chromium-nickel autoclaves. Tourmaline growth on a seed crystal occurs only if separate tourmaline-forming components (monocrystalline corundum and quartz bars) are used as charge. All tourmalines specified above grow in analogous (+) direction of the optical axis with a speed of 0.05 mm/day by faces of the trigonal pyramid, except tourmalines containing chromium. They grow in analogous (+0001) direction with a speed 0.05 mm/day, and in antilogous (-0001) direction with a speed of 0.01 mm/day by faces of the trigonal pyramid and in prism direction with a speed of 0.001 mm/day. Along with the large single crystals, a great amount of finest (30-150 μm in size) tourmaline crystals was formed during the runs by spontaneous nucleation both on the surface of the seed crystals and in the charge.

Study of crystallization mechanisms of Fe nanoparticle

NASA Astrophysics Data System (ADS)

Kien, P. H.; Trang, G. T. T.; Hung, P. K.

2017-06-01

In this paper, the nanoparticle (NP) Fe was investigated by means of molecular dynamics simulation. The crystallization mechanism was studied through the time evolution of crystal cluster and potential energies of different atom types. The simulation shows that the NP was crystallized into bcc crystal structure when it was annealed at 900 K for long times. At early stage of the annealing, small nuclei form in different places of NP and dissolve for short times. After long times some nuclei form and gather nearby which create the stable clusters in the core of NP. After that the crystal clusters grow in the direction to cover the core and then to spread into the surface of NP. Analyzing the energies of different type atoms, we found that the crystal growth is originated from specific atomic arrangement in the boundary region of crystal clusters.

Improving the Quality of Protein Crystals Using Stirring Crystallization

NASA Astrophysics Data System (ADS)

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

2004-04-01

Recent reports state that a high magnetic field improves the crystal quality of bovine adenosine deaminase (ADA) with an inhibitor [Kinoshita et al.: Acta Cryst. D59 (2003) 1333]. In this paper, we examine the effect of stirring solution on ADA crystallization using a vapor-diffusion technique with rotary and figure-eight motion shakers. The probability of obtaining high-quality crystals is increased with stirring in a figure-eight pattern. Furthermore, rotary stirring greatly increased the probability of obtaining high-quality crystals, however, nucleation time was also increased. The crystal structure with the inhibitor was determined at a high resolution using a crystal obtained from a stirred solution. These results indicate that stirring with simple equipment is as useful as the high magnetic field technique for protein crystallization.

Growth and characterization of hexamethylenetetramine crystals grown from solution

NASA Astrophysics Data System (ADS)

Babu, B.; Chandrasekaran, J.; Balaprabhakaran, S.

2014-06-01

Organic nonlinear optical single crystals of hexamethylenetetramine (HMT; 10 × 10 × 5 mm3) were prepared by crystallization from methanol solution. The grown crystals were subjected to various characterization techniques such as single crystal XRD, powder XRD, UV-Vis and electrical studies. Single crystal XRD analysis confirmed the crystalline structure of the grown crystals. Their crystalline nature was also confirmed by powder XRD technique. The optical transmittance property was identified from UV-Vis spectrum. Dielectric measurements were performed as a function of frequency at different temperatures. DC conductivity and photoconductivity studies were also carried out for the crystal. The powder second harmonic generation efficiency (SHG) of the crystal was measured using Nd:YAG laser and the efficiency was found to be two times greater than that of potassium dihydrogen phosphate (KDP).

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.

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.

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.

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.

Crystal growth and characterization of semi organic nonlinear optical (NLO) piperazinium tetrachlorozincate monohydrate (PTCZ) single crystal

NASA Astrophysics Data System (ADS)

Karuppasamy, P.; Pandian, Muthu Senthil; Ramasamy, P.

2018-04-01

The semi-organic single crystal of piperazinium tetrachlorozincate monohydrate (PTCZ) was successfully grown by slow evaporation solution technique (SEST). The grown crystal was subjected to the single crystal XRD studies for confirming the unit cell parameters. The optical quality of the grown crystal was identified by the UV-Vis NIR spectrum analysis and the optical band gap energy was calculated. The photoconductivity study reveals that the grown crystal has positive photoconductive nature. The mechanical stability of the grown crystal was analyzed using Vickers microhardness analyzer. The third-order nonlinear optical properties such as nonlinear refractive index (n2), absorption co-efficient (β) and susceptibility (χ(3)) were studied by Z-scan technique at 640 nm using solid state laser.

Structural, mechanical, electrical and optical properties of a new lithium boro phthalate NLO crystal synthesized by a slow evaporation method

NASA Astrophysics Data System (ADS)

Mohanraj, K.; Balasubramanian, D.; Jhansi, N.

2017-11-01

A new non-linear optical (NLO) single crystal of lithium boro phthalate (LiBP) was grown by slow solvent evaporation technique. The powder sample was subjected to powder X-ray diffraction (PXRD) to find its crystalline nature and the crystal structure of the grown crystal was determined using single crystal X-ray (SXRD) diffraction analysis. The Fourier Transform Infrared (FTIR) spectrum was recorded for grown crystal to identify the various functional groups present in the compound. The mechanical property of the LiBP single crystal was studied using Vickers microhardness tester. The dielectric constant and dielectric loss measurements were carried out for the grown crystal at various temperatures. The grown crystal was subjected to UV-Visible Spectral Studies to analyze the linear optical behavior of the grown crystal. The Kurtz-Perry Powder technique was employed to measure the Second Harmonic Generation efficiency of the grown crystal.

Defect reduction in seeded aluminum nitride crystal growth

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

Bondokov, Robert T.; Morgan, Kenneth E.; Schowalter, Leo J.

2017-04-18

Bulk single crystal of aluminum nitride (AlN) having an areal planar defect density.ltoreq.100 cm.sup.-2. Methods for growing single crystal aluminum nitride include melting an aluminum foil to uniformly wet a foundation with a layer of aluminum, the foundation forming a portion of an AlN seed holder, for an AlN seed to be used for the AlN growth. The holder may consist essentially of a substantially impervious backing plate.

Defect reduction in seeded aluminum nitride crystal growth

DOEpatents

Bondokov, Robert T.; Morgan, Kenneth E.; Schowalter, Leo J.; Slack, Glen A.

2017-06-06

Bulk single crystal of aluminum nitride (AlN) having an areal planar defect density .ltoreq.100 cm.sup.-2. Methods for growing single crystal aluminum nitride include melting an aluminum foil to uniformly wet a foundation with a layer of aluminum, the foundation forming a portion of an AlN seed holder, for an AlN seed to be used for the AlN growth. The holder may consist essentially of a substantially impervious backing plate.

Defect reduction in seeded aluminum nitride crystal growth

DOEpatents

Bondokov, Robert T.; Schowalter, Leo J.; Morgan, Kenneth; Slack, Glen A; Rao, Shailaja P.; Gibb, Shawn Robert

2017-09-26

Bulk single crystal of aluminum nitride (AlN) having an areal planar defect density.ltoreq.100 cm.sup.-2. Methods for growing single crystal aluminum nitride include melting an aluminum foil to uniformly wet a foundation with a layer of aluminum, the foundation forming a portion of an AlN seed holder, for an AlN seed to be used for the AlN growth. The holder may consist essentially of a substantially impervious backing plate.

The stonehenge technique: a new method of crystal alignment for coherent bremsstrahlung experiments

NASA Astrophysics Data System (ADS)

Livingston, Kenneth

2005-08-01

In the coherent bremsstrahlung technique a thin diamond crystal oriented correctly in an electron beam can produce photons with a high degree of linear polarization.1 The crystal is mounted on a goniometer to control its orientation and it is necessary to measure the angular offsets a) between the crystal axes and the goniometer axes and b) between the goniometer and the electron beam axis. A method for measuring these offsets and aligning the crystal was developed by Lohman et al, and has been used successfully in Mainz.2 However, recent attempts to investigate new crystals have shown that this approach has limitations which become more serious at higher beam energies where more accurate setting of the crystal angles, which scale with l/Ebeam, is required. (Eg. the recent installation of coherent bremsstrahlung facility at Jlab, with Ebeam = 6 GeV ) This paper describes a new, more general alignment technique, which overcomes these limitations. The technique is based on scans where the horizontal and vertical rotation axes of the goniometer are adjusted in a series of steps to make the normal to the crystal describe a cone of a given angle. For each step in the scan, the photon energy spectrum is measured using a tagging spectrometer, and the offsets between the electron beam and the crystal lattice are inferred from the resulting 2D plot. Using this method, it is possible to align the crystal with the beam quickly, and hence to set any desired orientation of the crystal relative to the beam. This is essential for any experiment requiring linearly polarized photons produced via coherent bremsstrahlung, and is also required for a systematic study of the channeling radiation produced by the electron beam incident on the crystal.

Crystal growth, piezoelectric, non-linear optical and mechanical properties of lithium hydrogen oxalate monohydrate single crystal

NASA Astrophysics Data System (ADS)

Chandran, Senthilkumar; Paulraj, Rajesh; Ramasamy, P.

2017-05-01

Semi-organic lithium hydrogen oxalate monohydrate non-linear optical single crystals have been grown by slow evaporation solution growth technique at 35 °C. Single crystal X-ray diffraction study showed that the grown crystal belongs to the triclinic system with space group P1. The mechanical strength decreases with increasing load. The piezoelectric coefficient is found to be 1.41 pC/N. The nonlinear optical property was measured using Kurtz Perry powder technique and SHG efficiency was almost equal to that of KDP.

Phoenito experiments: combining the strengths of commercial crystallization automation.

PubMed

Newman, Janet; Pham, Tam M; Peat, Thomas S

2008-11-01

The use of crystallization robots for initial screening in macromolecular crystallization is well established. This paper describes how four general optimization techniques, growth-rate modulation, fine screening, seeding and additive screening, have been adapted for automation in a medium-throughput crystallization service facility. The use of automation for more challenging optimization experiments is discussed, as is a novel way of using both the Mosquito and the Phoenix nano-dispensing robots during the setup of a single crystallization plate. This dual-dispenser technique plays to the strengths of both machines.

Phoenito experiments: combining the strengths of commercial crystallization automation

PubMed Central

Newman, Janet; Pham, Tam M.; Peat, Thomas S.

2008-01-01

The use of crystallization robots for initial screening in macromolecular crystallization is well established. This paper describes how four general optimization techniques, growth-rate modulation, fine screening, seeding and additive screening, have been adapted for automation in a medium-throughput crystallization service facility. The use of automation for more challenging optimization experiments is discussed, as is a novel way of using both the Mosquito and the Phoenix nano-dispensing robots during the setup of a single crystallization plate. This dual-dispenser technique plays to the strengths of both machines. PMID:18997323

Dynamically controlled crystallization method and apparatus and crystals obtained thereby

NASA Technical Reports Server (NTRS)

Arnowitz, Leonard (Inventor); Steinberg, Emanuel (Inventor)

2003-01-01

A method and apparatus for dynamically controlling the crystallization of molecules including a crystallization chamber (14) or chambers for holding molecules in a precipitant solution, one or more precipitant solution reservoirs (16, 18), communication passages (17, 19) respectively coupling the crystallization chamber(s) with each of the precipitant solution reservoirs, and transfer mechanisms (20, 21, 22, 24, 26, 28) configured to respectively transfer precipitant solution between each of the precipitant solution reservoirs and the crystallization chamber(s). The transfer mechanisms are interlocked to maintain a constant volume of precipitant solution in the crystallization chamber(s). Precipitant solutions of different concentrations are transferred into and out of the crystallization chamber(s) to adjust the concentration of precipitant in the crystallization chamber(s) to achieve precise control of the crystallization process. The method and apparatus can be used effectively to grow crystals under reduced gravity conditions such as microgravity conditions of space, and under conditions of reduced or enhanced effective gravity as induced by a powerful magnetic field.

