High resolution synchrotron X-radiation diffraction imaging of crystals grown in microgravity and closely related terrestrial crystals

NASA Technical Reports Server (NTRS)

Steiner, Bruce; Dobbyn, Ronald C.; Black, David; Burdette, Harold; Kuriyama, Masao; Fripp, Archibald; Simchik, Richard

1991-01-01

Irregularities in three crystals grown in space and in four terrestrial crystals grown under otherwise comparable conditions have been observed in high resolution diffraction imaging. The images provide important new clues to the nature and origins of irregularities in each crystal. For two of the materials, mercuric iodide and lead tin telluride, more than one phase (an array of non-diffracting inclusions) was observed in terrestrial samples; but the formation of these multiple phases appears to have been suppressed in directly comparable crystals grown in microgravity. The terrestrial seed crystal of triglycine sulfate displayed an unexpected layered structure, which propagated during directly comparable space growth. Terrestrial Bridgman regrowth of gallium arsenide revealed a mesoscopic structure substantially different from that of the original Czochralski material. A directly comparable crystal is to be grown shortly in space.

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).

Solution-Grown Rubrene Crystals as Radiation Detecting Devices

DOE PAGES

Carman, Leslie; Martinez, H. Paul; Voss, Lars; ...

2017-01-11

There has been increased interest in organic semiconductors over the last decade because of their unique properties. Of these, 5, 6, 11, 12-tetraphenylnaphthacene (rubrene) has generated the most interest because of its high charge carrier mobility. In this paper, large single crystals with a volume of ~1 cm 3 were grown from solution by a temperature reduction technique. The faceted crystals had flat surfaces and cm-scale, visually defect-free areas suitable for physical characterization. X-ray diffraction analysis indicates that solvent does not incorporate into the crystals and photoluminescence spectra are consistent with pristine, high-crystallinity rubrene. Furthermore, the response curve to pulsedmore » optical illumination indicates that the solution grown crystals are of similar quality to those grown by physical vapor transport, albeit larger. The good quality of these crystals in combination with the improvement of electrical contacts by application of conductive polymer on the graphite electrodes have led to the clear observation of alpha particles with these rubrene detectors. Finally, preliminary results with a 252Cf source generate a small signal with the rubrene detector and may demonstrate that rubrene can also be used for detecting high-energy neutrons.« less

Numerical simulation of thermal stress distributions in Czochralski-grown silicon crystals

NASA Astrophysics Data System (ADS)

Kumar, M. Avinash; Srinivasan, M.; Ramasamy, P.

2018-04-01

Numerical simulation is one of the important tools in the investigation and optimization of the single-crystal silicon grown by the Czochralski (Cz) method. A 2D steady global heat transfer model was used to investigate the temperature distribution and the thermal stress distributions at particular crystal position during the Cz growth process. The computation determines the thermal stress such as von Mises stress and maximum shear stress distribution along grown crystal and shows possible reason for dislocation formation in the Cz-grown single-crystal silicon.

Large scale crystallization of protein pharmaceuticals in microgravity via temperature change

NASA Technical Reports Server (NTRS)

Long, Marianna M.

1992-01-01

The major objective of this research effort is the temperature driven growth of protein crystals in large batches in the microgravity environment of space. Pharmaceutical houses are developing protein products for patient care, for example, human insulin, human growth hormone, interferons, and tissue plasminogen activator or TPA, the clot buster for heart attack victims. Except for insulin, these are very high value products; they are extremely potent in small quantities and have a great value per gram of material. It is feasible that microgravity crystallization can be a cost recoverable, economically sound final processing step in their manufacture. Large scale protein crystal growth in microgravity has significant advantages from the basic science and the applied science standpoints. Crystal growth can proceed unhindered due to lack of surface effects. Dynamic control is possible and relatively easy. The method has the potential to yield large quantities of pure crystalline product. Crystallization is a time honored procedure for purifying organic materials and microgravity crystallization could be the final step to remove trace impurities from high value protein pharmaceuticals. In addition, microgravity grown crystals could be the final formulation for those medicines that need to be administered in a timed release fashion. Long lasting insulin, insulin lente, is such a product. Also crystalline protein pharmaceuticals are more stable for long-term storage. Temperature, as the initiation step, has certain advantages. Again, dynamic control of the crystallization process is possible and easy. A temperature step is non-invasive and is the most subtle way to control protein solubility and therefore crystallization. Seeding is not necessary. Changes in protein and precipitant concentrations and pH are not necessary. Finally, this method represents a new way to crystallize proteins in space that takes advantage of the unique microgravity environment. The results

Comparative analysis of anti-polyglutamine Fab crystals grown on Earth and in microgravity.