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.

Characterization of zinc selenide single crystals

NASA Technical Reports Server (NTRS)

Gerhardt, Rosario A.

1996-01-01

ZnSe single crystals of high quality and low impurity levels are desired for use as substrates in optoelectronic devices. This is especially true when the device requires the formation of homoepitaxial layers. While ZnSe is commercially available, it is at present extremely expensive due to the difficulty of growing single crystal boules with low impurity content and the resultant low yields. Many researchers have found it necessary to heat treat the crystals in liquid Zn in order to remove the impurities, lower the resistivity and activate the photoluminescence at room temperature. The physical vapor transport method (PVT) has been successfully used at MSFC to grow many single crystals of II-VI semiconducting materials including ZnSe. The main goal at NASA has been to try to establish the effect of gravity on the growth parameters. To this effect, crystals have been grown vertically upwards or horizontally. Both (111) and (110) oriented ZnSe crystals have been obtained via unseeded PVT growth. Preliminary characterization of the horizontally grown crystals has revealed that Cu is a major impurity and that the low temperature photoluminescence spectra is dominated by the copper peak. The ratio of the copper peak to the free exciton peak is being used to determine variations in composition throughout the crystal. It was the intent of this project to map the copper composition of various crystals via photoluminescence first, then measure their electrical resistivity and capacitance as a function of frequency before proceeding with a heat treatment designed to remove the copper impurities. However, equipment difficulties with the photoluminescence set up, having to establish a procedure for measuring the electrical properties of the as-grown crystals and time limitations made us re-evaluate the project goals. Vertically grown samples designated as ZnSe-25 were chosen to be measured electrically since they were not expected to show as much variation in their composition through their cross-section as the horizontally grown samples.

High purity, low dislocation GaAs single crystals

NASA Technical Reports Server (NTRS)

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

1983-01-01

Liquid encapsulated Czochralski crystal growth techniques for producing undoped, high resistivity, low dislocation material suitable for device applications is described. Technique development resulted in reduction of dislocation densities in 3 inch GaAs crystals. Control over the melt stoichiometry was determined to be of critical importance for the reduction of twinning and polycrystallinity during growth.

Study on optical properties of L-valine doped ADP crystal

NASA Astrophysics Data System (ADS)

Shaikh, R. N.; Anis, Mohd.; Shirsat, M. D.; Hussaini, S. S.

2015-02-01

Single crystal of L-valine doped ammonium dihydrogen phosphate has been grown by slow evaporation method at room temperature. The crystalline nature of the grown crystal was confirmed using powder X-ray diffraction technique. The different functional groups of the grown crystal were identified using Fourier transform infrared analysis. The UV-visible studies were employed to examine the high optical transparency and influential optical constants for tailoring materials suitability for optoelectronics applications. The cutoff wavelength of the title crystal was found to be 280 nm with wide optical band gap of 4.7 eV. The dielectric measurements were carried to determine the dielectric constant and dielectric loss at room temperature. The grown crystal has been characterized by thermogravimetric analysis. The second harmonic generation efficiency of the grown crystal was determined by the classical Kurtz powder technique and it is found to be 1.92 times that of potassium dihydrogen phosphate. The grown crystal was identified as third order nonlinear optical material employing Z-scan technique using He-Ne laser operating at 632.8 nm.

Synthesis, growth, structural characterization, Hirshfeld analysis and nonlinear optical studies of a methyl substituted chalcone

NASA Astrophysics Data System (ADS)

Prabhu, Shobha R.; Jayarama, A.; Chandrasekharan, K.; Upadhyaya, V.; Ng, Seik Weng

2017-05-01

A new chalcone compound (2E)-3-(3-methylphenyl)-1-(4-nitrophenyl)prop-2-en-1-one (3MPNP) with molecular formula C16H13NO3 has been synthesized and crystallized by slow solvent evaporation technique. The Fourier transform infrared, Fourier transform Raman and nuclear magnetic resonance techniques were used for structural characterization. UV-visible absorption studies were carried out to study the transparency of the crystal in the visible region. Differential scanning calorimetry study shows thermal stability of crystals up to temperature 122 °C. Single crystal X-ray diffraction and powder X-ray diffraction techniques were used to study crystal structure and cell parameters. The Hirshfeld surface and 2-D fingerprint analysis were performed to study the nature of interactions and their quantitative contributions towards the crystal packing. The third order non-linear optical properties have been studied using single beam Z-scan technique and the results show that the material is a potential candidate for optical device applications such as optical limiters and optical switches.

Crystal growth, structural, optical, dielectric and thermal studies of an amino acid based organic NLO material: L-phenylalanine L-phenylalaninium malonate.

PubMed

Prakash, M; Geetha, D; Caroline, M Lydia; Ramesh, P S

2011-12-01

Good transparent single crystals of L-phenylalanine L-phenylalaninium malonate (LPPMA) have been grown successfully by slow evaporation technique from aqueous solution. Single crystal X-ray diffractometer was utilized to measure unit cell parameter and to confirm the crystal structure. The chemical structure of compound was established by FT-NMR technique. The vibrational modes of the molecules of elucidated from FTIR spectra. Its optical behaviour has been examined by UV-vis spectral analysis, which shows the absence of absorbance in the visible region. Thermal properties of the LPPMA crystal were carried out by thermo gravimetric analysis (TGA) and differential thermal analysis (DTA) techniques, which indicate that the material does not decompose before melting. The melting point of grown crystal was observed as 180°C by melting point apparatus. The NLO property was confirmed by the powder technique of Kurtz and Perry. The dielectric behaviour of the sample was also studied for the first time. Copyright © 2011 Elsevier B.V. All rights reserved.

Visualizing the Impurity Depletion Zone Around Holoferritin Crystals Growing in Gel with Ferritin Dimers

NASA Technical Reports Server (NTRS)

Chernov, A. A.; Garcia-Ruiz, J. M.; Thomas, B. R.

2000-01-01

Colorless transparent apoferritin (Mr = 450KDa) crystals have been grown from gel with Cd(2+) as precipitant in the presence of reddish brown-colored ferritin dimers (Mr = 900KDa). In agreement with our previous measurements, showing preferential trapping of dimers (distribution coefficient K = 4), the apoferritin crystals become strongly colored while the gel solution around them became nearly colorless. The depth of the depletion with respect to the colored dimer impurity allowed us to visualize the impurity depletion zone. Depletion with respect to impurity as compared to the crystallizing protein is discussed.

Zeolite crystal growth in space - What has been learned

NASA Technical Reports Server (NTRS)

Sacco, A., Jr.; Thompson, R. W.; Dixon, A. G.

1993-01-01

Three zeolite crystal growth experiments developed at WPI have been performed in space in last twelve months. One experiment, GAS-1, illustrated that to grow large, crystallographically uniform crystals in space, the precursor solutions should be mixed in microgravity. Another experiment evaluated the optimum mixing protocol for solutions that chemically interact ('gel') on contact. These results were utilized in setting the protocol for mixing nineteen zeolite solutions that were then processed and yielded zeolites A, X and mordenite. All solutions in which the nucleation event was influenced produced larger, more 'uniform' crystals than did identical solutions processed on earth.

Reduction of Defects in Germanium-Silicon

NASA Technical Reports Server (NTRS)

Szofran, F. R.; Benz, K. W.; Cobb, S. D.; Croell, A.; Dold, P.; Kaiser, N.; Motakel, S.; Walker, J. S.

2000-01-01

Crystals grown without contact with a container have far superior quality to otherwise similar crystals grown in direct contact with a container. In addition to float-zone processing, detached-Bridgman growth is a promising tool to improve crystal quality, without the limitations of float zoning. Detached growth has been found to occur frequently during microg experiments and considerable improvements of crystal quality have been reported for those cases. However, no thorough understanding of the process or quantitative assessment of the quality improvements exists so far. This project is determining the means to reproducibly grow Ge-Si alloys in the detached mode.

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%.

Size control of Au NPs supported by pH operation

NASA Astrophysics Data System (ADS)

Ichiji, Masumi; Akiba, Hiroko; Hirasawa, Izumi

2017-07-01

Au NPs are expected to become useful functional particles, as particle gun used for plant gene transfer and also catalysts. We have studied PSD (particle size distribution) control of Au NPs by reduction crystallization. Previous study found out importance of seeds policy and also feeding profile. In this paper, effect of pH in the reduction crystallization was investigated to clarify the possibility of Au NPs PSD control by pH operation and also their growth process. Au NPs of size range 10-600 nm were obtained in single-jet system using ascorbic acid (AsA) as a reducing agent with adjusting pH of AsA. Au NPs are found to grow in the process of nucleation, agglomeration, agglomeration growth and surface growth. Au NPs tend to grow by agglomeration and become larger size in lower pH regions, and to grow only by surface growth and become smaller size in higher pH regions.

Spectroscopic studies of gel grown zinc doped calcium hydrogen phosphate dihydrate crystals

NASA Astrophysics Data System (ADS)

Suryawanshi, V. B.; Chaudhari, R. T.

2018-05-01

The influence of zinc doping on the gel grown calcium hydrogen phosphate dihydrate crystals was studied using the spectroscopic techniques, which included SEM, FTIR and EDAX. It was found that, zinc ions transform the morphology of brushite crystals from rectangular plate shaped crystals to branching microcrystal patterns. However in FT-IR spectroscopy, as compared to undoped brushite crystals few vibrations were shifted to higher value. The observed changes in the vibrations were due to the impact of zinc ions. EDAX techniques is use to determine the percentage composition of elements present in the doped crystals. It revealed that the sample was of a mixed composition.

Growing Oxide Nanowires and Nanowire Networks by Solid State Contact Diffusion into Solution-Processed Thin Films.