PubMed

Owens, Gwen E; New, Danielle M; Olvera, Alejandra I; Manzella, Julia Ashlyn; Macon, Brittney L; Dunn, Joshua C; Cooper, David A; Rouleau, Robyn L; Connor, Daniel S; Bjorkman, Pamela J

2016-10-01

Huntington's disease is one of nine neurodegenerative diseases caused by a polyglutamine (polyQ)-repeat expansion. An anti-polyQ antigen-binding fragment, MW1 Fab, was crystallized both on Earth and on the International Space Station, a microgravity environment where convection is limited. Once the crystals returned to Earth, the number, size and morphology of all crystals were recorded, and X-ray data were collected from representative crystals. The results generally agreed with previous microgravity crystallization studies. On average, microgravity-grown crystals were 20% larger than control crystals grown on Earth, and microgravity-grown crystals had a slightly improved mosaicity (decreased by 0.03°) and diffraction resolution (decreased by 0.2 Å) compared with control crystals grown on Earth. However, the highest resolution and lowest mosaicity crystals were formed on Earth, and the highest-quality crystal overall was formed on Earth after return from microgravity.

Comparative analysis of anti-polyglutamine Fab crystals grown on Earth and in microgravity

PubMed Central

Owens, Gwen E.; New, Danielle M.; Olvera, Alejandra I.; Manzella, Julia Ashlyn; Macon, Brittney L.; Dunn, Joshua C.; Cooper, David A.; Rouleau, Robyn L.; Connor, Daniel S.; Bjorkman, Pamela J.

2016-01-01

Huntington’s disease is one of nine neurodegenerative diseases caused by a polyglutamine (polyQ)-repeat expansion. An anti-polyQ antigen-binding fragment, MW1 Fab, was crystallized both on Earth and on the International Space Station, a microgravity environment where convection is limited. Once the crystals returned to Earth, the number, size and morphology of all crystals were recorded, and X-ray data were collected from representative crystals. The results generally agreed with previous microgravity crystallization studies. On average, microgravity-grown crystals were 20% larger than control crystals grown on Earth, and microgravity-grown crystals had a slightly improved mosaicity (decreased by 0.03°) and diffraction resolution (decreased by 0.2 Å) compared with control crystals grown on Earth. However, the highest resolution and lowest mosaicity crystals were formed on Earth, and the highest-quality crystal overall was formed on Earth after return from microgravity. PMID:27710941

Crystallization of bovine insulin on a flow-free droplet-based platform

NASA Astrophysics Data System (ADS)

Chen, Fengjuan; Du, Guanru; Yin, Di; Yin, Ruixue; Zhang, Hongbo; Zhang, Wenjun; Yang, Shih-Mo

2017-03-01

Crystallization is an important process in the pharmaceutical manufacturing industry. In this work, we report a study to create the zinc-free crystals of bovine insulin on a flow-free droplet-based platform we previously developed. The benefit of this platform is its promise to create a single type of crystals under a simpler and more stable environment and with a high throughput. The experimental result shows that the bovine insulin forms a rhombic dodecahedra shape and the coefficient variation (CV) in the size of crystals is less than 5%. These results are very promising for the insulin production.