PubMed

Glynn, Colm; McNulty, David; Geaney, Hugh; O'Dwyer, Colm

2016-11-01

New techniques to directly grow metal oxide nanowire networks without the need for initial nanoparticle seed deposition or postsynthesis nanowire casting will bridge the gap between bottom-up formation and top-down processing for many electronic, photonic, energy storage, and conversion technologies. Whether etched top-down, or grown from catalyst nanoparticles bottom-up, nanowire growth relies on heterogeneous material seeds. Converting surface oxide films, ubiquitous in the microelectronics industry, to nanowires and nanowire networks by the incorporation of extra species through interdiffusion can provide an alternative deposition method. It is shown that solution-processed thin films of oxides can be converted and recrystallized into nanowires and networks of nanowires by solid-state interdiffusion of ionic species from a mechanically contacted donor substrate. NaVO 3 nanowire networks on smooth Si/SiO 2 and granular fluorine-doped tin oxide surfaces can be formed by low-temperature annealing of a Na diffusion species-containing donor glass to a solution-processed V 2 O 5 thin film, where recrystallization drives nanowire growth according to the crystal habit of the new oxide phase. This technique illustrates a new method for the direct formation of complex metal oxide nanowires on technologically relevant substrates, from smooth semiconductors, to transparent conducting materials and interdigitated device structures. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Crystallization of the Fab from a human monoclonal antibody against gp 41 of human immunodeficiency virus type I

NASA Technical Reports Server (NTRS)

Casale, Elena; He, Xiao-Min; Snyder, Robert S.; Carter, Daniel C.; Wenisch, Elisabeth; Jungbauer, Alois; Tauer, Christa; Ruker, Florian; Righetti, Pier Giorgio

1990-01-01

A monoclonal IgG antibody directed against gp 41 from the human immunodeficiency virus (HIV-1) has been crystallized in both intact and Fab forms. Crystals of the intact antibody grow as tetragonal-like prisms too small for conventional X-ray analysis. However, the Fab portion of the antibody produces suitable platelike crystals which belong to the space group P2(1)2(1)2(1) with unit cell constants of a = 66.5 A, b = 74.3 A, and c = 105.3 A. There is one molecule of Fab in the asymmetric unit. The Fab crystals show diffraction to d-spacings less than 3.0 A.

Crystal growth of triphenylphosphine oxide 4-nitrophenol (TP4N) for nonlinear optical (NLO) applications

NASA Astrophysics Data System (ADS)

Pandian, Muthu Senthil; Karuppasamy, P.; Kamalesh, T.; Ramasamy, P.; Verma, Sunil

2018-04-01

The optically good quality organic single crystals of triphenylphosphine oxide 4-nitrophenol (TP4N) were successfully grown by slow evaporation solution technique (SEST) using methanol as solvent. The lattice parameters of the grown crystal were confirmed by single crystal X-ray diffraction analysis. The optical transmittance, cut-off wavelength and band gap of the TP4N crystal were obtained by UV-Vis NIR spectrum analysis. The photoluminescence studies were carried out to find out the luminesce properties of TP4N single crystal. The photoconductivity studies reveal that the TP4N crystal has negative photoconductive nature. The third order nonlinear susceptibility (χ(3)) of TP4N crystal was evaluated using the Z-scan technique at 640 nm.

Growth, optical, ICP and thermal studies of nonlinear optical single crystal: Sodium acid phthalate (NaAP)

NASA Astrophysics Data System (ADS)

Mahadevan, M.; Arivanandhan, M.; Elangovan, K.; Anandan, P.; Ramachandran, K.

2017-07-01

Good quality single crystals of sodium acid phthalate (NaAP) were grown by slow evaporation technique. Single crystal X-ray diffraction study of the grown crystal reveals that the crystal belongs to orthorhombic system with space group B2ab. Fourier transform infrared spectrum confirms the presence of the functional groups of the grown material. Inductively coupled plasma emission spectroscopy analysis is used to confirm the presence of Na element in the sample. Thermal analysis of the NaAP crystal shows that the crystal is stable up to 140°C. Optical transmittance of the grown crystal was recorded in the wavelength range from 200 and 800 nm using UV-Vis-NIR spectrophotometer. The second harmonic generation of NaAP was analysed using Kurtz powder technique.

The improved scintillation crystal lead tungstate scintillation for PET

NASA Astrophysics Data System (ADS)

Wan, Youbao; WU, Rurong; Xiao, Linrong; Zhang, Jianxin; Yang, Peizhi; Yan, Hui

2009-07-01

As a valuable material for the detecting of γ-ray, PbWO4 and BaF2:PbWO4 crystals were grown by a novel multi-crucible temperature gradient system developed by ourselves. Utilizing a topical partial heating method, this system can form a topical partial high temperature in its hearth. Thus this system could melt raw materials in step by step as requirement. The advantage of this method is that there would be solid obstruct left on the melt in the procedure of the crystal growing up. The left obstruct could prevent the volatilization of the component in the melt. Hence it is helpful for the composition homogenization in the crystal. The system also offers a sustaining device for multi-crucibles and thus it can grow many crystals simultaneity. The optical properties and scintillation properties of the crystals were studied. The results reveal that the ions doping improves the scintillation properties of the crystal. The transmittance spectra show that the transmittance of BaF2:PbWO4 crystals are better than that of PbWO4 crystals. For the PbWO4 crystals, their absorption edge is at 325nm, and their maximum transmittance is 68%. For the BaF2:PbWO4 crystals, their absorption edge is at 325nm and their maximum transmittance is upto76%. The X-ray excited luminescence spectra shows that the luminescence peak is at 420nm for the samples of PbWO4 crystal while the peak is at 430nm for the samples of BaF2:PbWO4 crystal respectively. The luminescence intensity of the samples of BaF2:PbWO4 crystal is about two times than that of PbWO4 crystal. And their peak shape is different for the two kind of crystal. The light yield of BaF2:PbWO4 crystals is about 2.9 times than that of PbWO4 crystal Analyzing these scintillation properties, we find that the VPb 3+ and VO- defects do harm for the optical properties of the crystal. Ions doping method could reduce the defect concentration and improving its illumination performance of the crystal. Specially, the doped F- ions in O2- site can induce the aberrance of the [WO4]2- tetrahedron and form [WO3F]- tetrahedron which has more active blue light yield, thus improve the light yield of the crystal. The improved light yield of BaF2:PbWO4 crystals is valuable for the medical diagnosing instrument PET and CT with high resolving power

Apoferritin crystals

NASA Technical Reports Server (NTRS)

2001-01-01

Dr. Alexander Chernov, of the Universities Space Research Association (USRA) and based at Marshall Space Flight Center, is investigating why protein crystals grown in space are, in about 20 percent of cases, better-ordered than those grown on the ground. They are testing the idea that the amount of impurities trapped by space-grown crystals may be different than the amount trapped by crystals grown on Earth because convection is negligible in microgravity. The concentrations or impurities in many space-grown crystals turned out to be several times lower than that in the terrestrial ones, sometimes below the detection limit. The ground-based experiment also showed that the amount of impurities per unit volume of the crystals was usually higher than the amount per unit volume of the solution. This means that a growing crystal actually purifies the solution in its immediate vicinity. Here, an impurity depletion zone is created around apoferritin crystals grown in gel, imitating microgravity conditions.

Passive particle dosimetry. [silver halide crystal growth

NASA Technical Reports Server (NTRS)

Childs, C. B.

1977-01-01

Present methods of dosimetry are reviewed with emphasis on the processes using silver chloride crystals for ionizing particle dosimetry. Differences between the ability of various crystals to record ionizing particle paths are directly related to impurities in the range of a few ppm (parts per million). To understand the roles of these impurities in the process, a method for consistent production of high purity silver chloride, and silver bromide was developed which yields silver halides with detectable impurity content less than 1 ppm. This high purity silver chloride was used in growing crystals with controlled doping. Crystals were grown by both the Czochalski method and the Bridgman method, and the Bridgman grown crystals were used for the experiments discussed. The distribution coefficients of ten divalent cations were determined for the Bridgman crystals. The best dosimeters were made with silver chloride crystals containing 5 to 10 ppm of lead; other impurities tested did not produce proper dosimeters.

Unique Crystallization of Fullerenes: Fullerene Flowers

PubMed Central

Kim, Jungah; Park, Chibeom; Song, Intek; Lee, Minkyung; Kim, Hyungki; Choi, Hee Cheul

2016-01-01

Solution-phase crystallization of fullerene molecules strongly depends on the types of solvent and their ratios because solvent molecules are easily included in the crystal lattice and distort its structure. The C70 (solute)–mesitylene (solvent) system yields crystals with various morphologies and structures, such as cubes, tubes, and imperfect rods. Herein, using C60 and C70 dissolved in mesitylene, we present a novel way to grow unique flower-shaped crystals with six symmetric petals. The different solubility of C60 and C70 in mesitylene promotes nucleation of C70 with sixfold symmetry in the early stage, which is followed by co-crystallization of both C60 and C70 molecules, leading to lateral petal growth. Based on the growth mechanism, we obtained more complex fullerene crystals, such as multi-deck flowers and tube-flower complexes, by changing the sequence and parameters of crystallization. PMID:27561446

Polycrystalline semiconductor processing

DOEpatents

Glaeser, Andreas M.; Haggerty, John S.; Danforth, Stephen C.

1983-01-01

A process for forming large-grain polycrystalline films from amorphous films for use as photovoltaic devices. The process operates on the amorphous film and uses the driving force inherent to the transition from the amorphous state to the crystalline state as the force which drives the grain growth process. The resultant polycrystalline film is characterized by a grain size that is greater than the thickness of the film. A thin amorphous film is deposited on a substrate. The formation of a plurality of crystalline embryos is induced in the amorphous film at predetermined spaced apart locations and nucleation is inhibited elsewhere in the film. The crystalline embryos are caused to grow in the amorphous film, without further nucleation occurring in the film, until the growth of the embryos is halted by imgingement on adjacently growing embryos. The process is applicable to both batch and continuous processing techniques. In either type of process, the thin amorphous film is sequentially doped with p and n type dopants. Doping is effected either before or after the formation and growth of the crystalline embryos in the amorphous film, or during a continuously proceeding crystallization step.

Polycrystalline semiconductor processing

DOEpatents

Glaeser, A.M.; Haggerty, J.S.; Danforth, S.C.

1983-04-05

A process is described for forming large-grain polycrystalline films from amorphous films for use as photovoltaic devices. The process operates on the amorphous film and uses the driving force inherent to the transition from the amorphous state to the crystalline state as the force which drives the grain growth process. The resultant polycrystalline film is characterized by a grain size that is greater than the thickness of the film. A thin amorphous film is deposited on a substrate. The formation of a plurality of crystalline embryos is induced in the amorphous film at predetermined spaced apart locations and nucleation is inhibited elsewhere in the film. The crystalline embryos are caused to grow in the amorphous film, without further nucleation occurring in the film, until the growth of the embryos is halted by impingement on adjacently growing embryos. The process is applicable to both batch and continuous processing techniques. In either type of process, the thin amorphous film is sequentially doped with p and n type dopants. Doping is effected either before or after the formation and growth of the crystalline embryos in the amorphous film, or during a continuously proceeding crystallization step. 10 figs.