Comparative Analysis of Thaumatin Crystals Grown on Earth and in Microgravity. Experiment 23

NASA Technical Reports Server (NTRS)

Ng, Joseph D.; Lorber, Bernard; Giege, Richard; Koszelak, Stanley; Day, John; Greenwood, Aaron; McPherson, Alexander

1998-01-01

The protein thaumatin was studied as a model macromolecule for crystallization in microgravity environment experiments conducted on two U.S. Space Shuttle missions (second United States Microgravity Laboratory (USML-2) and Life and Microgravity Spacelab (LMS)). In this investigation we evaluated and compared the quality of space- and Earth-grown thaumatin crystals using x-ray diffraction analysis and characterized them according to crystal size, diffraction resolution limit, and mosaicity. Two different approaches for growing thaumatin crystals in the microgravity environment, dialysis and liquid-liquid diffusion, were employed as a joint experiment by our two investigative teams. Thaumatin crystals grown under a microgravity environment were generally larger in volume with fewer total crystals. They diffracted to significantly higher resolution and with improved diffraction properties as judged by relative Wilson plots. The mosaicity for space-grown crystals was significantly less than for those grown on Earth. Increasing concentrations of protein in the crystallization chambers under microgravity lead to larger crystals. The data presented here lend further support to the idea that protein crystals of improved quality can be obtained in a microgravity environment.

Oxygen-induced recombination centers in as-grown Czochralski silicon crystals

NASA Technical Reports Server (NTRS)

Nauka, K.; Gatos, H. C.; Lagowski, J.

1983-01-01

Simultaneous quantitative microprofiles of the interstitial oxygen concentration and of the excess carrier lifetime are obtained in Czochralski-grown Si crystals employing double laser absorption scanning. It is found that oxygen concentration maxima and minima along the crystal growth direction coincide with lifetime minima and maxima, respectively. Another finding is that the magnitude of oxygen-induced lifetime changes increases dramatically in going from the center to the periphery of the crystal. The findings discussed imply that 'as-grown' oxygen precipitates figure in lifetime-limiting processes.

Neutralization of Hydroxide Ion in Melt-Grown NaCl Crystals

NASA Technical Reports Server (NTRS)

Otterson, Dumas A.

1961-01-01

Many recent studies of solid-state phenomena, particularly in the area of crystal imperfections, have involved the use of melt-grown NaCl single crystals. Quite often trace impurities in these materials have had a prominent effect on these phenomena. Trace amounts of hydroxide ion have been found in melt-grown NaCl crystals. This paper describes a nondestructive method of neutralizing the hydroxide ion in such crystals. Crystals of similar hydroxide content are maintained at an elevated temperature below the melting point of NaCl in a flowing atmosphere containing. dry hydrogen chloride. Heat treatment is continued until an analysis of the test specimens shows no excess hydroxide ion. A colorimetric method previously described4 is used for this analysis.

Anisotropy of electrical resistivity in PVT grown WSe2-x crystals

NASA Astrophysics Data System (ADS)

Solanki, G. K.; Patel, Y. A.; Agarwal, M. K.

2018-05-01

Single crystals of p-type WSe2 and WSe1.9 were grown by a physical vapour transport technique. The anisotropy in d.c. electrical resistivity was investigated in these grown crystals. The off-stoichiometric WSe1.9 exhibited a higher anisotropy ratio as compared to WSe2 crystals. The electron microscopic examination revealed the presence of a large number of stacking faults in these crystals. The resistivity enhancement along the c-axis and anisotropic effective mass ratio explained on the basis of structural disorder introduced due to off-stoichiometry.

Te-and Zn-Doped InSb Crystals Grown in Microgravity

NASA Technical Reports Server (NTRS)

Ostrogorsky, A. G.; Marin, C.; Volz, M.; Bonner, W. A.; Duffar, T.

2004-01-01

In 2002, within the SUBSA (Solidification Using a Baffle in Sealed Ampoules) investigation, seven doped InSb crystals were grown in microgravity at the International Space Station. The key goals of the SUBSA investigation are: (a) to clarify the origin of the melt convection in space laboratories; (b) to reduce melt convection to the level which allows reproducible diffusion-controlled segregation; (e) to explore the submerged baffle process and liquid encapsulation in microgravity. 30 crystal growth experiments were conducted in the ground unit, to optimize the design of flight ampoules and to test the transparent SUBSA furnace developed by TecMasters Inc. The specially designed furnace, allowed observation of the crystal growth process (melting, seeding, motion of the solid-liquid interface, etc.). In the summer of 2002, eight crystal growth experiments were conducted in the Microgravity Science Glovebox (MSG) facility at the ISS. Four Te-doped (k = 0.5) and three Zn-doped (k2.9) crystals were grown on undoped seeds. In one experiment, we were not able to seed and grow. The seven grown crystals were sectioned and analyzed using SIMS. The design of the SUBSA ampoules, the segregation data and the video images obtained during the SUBSA flight experiments will be presented and discussed.