The Complete Reconfiguration of Dendritic Gold

NASA Astrophysics Data System (ADS)

Paneru, Govind; Flanders, Bret

2014-03-01

Reconfigurability-by-design is an important strategy in modern materials science, as materials with this capability could potentially be used to confer hydrophobic, lipophobic, or anti-corrosive character to substrates in a regenerative manner. The present work extends the directed electrochemical nanowire assembly (DENA) methodology, which is a technique that employs alternating voltages to grow single crystalline metallic nanowires and nano-dendrites from simple salt solutions, to enable the complete dissolution of macroscopic arrays of metallic dendrites following their growth. Our main finding is that structural reconfiguration of dendritic gold is induced by changes in the MHz-level frequencies of voltages that are applied to the dendrites. Cyclic voltammetry and micro-Raman spectroscopy have been used to show that dendritic gold grows and dissolves by the same chemical mechanisms as bulk gold. Hence, the redox chemistry that occurs at the crystal-solution interface is no different than the established electrochemistry of gold. What differs in this process and allows for reconfiguration to occur is the diffusive behavior of the gold chloride molecules in the solution adjacent to the interface. We will present a simple model that captures the physics of this behavior.

EPR investigation of electronic excitations in rare gas solids (Review Article)

NASA Astrophysics Data System (ADS)

Zhitnikov, R. A.; Dmitriev, Yu. A.

1998-10-01

The methods are described for producing unstable paramagnetic excited states in rare gas cryocrystals Ne, Ar, Kr, and Xe through the trapping, in the cryocrystals growing from the gas phase, the products of the gas discharge taking place in the same or other rare gas. The paper presents a technique and results of an observation and investigation of excited states in rare gas cryocrystals with electron paramagnetic resonance (EPR). The discovered unstable paramagnetic centers are interpreted as being local metastable excited np5(n+1)s atomic-type states in rare gas cryocrystals which are subject to the action of the anisotropic electric field resulted from the crystal surroundings distorted by the center. An account is given of the mechanisms for formation of observed paramagnetic excited states in cryocrystals which arise owing to the excitation energy of the metastable 3P2 atoms of Ne, Ar, Kr, Xe and He 23S1 and 21S0 atoms that form in the discharge in an appropriate gas and trap in the growing cryocrystal.

Growth, structural, spectral, mechanical, thermal and dielectric characterization of phosphoric acid admixtured L-alanine (PLA) single crystals.

PubMed

Rose, A S J Lucia; Selvarajan, P; Perumal, S

2011-10-15

Phosphoric acid admixtured L-alanine (PLA) single crystals were grown successfully by solution method with slow evaporation technique at room temperature. Crystals of size 18 mm×12 mm×8 mm have been obtained in 28 days. The grown crystals were colorless and transparent. The solubility of the grown samples has been found out at various temperatures. The lattice parameters of the grown crystals were determined by X-ray diffraction technique. The reflection planes of the sample were confirmed by the powder X-ray diffraction study and diffraction peaks were indexed. Fourier transform infrared (FTIR) studies were used to confirm the presence of various functional groups in the crystals. UV-visible transmittance spectrum was recorded to study the optical transparency of grown crystal. The nonlinear optical (NLO) property of the grown crystal was confirmed by Kurtz-Perry powder technique and a study of its second harmonic generation efficiency in comparison with potassium dihydrogen phosphate (KDP) has been made. The mechanical strength of the crystal was estimated by Vickers hardness test. The grown crystals were subjected to thermo gravimetric and differential thermal analysis (TG/DTA). The dielectric behavior of the sample was also studied. Copyright © 2011 Elsevier B.V. All rights reserved.

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.

Melting of α'- and α-crystals of poly(lactic acid)

NASA Astrophysics Data System (ADS)

Di Lorenzo, Maria Laura; Androsch, René

2016-05-01

The influence of chain structure on thermal stability of α'-crystals of poly(lactic acid) (PLA) with high L-lactic acid content (96-100 %) is detailed in this contribution. α'-crystals of PLA grow at temperatures below 120 °C, and spontaneously transform into stable α-modification during heating. Using conventional differential scanning calorimetry (DSC) and fast scanning chip calorimetry (FSC), a wide range of scanning rates, between about 10-1 and 102 K s-1 could be tested. It was found that reorganization of disordered α'-crystals into stable α-crystals can be suppressed by fast heating. The critical heating rate needed to completely melt α'-crystals and to avoid formation of α-crystals on continuation of heating varies with the chain composition, and decreases upon increase of the D-lactic acid content in the PLA chain.

Selecting Temperature for Protein Crystallization Screens Using the Temperature Dependence of the Second Virial Coefficient

PubMed Central

Liu, Jun; Yin, Da-Chuan; Guo, Yun-Zhu; Wang, Xi-Kai; Xie, Si-Xiao; Lu, Qin-Qin; Liu, Yong-Ming

2011-01-01

Protein crystals usually grow at a preferable temperature which is however not known for a new protein. This paper reports a new approach for determination of favorable crystallization temperature, which can be adopted to facilitate the crystallization screening process. By taking advantage of the correlation between the temperature dependence of the second virial coefficient (B 22) and the solubility of protein, we measured the temperature dependence of B 22 to predict the temperature dependence of the solubility. Using information about solubility versus temperature, a preferred crystallization temperature can be proposed. If B 22 is a positive function of the temperature, a lower crystallization temperature is recommended; if B 22 shows opposite behavior with respect to the temperature, a higher crystallization temperature is preferred. Otherwise, any temperature in the tested range can be used. PMID:21479212

Experimental cocrystal screening and solution based scale-up cocrystallization methods.

PubMed

Malamatari, Maria; Ross, Steven A; Douroumis, Dennis; Velaga, Sitaram P

2017-08-01

Cocrystals are crystalline single phase materials composed of two or more different molecular and/or ionic compounds generally in a stoichiometric ratio which are neither solvates nor simple salts. If one of the components is an active pharmaceutical ingredient (API), the term pharmaceutical cocrystal is often used. There is a growing interest among drug development scientists in exploring cocrystals, as means to address physicochemical, biopharmaceutical and mechanical properties and expand solid form diversity of the API. Conventionally, coformers are selected based on crystal engineering principles, and the equimolar mixtures of API and coformers are subjected to solution-based crystallization that are commonly employed in polymorph and salt screening. However, the availability of new knowledge on cocrystal phase behaviour in solid state and solutions has spurred the development and implementation of more rational experimental cocrystal screening as well as scale-up methods. This review aims to provide overview of commonly employed solid form screening techniques in drug development with an emphasis on cocrystal screening methodologies. The latest developments in understanding and the use of cocrystal phase diagrams in both screening and solution based scale-up methods are also presented. Final section is devoted to reviewing the state of the art research covering solution based scale-up cocrystallization process for different cocrystals besides more recent continuous crystallization methods. Copyright © 2017 Elsevier B.V. All rights reserved.

Controlled Growth of Large-Area Aligned Single-Crystalline Organic Nanoribbon Arrays for Transistors and Light-Emitting Diodes Driving

NASA Astrophysics Data System (ADS)

Wang, Wei; Wang, Liang; Dai, Gaole; Deng, Wei; Zhang, Xiujuan; Jie, Jiansheng; Zhang, Xiaohong

2017-10-01

Organic field-effect transistors (OFETs) based on organic micro-/nanocrystals have been widely reported with charge carrier mobility exceeding 1.0 cm2 V-1 s-1, demonstrating great potential for high-performance, low-cost organic electronic applications. However, fabrication of large-area organic micro-/nanocrystal arrays with consistent crystal growth direction has posed a significant technical challenge. Here, we describe a solution-processed dip-coating technique to grow large-area, aligned 9,10-bis(phenylethynyl) anthracene (BPEA) and 6,13-bis(triisopropylsilylethynyl) pentacene (TIPS-PEN) single-crystalline nanoribbon arrays. The method is scalable to a 5 × 10 cm2 wafer substrate, with around 60% of the wafer surface covered by aligned crystals. The quality of crystals can be easily controlled by tuning the dip-coating speed. Furthermore, OFETs based on well-aligned BPEA and TIPS-PEN single-crystalline nanoribbons were constructed. By optimizing channel lengths and using appropriate metallic electrodes, the BPEA and TIPS-PEN-based OFETs showed hole mobility exceeding 2.0 cm2 V-1 s-1 (average mobility 1.2 cm2 V-1 s-1) and 3.0 cm2 V-1 s-1 (average mobility 2.0 cm2 V-1 s-1), respectively. They both have a high on/off ratio ( I on/ I off) > 109. The performance can well satisfy the requirements for light-emitting diodes driving.

Crystal-to-glass-transition induced elastic anomaly of cerium-iron multilayer films and texture-related mechanical properties after hydrogenation

NASA Astrophysics Data System (ADS)

Hassdorf, R.; Arend, M.; Felsch, W.

1995-04-01

The flexural modulus EF of pure and hydrided cerium-iron multilayer films has been measured at 300 K as a function of the modulation wavelength Λ using a vibrating-reed technique. EF is strongly correlated to the structure of the layered systems. In the pure Ce/Fe multilayers, the Fe sublayers show a structural transition from an amorphous to the bcc crystalline phase for a thickness near 20 Å. At this transition, the modulus EF is reduced by ~70%. The elastic softening occurs already, as a precursor to the structural change, for the crystalline Fe sublayers somewhat above the thickness for amorphous growth. This behavior reveals close similarities to the crystal-to-glass transition in bulk metallic alloys and compounds which seems to be driven by a shear instability of the crystal lattice. Hydrogenation leads to multilayers built of CeH~2/Fe. The Fe sublayers grow in the bcc structure above 10 Å, with a pronounced (110) or (111) texture for low- or room-temperature deposition. The flexural moduli are larger as compared to the nonhydrided multilayers and distinctly different for the two Fe textures. A simple calculation shows that the texture-related differences mainly result from the bulk properties of the Fe layers, but a contribution of interfacial effects cannot be excluded.

In situ diagnostics of the crystal-growth process through neutron imaging: application to scintillators

DOE PAGES

Tremsin, Anton S.; Makowska, Małgorzata G.; Perrodin, Didier; ...

2016-04-12

Neutrons are known to be unique probes in situations where other types of radiation fail to penetrate samples and their surrounding structures. In this paper it is demonstrated how thermal and cold neutron radiography can provide time-resolved imaging of materials while they are being processed (e.g.while growing single crystals). The processing equipment, in this case furnaces, and the scintillator materials are opaque to conventional X-ray interrogation techniques. The distribution of the europium activator within a BaBrCl:Eu scintillator (0.1 and 0.5% nominal doping concentrations per mole) is studiedin situduring the melting and solidification processes with a temporal resolution of 5–7 s.more » The strong tendency of the Eu dopant to segregate during the solidification process is observed in repeated cycles, with Eu forming clusters on multiple length scales (only for clusters larger than ~50 µm, as limited by the resolution of the present experiments). It is also demonstrated that the dopant concentration can be quantified even for very low concentration levels (~0.1%) in 10 mm thick samples. The interface between the solid and liquid phases can also be imaged, provided there is a sufficient change in concentration of one of the elements with a sufficient neutron attenuation cross section. Tomographic imaging of the BaBrCl:0.1%Eu sample reveals a strong correlation between crystal fractures and Eu-deficient clusters. The results of these experiments demonstrate the unique capabilities of neutron imaging forin situdiagnostics and the optimization of crystal-growth procedures.« less

High Thermal Rectifications Using Liquid Crystals Confined into a Conical Frustum

NASA Astrophysics Data System (ADS)

Silva, José Guilherme; Fumeron, Sébastien; Moraes, Fernando; Pereira, Erms

2018-05-01

In recent years, phononics, that studies thermal analogs of electronic devices, has become an important subject due to the need for better use of energy resources influenced by growing demand. On developing of these analogs, for example, thermal diodes, a successful route is the design of nanostructured materials (e.g., carbon nanotubes). However, these materials entail increased costs due to the use of complex techniques/equipments, while alternative cheaper materials present nearly comparable efficiency. In this work, we investigate how a thermal diode made by an alternative material (nematic liquid crystal), confined in a conical frustum capillary, can be optimized to achieve high rectifications. In such capillary tube, the thermotropic nematic liquid crystal 5CB produces an axially anisotropic defect called escaped radial disclination. With the molecular director field of such structure, we obtain the thermal conductivity tensor of the diode and solve the steady-state regime of Laplace and Fourier equations using the finite element method. We observed the anisotropy of the system with the non-linear temperature dependences of the molecular thermal conductivities that rectify the heat flux at rates up to 1266% at room temperature. Studying the sensitivity of the system with respect to shape and molecular and thermal aspects, we found that the improved thermal diode is suitable to be miniaturized and applied on well-determined areas, and it is robust against variations of the inward pumped heat flux. This work contributes to the usage of liquid crystals in non-display devices, having potential applications on controlling the heat flux through surfaces.

High-throughput determination of structural phase diagram and constituent phases using GRENDEL

NASA Astrophysics Data System (ADS)

Kusne, A. G.; Keller, D.; Anderson, A.; Zaban, A.; Takeuchi, I.

2015-11-01

Advances in high-throughput materials fabrication and characterization techniques have resulted in faster rates of data collection and rapidly growing volumes of experimental data. To convert this mass of information into actionable knowledge of material process-structure-property relationships requires high-throughput data analysis techniques. This work explores the use of the Graph-based endmember extraction and labeling (GRENDEL) algorithm as a high-throughput method for analyzing structural data from combinatorial libraries, specifically, to determine phase diagrams and constituent phases from both x-ray diffraction and Raman spectral data. The GRENDEL algorithm utilizes a set of physical constraints to optimize results and provides a framework by which additional physics-based constraints can be easily incorporated. GRENDEL also permits the integration of database data as shown by the use of critically evaluated data from the Inorganic Crystal Structure Database in the x-ray diffraction data analysis. Also the Sunburst radial tree map is demonstrated as a tool to visualize material structure-property relationships found through graph based analysis.

Crystalline perfection and optical studies of L-Histidinium dihydrogen phosphate orthophosphoric acid (LHDP) single crystals

NASA Astrophysics Data System (ADS)

Ittyachan, Reena; Arunkumar, A.; Bhagavannarayana, G.

2015-10-01

Single crystals of L-Histidinium dihydrogenphosphate orthophosphoric acid (LHDP) were grown by slow evaporation solution growth technique. The grown crystals were confirmed by single crystal X-ray diffraction techniques. The HRXRD rocking curve measurements revealed the crystalline perfection of grown crystal and the absence of structural grain boundaries. The lower optical cut-off wavelength for this crystal was observed at 240 nm. The third order nonlinear refractive index (n2), nonlinear absorption coefficient (β) and susceptibility (χ(3)) were calculated by Z-scan studies using Nd: YAG laser as a source. The single shot laser damage threshold of grown crystal was measured to be 6.286 GW/cm2 using Nd: YAG laser.

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

2006 Global Demilitarization Symposium Volume 1 Presentations

DTIC Science & Technology

2006-05-04

produce inorganic crystals in continuous-reaction mode: Continuous synthesis of CdSe–ZnS composite nanoparticles in a microfluidic reactor, Hongzhi...crystallize lead azide nanoparticles , and to grow them into dextrinated microparticles; Point of Application Microfluidic Synthesis of Sensitive...National Laboratory Point of Application Synthesis of Sensitive Explosive Mr. Karl Wally, Sandia National Laboratories Session III- A Session

Construction of hydrophobic wood surfaces by room temperature deposition of rutile (TiO2) nanostructures

Treesearch

Rongbo Zheng; Mandla A. Tshabalala; Qingyu Li; Hongyan Wang

2015-01-01

A convenient room temperature approach was developed for growing rutile TiO2 hierarchical structures on the wood surface by direct hydrolysis and crystallization of TiCl3 in saturated NaCl aqueous solution.The morphology and the crystal structure of TiO2 coated on the wood surface were characterized...

Asymmetric Die Grows Purer Silicon Ribbon

NASA Technical Reports Server (NTRS)

Kalejs, J. P.; Chalmers, B.; Surek, T.

1983-01-01

Concentration of carbide impurities in silicon ribbon is reduced by growing crystalline ribbon with die one wall higher than other. Height difference controls shape of meniscus at liquid/crystal interface and concentrates silicon carbide impurity near one of broad faces. Opposite face is left with above-average purity. Significantly improves efficiency of solar cells made from ribbon.

Diagnostic of protein crystallization by dynamic light scattering; an application to an aminoacyl-tRNA synthetase

NASA Astrophysics Data System (ADS)

Mikol, Vincent; Vincendon, Pascale; Eriani, Gilbert; Hirsch, Ernest; Giegé, Richard

1991-03-01

The apparent hydrodynamic radius of a truncated form of baker's yeast aspartyl-tRNA synthetase has been measured in various precipitating agent solutions as a function of the protein concentration by dynamic light scattering. In solvents containing ammonium sulfate or 2-methyl-2,4-pentanediol as the precipitating agent the protein remains essentially monodisperse, whereas in the presence of polyethylene glycol interactions and aggregations between protein molecules are detected before reaching supersaturation. These data are indications of possible crystallizations of the protein by the two former precipitants and no crystallization by the latter one. Crystallization experiments indeed have shown that the truncated synthetase crystallizes in the presence of ammonium sulfate and that no crystals grow in solvents containing polyethylene glycol.

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.

Comparison study of PE epitaxy on carbon nanotubes and graphene oxide and PE/graphene oxide as amphiphilic molecular structure for solvent separation

NASA Astrophysics Data System (ADS)

He, Linghao; Zheng, Xiaoli; Xu, Qun; Chen, Zhimin; Fu, Jianwei

2012-03-01

Carbon nanotubes (CNTs) and graphene nanosheets, as one-dimensional and two-dimensional carbon-based nanomaterials respectively, have different abilities to induce the polymer crystallization. In this study, hybrid materials, polyethylene (PE) decorating on CNTs and graphene oxide (GO), were prepared by a facile and efficient method using supercritical carbon dioxide (SC CO2) as anti-solvent. And the morphology and crystallization behavior of PE on CNTs and GO were investigated by transmission electron microscopy, Fourier transform infrared spectroscopy, Raman spectra, wide angle X-ray diffraction, and differential scanning calorimetry. Although both CNTs and GO could act as nucleating agents to induce PE epitaxial growth, CNTs were decorated by PE lamellar crystals forming nanohybrid "shish-kebab" (NHSK) structure, whereas GO sheets were only decorated with petal-like PE crystals. The varying morphologies of the nanohybrids depend on the PE epitaxy and the interactions between polymer chains and substrates. High surface curvature and the perfect ordered crystal structure of CNTs make PE crystals periodically grow on CNTs. While PE crystals grow and form multiple orientation-lamellae on GO due to the lattice matching and complex interactions between PE chains and GO. In addition, our experimental results show an interesting and evident stratification phenomenon for the PE/GO hybrid material, implying that GO decorated by PE have a screening function for the solvents. We anticipate that this work can widen the area of functionalization of carbon-based nanomaterials with a controlled means by an environmentally benign method, which are important for the functional design in nanodevice applications.

Nanoliter-Scale Protein Crystallization and Screening with a Microfluidic Droplet Robot

PubMed Central

Zhu, Ying; Zhu, Li-Na; Guo, Rui; Cui, Heng-Jun; Ye, Sheng; Fang, Qun

2014-01-01

Large-scale screening of hundreds or even thousands of crystallization conditions while with low sample consumption is in urgent need, in current structural biology research. Here we describe a fully-automated droplet robot for nanoliter-scale crystallization screening that combines the advantages of both automated robotics technique for protein crystallization screening and the droplet-based microfluidic technique. A semi-contact dispensing method was developed to achieve flexible, programmable and reliable liquid-handling operations for nanoliter-scale protein crystallization experiments. We applied the droplet robot in large-scale screening of crystallization conditions of five soluble proteins and one membrane protein with 35–96 different crystallization conditions, study of volume effects on protein crystallization, and determination of phase diagrams of two proteins. The volume for each droplet reactor is only ca. 4–8 nL. The protein consumption significantly reduces 50–500 fold compared with current crystallization stations. PMID:24854085

Nanoliter-scale protein crystallization and screening with a microfluidic droplet robot.

PubMed

Zhu, Ying; Zhu, Li-Na; Guo, Rui; Cui, Heng-Jun; Ye, Sheng; Fang, Qun

2014-05-23

Large-scale screening of hundreds or even thousands of crystallization conditions while with low sample consumption is in urgent need, in current structural biology research. Here we describe a fully-automated droplet robot for nanoliter-scale crystallization screening that combines the advantages of both automated robotics technique for protein crystallization screening and the droplet-based microfluidic technique. A semi-contact dispensing method was developed to achieve flexible, programmable and reliable liquid-handling operations for nanoliter-scale protein crystallization experiments. We applied the droplet robot in large-scale screening of crystallization conditions of five soluble proteins and one membrane protein with 35-96 different crystallization conditions, study of volume effects on protein crystallization, and determination of phase diagrams of two proteins. The volume for each droplet reactor is only ca. 4-8 nL. The protein consumption significantly reduces 50-500 fold compared with current crystallization stations.

Solid-state reaction kinetics and optical studies of cadmium doped magnesium hydrogen phosphate crystals

NASA Astrophysics Data System (ADS)

Verma, Madhu; Gupta, Rashmi; Singh, Harjinder; Bamzai, K. K.

2018-04-01

The growth of cadmium doped magnesium hydrogen phosphate was successfully carried out by using room temperature solution technique i.e., gel encapsulation technique. Grown crystals were confirmed by single crystal X-ray diffraction (XRD). The structure of the grown crystal belongs to orthorhombic crystal system and crystallizes in centrosymmetric space group. Kinetics of the decomposition of the grown crystals were studied by non-isothermal analysis. Thermo gravimetric / differential thermo analytical (TG/DTA) studies revealed that the grown crystal is stable upto 119 °C. The various steps involved in the thermal decomposition of the material have been analysed using Horowitz-Metzger, Coats-Redfern and Piloyan-Novikova equations for evaluating various kinetic parameters. The optical studies shows that the grown crystals possess wide transmittance in the visible region and significant optical band gap of 5.5ev with cut off wavelength of 260 nm.

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.

A Few Good Crystals Please

NASA Technical Reports Server (NTRS)

Judge, Russell A.; Snell, Edward H.