Nanostructures of Indium Gallium Nitride Crystals Grown on Carbon Nanotubes.

PubMed

Park, Ji-Yeon; Man Song, Keun; Min, Yo-Sep; Choi, Chel-Jong; Seok Kim, Yoon; Lee, Sung-Nam

2015-11-16

Nanostructure (NS) InGaN crystals were grown on carbon nanotubes (CNTs) using metalorganic chemical vapor deposition. The NS-InGaN crystals, grown on a ~5-μm-long CNT/Si template, were estimated to be ~100-270 nm in size. Transmission electron microscope examinations revealed that single-crystalline InGaN NSs were formed with different crystal facets. The observed green (~500 nm) cathodoluminescence (CL) emission was consistent with the surface image of the NS-InGaN crystallites, indicating excellent optical properties of the InGaN NSs on CNTs. Moreover, the CL spectrum of InGaN NSs showed a broad emission band from 490 to 600 nm. Based on these results, we believe that InGaN NSs grown on CNTs could aid in overcoming the green gap in LED technologies.

Dopant Segregation in Earth- and Space-Grown InP Crystals

NASA Astrophysics Data System (ADS)

Danilewsky, Andreas Nikolaus; Okamoto, Yusuke; Benz, Klaus Werner; Nishinaga, Tatau

1992-07-01

Macro- and microsegregation of sulphur in InP crystals grown from In solution by the travelling heater method under microgravity and normal gravity are analyzed using spatially resolved photoluminescence. Whereas the macrosegregation in earth- as well as space-grown crystals is explained by conventional steady-state models based on the theory of Burton, Prim and Slichter (BPS), the microsegregation can only be understood in terms of the non-steady-state step exchange model.

A comparison between protein crystals grown with vapor diffusion methods in microgravity and protein crystals using a gel liquid-liquid diffusion ground-based method

NASA Technical Reports Server (NTRS)

Miller, Teresa Y.; He, Xiao-Min; Carter, Daniel C.

1992-01-01

Crystals of human serum albumin have been successfully grown in a variety of gels using crystallization conditions otherwise equivalent to those utilized in the popular hanging-drop vapor-equilibrium method. Preliminary comparisons of gel grown crystals with crystals grown by the vapor diffusion method via both ground-based and microgravity methods indicate that crystals superior in size and quality may be grown by limiting solutal convection. Preliminary X-ray diffraction statistics are presented.

Optical, structural, thermal and dielectric spectroscopy characterizations of seeded melt grown 2-hydroxy biphenyl single crystal.

PubMed

Sadhasivam, S; Rajesh, Narayana Perumal

2014-09-15

Organic single crystal of 2-hydroxy biphenyl (2-HB) was grown by top seeded melt growth method. Scanning electron microscopy studies has been carried out on the surface of the grown crystals to investigate the nature of growth and defects. The crystalline perfection and lattice parameters of 2-HB has been determined by single crystal XRD analysis and it belongs to orthorhombic crystal system with space group Fdd2. The functional groups and molecular associations were confirmed by FT-IR. The optical characteristics such as cut-off and transmittance were carried out using UV-Vis-NIR spectra. Absence of absorption in the region between 320 and 1100 nm makes the grown crystal desirable to optical applications. Thermal stability of grown crystals was characterized by thermogravimetric (TGA), differential thermal analysis (DTA) and differential scanning calorimetric (DSC) analyses. Broadband dielectric studies reveals that dielectric constant of grown crystal is low. The resistivity of grown crystal was studied by impedance analysis. The second harmonic generation intensity of 3.8 mJ was studied. The grown crystal belongs to soft material studied by hardness test. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

Structural analysis of benzothienobenzothiophene-based soluble organic semiconducting crystals grown by liquid crystal solvent

NASA Astrophysics Data System (ADS)

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

2018-06-01

In this study, we analyzed organic semiconducting single crystals composed of benzothienobenzothiophene derivatives (2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene, C8-BTBT) grown by nematic-phase liquid crystal (LC) solvent. As a result, we clarified that the crystal b-axis direction of the C8-BTBT single crystals was consistent with the LC alignment direction. By optical evaluation and simulation based on density functional theory, we found that the C8-BTBT single crystals in LC solvent exhibited a novel molecular conformation having alkyl chains oriented toward the b-axis.

Crystallization and preliminary crystallographic investigation of a low-pH native insulin monomer with flexible behaviour.

PubMed

Zhang, Youshang; Whittingham, Jean L; Turkenburg, Johan P; Dodson, Eleanor J; Brange, Jens; Dodson, G Guy

2002-01-01

Insulin naturally aggregates as dimers and hexamers, whose structures have been extensively analysed by X-ray crystallography. Structural determination of the physiologically relevant insulin monomer, however, is an unusual challenge owing to the difficulty in finding solution conditions in which the concentration of insulin is high enough for crystallization yet the molecule remains monomeric. By utilizing solution conditions known to inhibit insulin assembly, namely 20% acetic acid, crystals of insulin in the monomeric state have been obtained. The crystals are strongly diffracting and a data set extending to 1.6 A has recently been collected. The crystals nominally belong to the space group I422, with unit-cell parameters a = b = 57.80, c = 54.61 A, giving rise to one molecule in the asymmetric unit. Preliminary electron-density maps show that whilst most of the insulin monomer is well ordered and similar in conformation to other insulin structures, parts of the B-chain C-terminus main chain adopt more than one conformation.

Origin of green luminescence in hydrothermally grown ZnO single crystals

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

Čížek, J., E-mail: jakub.cizek@mff.cuni.cz; Hruška, P.; Melikhova, O.

2015-06-22

Combining photoluminescence and positron annihilation studies of hydrothermally grown ZnO crystals with stoichiometry varied by controlled annealing enabled us to clarify the origin of green luminescence. It was found that green luminescence in ZnO has multiple origins and consists of a band at 2.3(1) eV due to recombination of electrons of the conduction band by zinc vacancy acceptors coupled with hydrogen and a band at 2.47(2) eV related to oxygen vacancies. The as-grown ZnO crystals contain zinc vacancies associated with hydrogen and exhibit a green luminescence at 2.3(1) eV. Annealing in Zn vapor removed zinc vacancies and introduced oxygen vacancies.more » This led to disappearance of the green luminescence band at 2.3(1) eV and appearance of a green emission at higher energy of 2.47(2) eV. Moreover, the color of the crystal was changed from colorless to dark red. In contrast, annealing of the as-grown crystal in Cd vapor did not remove zinc vacancies and did not cause any significant change of green luminescence nor change in coloration.« less

Origin of green luminescence in hydrothermally grown ZnO single crystals

NASA Astrophysics Data System (ADS)

Čížek, J.; Valenta, J.; Hruška, P.; Melikhova, O.; Procházka, I.; Novotný, M.; Bulíř, J.

2015-06-01

Combining photoluminescence and positron annihilation studies of hydrothermally grown ZnO crystals with stoichiometry varied by controlled annealing enabled us to clarify the origin of green luminescence. It was found that green luminescence in ZnO has multiple origins and consists of a band at 2.3(1) eV due to recombination of electrons of the conduction band by zinc vacancy acceptors coupled with hydrogen and a band at 2.47(2) eV related to oxygen vacancies. The as-grown ZnO crystals contain zinc vacancies associated with hydrogen and exhibit a green luminescence at 2.3(1) eV. Annealing in Zn vapor removed zinc vacancies and introduced oxygen vacancies. This led to disappearance of the green luminescence band at 2.3(1) eV and appearance of a green emission at higher energy of 2.47(2) eV. Moreover, the color of the crystal was changed from colorless to dark red. In contrast, annealing of the as-grown crystal in Cd vapor did not remove zinc vacancies and did not cause any significant change of green luminescence nor change in coloration.

Temperature dependence of single-crystal elastic constants of flux-grown alpha-GaPO(4).