1999-01-01

Part of the challenge of macromolecular crystal growth for structure determination is obtaining an appropriate number of crystals with a crystal volume suitable for X-ray analysis. In this respect an understanding of the effect of solution conditions on macromolecule nucleation rates is advantageous. This study investigated the effects of solution conditions on the nucleation rate and final crystal size of two crystal systems; tetragonal lysozyme and glucose isomerase. Batch crystallization plates were prepared at given solution concentration and incubated at set temperatures over one week. The number of crystals per well with their size and axial ratios were recorded and correlated with solution conditions. Duplicate experiments indicate the reproducibility of the technique. Results for each system showing the effect of supersaturation, incubation temperature and solution pH on nucleation rates will be presented and discussed. In the case of lysozyme, having optimized solution conditions to produce an appropriate number of crystals of a suitable size, a batch of crystals were prepared under exactly the same conditions. Fifty of these crystals were analyzed by x-ray techniques. The results indicate that even under the same crystallization conditions, a marked variation in crystal properties exists.

Synthesis, structural, optical and thermal properties of N-methyl-N-aryl benzamide organic single crystals grown by a slow evaporation technique

NASA Astrophysics Data System (ADS)

Prabukanthan, P.; Lakshmi, R.; Harichandran, G.; Kumar, C. Sudarsana

2018-03-01

The organic materials, N-methyl-N-aryl benzamides were synthesized from benzoylation of N-methyl-4-nitrobenzenamine (MNBA) using suitably substituted benzoyl chlorides. The products were purified by recrystallization and their single crystal were grown by a slow evaporation technique. The crystals were characterized by FTIR, UV-Vis-NIR, 1H &13C NMR, and single & powder X-ray diffraction. Thermal stability of the crystals was studied by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Dielectric and NLO properties of MNPB, FMNPB and MMNPB crystals were studied. The second harmonic generation (SHG) has been confirmed by the Kurtz powder test for all these crystals and the SHG efficiency of MMNPB crystal was found to be 2.25 times higher than that of KDP crystal.

Crucibleless crystal growth and Radioluminescence study of calcium tungstate single crystal fiber

NASA Astrophysics Data System (ADS)

Silva, M. S.; Jesus, L. M.; Barbosa, L. B.; Ardila, D. R.; Andreeta, J. P.; Silva, R. S.

2014-11-01

In this article, single phase and high optical quality scheelite calcium tungstate single crystal fibers were grown by using the crucibleless laser heated pedestal growth technique. The as-synthesized calcium tungstate powders used for shaping seed and feed rods were investigated by X-ray diffraction technique. As-grown crystals were studied by Raman spectroscopy and Radioluminescence measurements. The results indicate that in both two cases, calcined powder and single crystal fiber, only the expected scheelite CaWO4 phase was observed. It was verified large homogeneity in the crystal composition, without the presence of secondary phases. The Radioluminescence spectra of the as-grown single crystal fibers are in agreement with that present in Literature for bulk single crystals, presented a single emission band centered at 420 nm when irradiated with β-rays.

Structural and optical properties of WTe2 single crystals synthesized by DVT technique

NASA Astrophysics Data System (ADS)

Dixit, Vijay; Vyas, Chirag; Pathak, V. M.; Soalanki, G. K.; Patel, K. D.

2018-05-01

Layered transition metal di-chalcogenide (LTMDCs) crystals have attracted much attention due to their potential in optoelectronic device applications recently due to realization of their monolayer based structures. In the present investigation we report growth of WTe2 single crystals by direct vapor transport (DVT) technique. These crystals are then characterized by energy dispersive analysis of x-rays (EDAX) to study stoichiometric composition after growth. The structural properties are studied by x-ray diffraction (XRD) and selected area electron diffraction (SAED) is used to confirm orthorhombic structure of grown WTe2 crystal. Surface morphological properties of the crystals are also studied by scanning electron microscope (SEM). The optical properties of the grown crystals are studied by UV-Visible spectroscopy which gives direct band gap of 1.44 eV for grown WTe2 single crystals.

An overview of heavy-atom derivatization of protein crystals

PubMed Central

Pike, Ashley C. W.; Garman, Elspeth F.; Krojer, Tobias; von Delft, Frank; Carpenter, Elisabeth P.

2016-01-01

Heavy-atom derivatization is one of the oldest techniques for obtaining phase information for protein crystals and, although it is no longer the first choice, it remains a useful technique for obtaining phases for unknown structures and for low-resolution data sets. It is also valuable for confirming the chain trace in low-resolution electron-density maps. This overview provides a summary of the technique and is aimed at first-time users of the method. It includes guidelines on when to use it, which heavy atoms are most likely to work, how to prepare heavy-atom solutions, how to derivatize crystals and how to determine whether a crystal is in fact a derivative. PMID:26960118

Crystallization and preliminary X-ray diffraction study of recombinant ribokinase from Thermus Species 2.9

NASA Astrophysics Data System (ADS)

Abramchik, Yu. A.; Timofeev, V. I.; Muravieva, T. I.; Esipov, R. S.; Kuranova, I. P.

2016-11-01

Ribokinase from a thermophilic strain of Thermus species 2.9 belonging to the carbohydrate ribokinase family (EC 2.7.1.15) was isolated, purified, and crystallized. The crystallization conditions were found by the vapor-diffusion technique and were then optimized to apply the capillary counter-diffusion technique. The X-ray diffraction data set was collected from the crystals, which were grown by the counter-diffusion technique, at the SPring-8 synchrotron radiation facility to 2.87 Å resolution. The crystals belong to sp. gr. P1211 and have the following unit-cell parameters: a = 81.613 Å, b = 156.132 Å, c = 87.714 Å, α = γ = 90°, β = 103.819°. The X-ray diffraction data set is suitable for determining the three-dimensional structure of the protein by the molecular-replacement method.

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.

Crystal growth, structural, low temperature thermoluminescence and mechanical properties of cubic fluoroperovskite single crystal (LiBaF3)

NASA Astrophysics Data System (ADS)

Daniel, D. Joseph; Ramasamy, P.; Ramaseshan, R.; Kim, H. J.; Kim, Sunghwan; Bhagavannarayana, G.; Cheon, Jong-Kyu

2017-10-01

Polycrystalline compounds of LiBaF3 were synthesized using conventional solid state reaction route and the phase purity was confirmed using powder X-ray diffraction technique. Using vertical Bridgman technique single crystal was grown from melt. Rocking curve measurements have been carried out to study the structural perfection of the grown crystal. The single peak of diffraction curve clearly reveals that the grown crystal was free from the structural grain boundaries. The low temperature thermoluminescence of the X-ray irradiated sample has been analyzed and found four distinguishable peaks having maximum temperatures at 18, 115, 133 and 216 K. Activation energy (E) and frequency factor (s) for the individual peaks have been studied using Peak shape method and the computerized curve fitting method combining with the Tmax- TStop procedure. Nanoindentation technique was employed to study the mechanical behaviour of the crystal. The indentation modulus and Vickers hardness of the grown crystal have values of 135.15 GPa and 680.81 respectively, under the maximum indentation load of 10 mN.

Polymer-directed crystallization of atorvastatin.

PubMed

Choi, Hyemin; Lee, Hyeseung; Lee, Min Kyung; Lee, Jonghwi

2012-08-01

Living organisms secrete minerals composed of peptides and proteins, resulting in "mesocrystals" of three-dimensional-assembled composite structures. Recently, this biomimetic polymer-directed crystallization technique has been widely applied to inorganic materials, although it has seldom been used with drugs. In this study, the technique was applied to the drowning-out crystallization of atorvastatin using various polymers. Nucleation and growth at optimized conditions successfully produced composite crystals with significant polymer contents and unusual characteristics. Atorvastatin composite crystals containing polyethylene glycol, polyacrylic acid, polyethylene imine, and chitosan showed a markedly decreased melting point and heat of fusion, improved stability, and sustained-release patterns. The use of hydroxypropyl cellulose yielded a unique combination of enhanced in vitro release and improved drug stability under a forced degradation condition. The formation hypothesis of unique mesocrystal structures was strongly supported by an X-ray diffraction pattern and substantial melting point reduction. This polymer-directed crystallization technique offers a novel and effective way, different from the solid dispersion approach, to engineer the release, stability, and processability of drug crystals. Copyright © 2012 Wiley Periodicals, Inc.

Synthesis, growth, structural, optical, luminescence, surface and HOMO LUMO analysis of 2-[2-(4-cholro-phenyl)-vinyl]-1-methylquinolinium naphthalene-2-sulfonate organic single crystals grown by a slow evaporation technique

NASA Astrophysics Data System (ADS)

Karthigha, S.; Kalainathan, S.; Maheswara Rao, Kunda Uma; Hamada, Fumio; Yamada, Manabu; Kondo, Yoshihiko

2016-02-01

Single crystals of 2-[2-(4-cholro-phenyl)-vinyl]-1-methylquinolinium naphthalene-2-sulfonate (4CLNS) were grown by a slow evaporation technique. The formation of molecule was confirmed from 1H NMR and FTIR analysis. The confirmation of crystal structure was done by single crystal XRD and atomic packing of grown crystal was identified. The grown single crystal crystallized in triclinic structure with centrosymmetric space group P-1. The crystalline nature of the synthesised material was recorded by powder XRD. The optical absorption properties of the grown crystals were analyzed by UV-vis spectral studies. The thermal behaviour of the title material has been studied by TG/DTA analysis which revealed the stability of the compound till its melting point 276.7 °C. The third order nonlinear optical property of 4CLNS was investigated in detail by Z scan technique and it confirms that the title crystal is suitable for photonic devices and NLO optical applications. Emissions at 519 nm in green region of the EM spectrum were found by photoluminescence studies. The charge transfer occurring within the molecule is explained by the calculated HOMO and LUMO energies.

Bread board float zone experiment system for high purity silicon

NASA Technical Reports Server (NTRS)

Kern, E. L.; Gill, G. L., Jr.

1982-01-01

A breadboard float zone experimental system has been established at Westech Systems for use by NASA in the float zone experimental area. A used zoner of suitable size and flexibility was acquired and installed with the necessary utilities. Repairs, alignments and modifications were made to provide for dislocation free zoning of silicon. The zoner is capable of studying process parameters used in growing silicon in gravity and is flexible to allow trying of new features that will test concepts of zoning in microgravity. Characterizing the state of the art molten zones of a growing silicon crystal will establish the data base against which improvements of zoning in gravity or growing in microgravity can be compared. 25 mm diameter was chosen as the reference size, since growth in microgravity will be at that diameter or smaller for about the next 6 years. Dislocation free crystals were growtn in the 100 and 111 orientations, using a wide set of growth conditions. The zone shape at one set of conditions was measured, by simultaneously aluminum doping and freezing the zone, lengthwise slabbing and delineating by etching. The whole set of crystals, grown under various conditions, were slabbed, polished and striation etched, revealing the growth interface shape and the periodic and aperiodic natures of the striations.

A Theory of the von Weimarn Rules Governing the Average Size of Crystals Precipitated from a Supersaturated Solution

NASA Technical Reports Server (NTRS)

Barlow, Douglas A.; Baird, James K.; Su, Ching-Hua

2003-01-01

More than 75 years ago, von Weimarn summarized his observations of the dependence of the average crystal size on the initial relative concentration supersaturation prevailing in a solution from which crystals were growing. Since then, his empirically derived rules have become part of the lore of crystal growth. The first of these rules asserts that the average crystal size measured at the end of a crystallization increases as the initial value of the relative supersaturation decreases. The second rule states that for a given crystallization time, the average crystal size passes through a maximum as a function of the initial relative supersaturation. Using a theory of nucleation and growth due to Buyevich and Mansurov, we calculate the average crystal size as a function of the initial relative supersaturation. We confirm the von Weimarn rules for the case where the nucleation rate is proportional to the third power or higher of the relative supersaturation.

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.

Real-time molecular scale observation of crystal formation.

PubMed

Schreiber, Roy E; Houben, Lothar; Wolf, Sharon G; Leitus, Gregory; Lang, Zhong-Ling; Carbó, Jorge J; Poblet, Josep M; Neumann, Ronny

2017-04-01

How molecules in solution form crystal nuclei, which then grow into large crystals, is a poorly understood phenomenon. The classical mechanism of homogeneous crystal nucleation proceeds via the spontaneous random aggregation of species from liquid or solution. However, a non-classical mechanism suggests the formation of an amorphous dense phase that reorders to form stable crystal nuclei. So far it has remained an experimental challenge to observe the formation of crystal nuclei from five to thirty molecules. Here, using polyoxometallates, we show that the formation of small crystal nuclei is observable by cryogenic transmission electron microscopy. We observe both classical and non-classical nucleation processes, depending on the identity of the cation present. The experiments verify theoretical studies that suggest non-classical nucleation is the lower of the two energy pathways. The arrangement in just a seven-molecule proto-crystal matches the order found by X-ray diffraction of a single bulk crystal, which demonstrates that the same structure was formed in each case.

Growth and characterization of organic material 4-dimethylaminobenzaldehyde single crystal.

PubMed

Jebin, R P; Suthan, T; Rajesh, N P; Vinitha, G; Madhusoodhanan, U

2015-01-25

The organic material 4-dimethylaminobenzaldehyde single crystals were grown by slow evaporation technique. The grown crystal was confirmed by the single crystal and powder X-ray diffraction analyses. The functional groups of the crystal have been identified from the Fourier Transform Infrared (FTIR) and FT-Raman studies. The optical property of the grown crystal was analyzed by UV-Vis-NIR and photoluminescence (PL) spectral measurements. The thermal behavior of the grown crystal was analyzed by thermogravimetric (TG) and differential thermal analyses (DTA). Dielectric measurements were carried out with different frequencies by using parallel plate capacitor method. The third order nonlinear optical properties of 4-dimethylaminobenzaldehyde was measured by the Z-scan technique using 532 nm diode pumped continuous wave (CW) Nd:YAG laser. Copyright © 2014 Elsevier B.V. All rights reserved.

Challenges and Solutions in Fabrication of Silica-Based Photonic Crystal Fibers: An Experimental Study

NASA Astrophysics Data System (ADS)

Amouzad Mahdiraji, G.; Chow, Desmond M.; Sandoghchi, S. R.; Amirkhan, F.; Dermosesian, E.; Shien Yeo, Kwok; Kakaei, Z.; Ghomeishi, M.; Poh, Soo Yong; Gang, Shee Yu; Mahamd Adikan, F. R.

2014-01-01

The fabrication process of photonic crystal fibers based on a stack-and-draw method is presented in full detail in this article. In addition, improved techniques of photonic crystal fiber preform preparation and fabrication are highlighted. A new method of connecting a handle to a preform using only a fiber drawing tower is demonstrated, which eliminates the need for a high-temperature glass working lathe. Also, a new technique of modifying the photonic crystal fiber structural pattern by sealing air holes of the photonic crystal fiber cane is presented. Using the proposed methods, several types of photonic crystal fibers are fabricated, which suggests potential for rapid photonic crystal fibers fabrication in laboratories equipped with and limited to only a fiber drawing tower.

Solution-Phase Processes of Macromolecular Crystallization

NASA Technical Reports Server (NTRS)

Pusey, Marc L.; Minamitani, Elizabeth Forsythe

2004-01-01

We have proposed, for the tetragonal form of chicken egg lysozyme, that solution phase assembly processes are needed to form the growth units for crystal nucleation and growth. The starting point for the self-association process is the monomeric protein, and the final crystallographic symmetry is defined by the initial dimerization interactions of the monomers and subsequent n-mers formed, which in turn are a function of the crystallization conditions. It has been suggested that multimeric proteins generally incorporate the underlying multimers symmetry into the final crystallographic symmetry. We posed the question of what happens to a protein that is known to grow as an n-mer when it is placed in solution conditions where it is monomeric. The trypsin-treated, or cut, form of the protein canavalin (CCAN) has been shown to nucleate and grow crystals as a trimer from neutral to slightly acidic solutions. Under these conditions the solution is composed almost wholly of trimers. The insoluble protein can be readily dissolved by weakly basic solution, which results in a solution that is monomeric. There are three possible outcomes to an attempt at crystallization of the protein under monomeric (high pH) conditions: 1) we will obtain the same crystals as under trimer conditions, but at different protein concentrations governed by the self association equilibria; 2) we will obtain crystals having a different symmetry, based upon a monomeric growth unit; 3) we will not obtain crystals. Obtaining the first result would be indicative that the solution-phase self-association process is critical to the crystal nucleation and growth process. The second result would be less clear, as it may also reflect a pH-dependent shift in the trimer-trimer molecular interactions. The third result, particularly for experiments in the transition pH's between trimeric and monomeric CCAN, would indicate that the monomer does not crystallize, and that solution phase self association is not part of the crystal nucleation and growth path. Results are presented for crystallization experiments of CCAN over the pH 6.8 to 9.6 range.

Microgravity

NASA Image and Video Library

1995-09-12

DCAM, developed by MSFC, grows crystals by the dialysis and liquid-liquid diffusion methods. In both methods, protein crystal growth is induced by changing conditions in the protein. In dialysis, a semipermeable membrane retains the protein solution in one compartment, while allowing molecules of precipitant to pass freely through the membrane from an adjacent compartment. As the precipitant concentration increases within the protein compartment, crystallization begins. In liquid-liquid diffusion, a protein solution and a precipitant solution are layered in a container and allowed to diffuse into each other. This leads to conditions which may induce crystallization of the protein. Liquid-liquid diffusion is difficult on Earth because density and temperature differences cause the solutions to mix rapidly.

Chemo-mechanics of salt damage in stone.

PubMed

Flatt, Robert J; Caruso, Francesco; Sanchez, Asel Maria Aguilar; Scherer, George W

2014-09-11

Many porous materials are damaged by pressure exerted by salt crystals growing in their pores. This is a serious issue in conservation science, geomorphology, geotechnical engineering and concrete materials science. In all cases, a central question is whether crystallization pressure will cause damage. Here we present an experiment in which the crystallization pressure and the pore saturation are varied in a controlled way. We demonstrate that a strain energy failure criterion can be used to predict when damage will occur. The experiment considered is the most widely used means to study the susceptibility to salt crystallization, so quantification of this test has far-reaching implications.

In situ data collection and structure refinement from microcapillary protein crystallization

PubMed Central

Yadav, Maneesh K.; Gerdts, Cory J.; Sanishvili, Ruslan; Smith, Ward W.; Roach, L. Spencer; Ismagilov, Rustem F.; Kuhn, Peter; Stevens, Raymond C.

2007-01-01

In situ X-ray data collection has the potential to eliminate the challenging task of mounting and cryocooling often fragile protein crystals, reducing a major bottleneck in the structure determination process. An apparatus used to grow protein crystals in capillaries and to compare the background X-ray scattering of the components, including thin-walled glass capillaries against Teflon, and various fluorocarbon oils against each other, is described. Using thaumatin as a test case at 1.8 Å resolution, this study demonstrates that high-resolution electron density maps and refined models can be obtained from in situ diffraction of crystals grown in microcapillaries. PMID:17468785

First X-ray crystal structure and internal reference diffusion-ordered NMR spectroscopy study of the prototypical Posner reagent, MeCu(SPh)Li(THF)3.

PubMed

Bertz, Steven H; Hardin, Richard A; Heavey, Thomas J; Jones, Daniel S; Monroe, T Blake; Murphy, Michael D; Ogle, Craig A; Whaley, Tara N

2013-07-29

Grow slow: The usual direct treatment of MeLi and CuSPh did not yield X-ray quality crystals of MeCu(SPh)Li. An indirect method starting from Me2CuLi⋅LiSPh and chalcone afforded the desired crystals by the slow reaction of the intermediate π-complex (see scheme). This strategy produced the first X-ray crystal structure of a Posner cuprate. A complementary NMR study showed that the contact ion pair was also the main species in solution. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Czochralski growth of NaNO3-LiNO3 solid solution single crystals using axial vibrational control technique

NASA Astrophysics Data System (ADS)

Avetissov, Igor; Sadovskiy, Andrei; Belov, Stanislav; Kong Khan, Chan; Mozhevitina, Elena; Sukhanova, Ekaterina; Zharikov, Eugeniy

2014-09-01

T-x diagram of LiNO3-NaNO3 quasi-binary system has been improved using an original technique based on Raman measurements of condense phase. (LiNO3)x(NaNO3)1-x solid solution single crystal has been grown at different regimes of axial vibrational control (AVC) technique. Significant difference in segregation coefficient behavior between AVC-CZ and conventional CZ grown crystals has appeared: with AVC intensity increase the segregation coefficient (SC) raises for light molecular weight elements, SC reduces for medium molecular weight elements, and SC remains practically unchangeable for heavy molecular weight elements. Effect of vibrational intensity on vibron and optical characteristics, microhardness of AVC-CZ (LiNO3)x(NaNO3)1-x solid solution single crystals has been studied. For the AVC-CZ crystals has been observed increases in microhardness as well as in optical transmission up to 10 rel% compare to conventional CZ grown crystals.

Characterization of a bent Laue double-crystal beam-expanding monochromator

DOE PAGES

Martinson, Mercedes; Samadi, Nazanin; Shi, Xianbo; ...

2017-10-19

A bent Laue double-crystal monochromator system has been designed for vertically expanding the X-ray beam at the Canadian Light Source's BioMedical Imaging and Therapy beamlines. Expansion by a factor of 12 has been achieved without deteriorating the transverse coherence of the beam, allowing phase-based imaging techniques to be performed with high flux and a large field of view. However, preliminary studies revealed a lack of uniformity in the beam, presumed to be caused by imperfect bending of the silicon crystal wafers used in the system. Results from finite-element analysis of the system predicted that the second crystal would be mostmore » severely affected and has been shown experimentally. It has been determined that the majority of the distortion occurs in the second crystal and is likely caused by an imperfection in the surface of the bending frame. Here, measurements were then taken to characterize the bending of the crystal using both mechanical and diffraction techniques. In particular, two techniques commonly used to map dislocations in crystal structures have been adapted to map local curvature of the bent crystals. One of these, a variation of Berg–Berrett topography, has been used to quantify the diffraction effects caused by the distortion of the crystal wafer. This technique produces a global mapping of the deviation of the diffraction angle relative to a perfect cylinder. Finally, this information is critical for improving bending and measuring tolerances of imperfections by correlating this mapping to areas of missing intensity in the beam.« less

Characterization of a bent Laue double-crystal beam-expanding monochromator

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

Martinson, Mercedes; Samadi, Nazanin; Shi, Xianbo

A bent Laue double-crystal monochromator system has been designed for vertically expanding the X-ray beam at the Canadian Light Source's BioMedical Imaging and Therapy beamlines. Expansion by a factor of 12 has been achieved without deteriorating the transverse coherence of the beam, allowing phase-based imaging techniques to be performed with high flux and a large field of view. However, preliminary studies revealed a lack of uniformity in the beam, presumed to be caused by imperfect bending of the silicon crystal wafers used in the system. Results from finite-element analysis of the system predicted that the second crystal would be mostmore » severely affected and has been shown experimentally. It has been determined that the majority of the distortion occurs in the second crystal and is likely caused by an imperfection in the surface of the bending frame. Here, measurements were then taken to characterize the bending of the crystal using both mechanical and diffraction techniques. In particular, two techniques commonly used to map dislocations in crystal structures have been adapted to map local curvature of the bent crystals. One of these, a variation of Berg–Berrett topography, has been used to quantify the diffraction effects caused by the distortion of the crystal wafer. This technique produces a global mapping of the deviation of the diffraction angle relative to a perfect cylinder. Finally, this information is critical for improving bending and measuring tolerances of imperfections by correlating this mapping to areas of missing intensity in the beam.« 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.

Comparison of PCR, culturing and Pap smear microscopy for accurate diagnosis of genital Actinomyces.

PubMed

Kaya, Dilek; Demirezen, Şayeste; Hasçelik, Gülşen; Gülmez Kivanç, Dolunay; Beksaç, Mehmet Sinan

2013-05-01

Members of the genus Actinomyces, Gram-positive, non-spore-forming anaerobic bacteria, are normal inhabitants of the mucosal surfaces of the oral, gastrointestinal and genital tracts. Identification of these bacteria using conventional methods is generally difficult because of their complex transport and growth requirements and their fastidious and slow-growing nature. However, in recent years, the advancement of molecular techniques has provided much improved identification and differentiation of closely related Actinomyces species. The aim of the present study was to evaluate the efficacy of the PCR technique in the diagnosis of genital Actinomyces in comparison with culturing and Papanicolaou (Pap) smear microscopy. Multiple sampling was conducted from 200 women using smear microscopy, culturing and PCR. Cyto-brushes were smeared on glass slides and stained using the routine Pap technique. Culturing was performed from a sterile swab, and Actinomyces were determined using the BBL Crystal ANR ID kit. PCR was performed from a second swab, and the Actinomyces type was determined using type-specific primers designed in our laboratory. Only one vaginal fluid sample (0.5%) revealed Actinomyces-like organisms on Pap smear examination. Actinomyces were detected in nine samples (4.5%) using the BBL Crystal ANR ID kit. Using PCR, eight samples (4%) were found positive for Actinomyces. No specimens that gave positive results by Pap smear microscopy and culturing could be confirmed by PCR. Pap smear microscopy and culturing were both found to have zero sensitivity for Actinomyces. PCR appears to be a sensitive and reliable diagnostic method for the detection of Actinomyces, which are difficult to cultivate from genital samples. PCR can be used for diagnostic confirmation in cases diagnosed by conventional methods, to prevent false-positive results.

Applications of thermal-gradients method for the optimization of α-amylase crystallization conditions based on dynamic and static light scattering data

NASA Astrophysics Data System (ADS)

Delboni, L. F.; Iulek, J.; Burger, R.; da Silva, A. C. R.; Moreno, A.

2002-02-01

The expression, purification, crystallization, and characterization by X-ray diffraction of α-amylase are described here. Dynamic and static light scattering methods with a temperature controller was used to optimize the crystallization conditions of α-amylase from Bacillus stearothermophilus an important enzyme in many fields of industrial activity. After applying thermal gradients for growing crystals, X-ray cryo-crystallographic methods were employed for the data collection. Crystals grown by these thermal-gradients diffracted up to a maximum resolution of 3.8 Å, which allowed the determination of the unit cell constants as follows: a=61.7 Å, b=86.7 Å, c=92.2 Å and space group C222 (or C222 1).

Microgravity

NASA Image and Video Library

2001-01-24

Dr. Alexander Chernov, of the Universities Space Research Association (USRA) and based at Marshall Space Flight Center, is investigating why protein crystals grown in space are, in about 20 percent of cases, better-ordered than those grown on the ground. They are testing the idea that the amount of impurities trapped by space-grown crystals may be different than the amount trapped by crystals grown on Earth because convection is negligible in microgravity. The concentrations or impurities in many space-grown crystals turned out to be several times lower than that in the terrestrial ones, sometimes below the detection limit. The ground-based experiment also showed that the amount of impurities per unit volume of the crystals was usually higher than the amount per unit volume of the solution. This means that a growing crystal actually purifies the solution in its immediate vicinity. Here, an impurity depletion zone is created around apoferritin crystals grown in gel, imitating microgravity conditions.

Barium iodide and strontium iodide crystals andd scintillators implementing the same

DOEpatents

Payne, Stephen A; Cherepy, Nerine J; Hull, Giulia E; Drobshoff, Alexander D; Burger, Arnold

2013-11-12

In one embodiment, a material comprises a crystal comprising strontium iodide providing at least 50,000 photons per MeV. A scintillator radiation detector according to another embodiment includes a scintillator optic comprising europium-doped strontium iodide providing at least 50,000 photons per MeV. A scintillator radiation detector in yet another embodiment includes a scintillator optic comprising SrI.sub.2 and BaI.sub.2, wherein a ratio of SrI.sub.2 to BaI.sub.2 is in a range of between 0:1 A method for manufacturing a crystal suitable for use in a scintillator includes mixing strontium iodide-containing crystals with a source of Eu.sup.2+, heating the mixture above a melting point of the strontium iodide-containing crystals, and cooling the heated mixture near the seed crystal for growing a crystal. Additional materials, systems, and methods are presented.

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.

Sequential x-ray diffraction topography at 1-BM x-ray optics testing beamline at the advanced photon source

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

Stoupin, Stanislav, E-mail: sstoupin@aps.anl.gov; Shvyd’ko, Yuri; Trakhtenberg, Emil

2016-07-27

We report progress on implementation and commissioning of sequential X-ray diffraction topography at 1-BM Optics Testing Beamline of the Advanced Photon Source to accommodate growing needs of strain characterization in diffractive crystal optics and other semiconductor single crystals. The setup enables evaluation of strain in single crystals in the nearly-nondispersive double-crystal geometry. Si asymmetric collimator crystals of different crystallographic orientations were designed, fabricated and characterized using in-house capabilities. Imaging the exit beam using digital area detectors permits rapid sequential acquisition of X-ray topographs at different angular positions on the rocking curve of a crystal under investigation. Results on sensitivity andmore » spatial resolution are reported based on experiments with high-quality Si and diamond crystals. The new setup complements laboratory-based X-ray topography capabilities of the Optics group at the Advanced Photon Source.« less

New Techniques in Characterization of Ferroelectric Materials

NASA Technical Reports Server (NTRS)

Sehirlioglu, Alp

2008-01-01

Two new techniques have been developed to characterize Pb(Mg1/3Nb2/3)O3-PbTiO3 (PMN-PT) based ferroelectric single crystals: (i) electro-thermal imaging, and (ii) single crystal x-ray diffraction in the transmission mode. (i) Electro-thermal imaging is a remote sensing technique that can detect the polarization direction and poling state of a whole crystal slice. This imaging technique utilizes an IR camera to determine the field induced temperature change and does not require any special or destructive sample preparation. In the resulting images it is possible to distinguish regions of 180 deg domains. This powerful technique can be used remotely during poling to determine the poling state of the crystal to avoid over-poling that can result in inferior properties and/or cracking of the crystals. Electro-thermal imaging produced the first direct observations of polarization rotation. Under bipolar field, the domains near the corners were the first to switch direction. As the field increased above the coercive field, domains at the center part of the crystals switched direction. (ii) X-ray diffraction in the transmission mode has long been used in structure determination of organic crystals and proteins; however, it is not used much to characterize inorganic systems. 0.7Pb(Mg1/3Nb2/3)O3-0.3PbTiO3 single crystals were examined by this XRD technique for the first time, and a never-before-seen super-lattice was revealed with a doubling of the unit cell in all three directions, giving a cell volume eight times that of a traditional perovskite unit cell. The significance of the super-lattice peaks increased with poling, indicating a structural contribution to ordering. Lack of such observations by electron diffraction in the transmission electron microscope examinations suggests the presence of a bulk effect.

Investigations of structural defects, crystalline perfection, metallic impurity concentration and optical quality of flat-top KDP crystal

NASA Astrophysics Data System (ADS)

Sharma, S. K.; Verma, Sunil; Singh, Yeshpal; Bartwal, K. S.; Tiwari, M. K.; Lodha, G. S.; Bhagavannarayana, G.

2015-08-01

KDP crystal grown using flat-top technique has been characterized using X-ray and optical techniques with the aim of correlating the defects structure and impurity concentration in the crystal with its optical properties. Crystallographic defects were investigated using X-ray topography revealing linear and arc like chains of dislocations and to conclude that defects do not originate from the flat-top part of the crystal. Etching was performed to quantify dislocation defects density. The crystalline perfection of the crystal was found to be high as the FWHM of the rocking curves measured at several locations was consistently low 6-9 arc s. The concentration of Fe metallic impurity quantified using X-ray fluorescence technique was approximately 5 times lower in the flat-top part which falls in pyramidal growth sector as compared to the region near to the seed which lies in prismatic sector. The spectrophotometric characterization for plates cut normal to different crystallographic directions in the flat-top potassium dihydrogen phosphate (FT-KDP) crystal was performed to understand the influence of metallic impurity distribution and growth sectors on the optical transmittance. The transmittance of the FT-KDP crystal at 1064 nm and its higher harmonics (2nd, 3rd, 4th and 5th) was determined from the measured spectra and the lower transmission in the UV region was attributed to increased absorption by Fe metallic impurity at these wavelengths. The results are in agreement with the results obtained using X-ray fluorescence and X-ray topography. Birefringence and Mach-Zehnder interferometry show that except for the region near to the seed crystal the optical homogeneity of the entire crystal was good. The laser-induced damage threshold (LDT) values are in the range 2.4-3.9 GW/cm2. The LDT of the plate taken from the flat-top region is higher than that from the bottom of the crystal, indicating that the flat-top technique has good optical quality and is comparable to those reported using rapid growth technique. The results indicate that the structural defects, crystalline quality and impurity concentration have a correlation with the optical properties of the FT-KDP crystal.