PubMed

Armand, P; Beaurain, M; Rufflé, B; Menaert, B; Papet, P

2009-06-01

The lattice parameter change with respect to temperature (T) has been measured using high-temperature powder X-ray diffraction techniques for high-temperature flux-grown GaPO(4) single crystals with the alpha-quartz structure. The lattice and the volume linear thermal expansion coefficients in the temperature range 303-1173 K were computed from the X-ray data. The percentage linear thermal expansions along the a and c axes at 1173 K are 1.5 and 0.51, respectively. The temperature dependence of the mass density rho of flux-grown GaPO(4) single crystals was evaluated using the volume thermal expansion coefficient alpha(V)(T) = 3.291 x 10(-5) - 2.786 x 10(-8) [T] + 4.598 x 10(-11)[T](2). Single-crystal high-resolution Brillouin spectroscopy measurements have been carried out at ambient pressure from 303 to 1123 K to determine the elastic constants C(IJ) of high-temperature flux-grown GaPO(4) material. The single-crystal elastic moduli were calculated using the sound velocities via the measured Brillouin frequency shifts Deltanu(B). These are, to our knowledge, the highest temperatures at which single-crystal elastic constants of alpha-GaPO(4) have been measured. Most of the room-temperature elastic constant values measured on flux-grown GaPO(4) material are higher than the ones found for hydrothermally grown GaPO(4) single crystals. The fourth-order temperature coefficients of both the Brillouin frequency shifts T(nuB)((n)) and the single-crystal elastic moduli T(C(IJ))((n)) were obtained. The first-order temperature coefficients of the C(IJ) are in excellent agreement with previous reports on low-temperature hydrothermally grown alpha-GaPO(4) single crystals, while small discrepancies in the higher-order temperature coefficients are observed. This is explained in terms of the OH content in the GaPO(4) network, which is an important parameter in the crystal thermal behavior.

Spherical crystals of Pb 1 - xSn xTe grown in microgravity

NASA Astrophysics Data System (ADS)

Kinoshita, Kyoichi; Yamada, Tomoaki

1996-07-01

Pb 1- xSn xTe spherical crystals were unintentionally obtained along with a cylindrical Pb 1 - xSn xTe crystal grown during the {SL-J}/{FMPT} mission on board the space shuttle "Endeavor". About 25 spherical crystals ranged from 0.5 to 11 mm in diameter. Melt leaked from the melt reservoir into the spring that plays the role of pushing the melt toward a seed crystal and eliminating free surface areas of the melt. Because of the surface tension of the melt, spherical melt drops formed in the hollow of the spring, then solidified into spherical crystals during the cooling process. Some of the crystals had lower dislocation densities, in the order of 10 4 cm -2, two orders smaller than those of terrestrially grown crystals from a melt. The experiment showed a way of stably positioning a large volume of liquid in microgravity without touching the crucible wall and a way of reducing crystalline defects by such growth.

Crystal growth, physical properties and computational insights of semi-organic non-linear optical crystal diphenylguanidinium perchlorate grown by conventional solvent evaporation method

NASA Astrophysics Data System (ADS)

Kajamuhideen, M. S.; Sethuraman, K.; Ramamurthi, K.; Ramasamy, P.

2018-02-01

A splendid nonlinear optical single crystals diphenylguanidinium perchlorate (DPGP) was lucratively grown by low cost solvent evaporation method with the dimensions of 8 × 4 × 2 mm3. Structural and morphological studies of grown crystal were confirmed using X-ray diffraction studies. The presence of diverse functional groups was identified using FTIR and RAMAN studies. The molecular structure of a grown crystal was inveterate by NMR studies. The optical transmittance of DPGP crystal was analyzed using UV-vis-NIR studies. Photoluminescence spectrum shows sharp, well defined emission peak at 388 nm. Thermal studies assign that adduct is stable with the melting point of 164 °C. Microhardness studies declare that DPGP crystal belongs to the soft material class and their yield strength and elastic stiffness constant values were evaluated. Photoconductivity studies revealed the negative photoconductive nature of DPGP crystal. Second harmonic generation (SHG) efficiency of the DPGP crystal was 1.4 times that of potassium dihydrogen phosphate. Etching studies were carried out for different etching time. The dielectric studies were performed at different frequency. Laser damage threshold properties of DPGP crystal were examined using Nd:YAG laser system. The HOMO-LUMO energy gap evident the charge transfer interaction of the molecule. The calculated first order hyperpolarizability value is 5 times greater than that of urea. Thus, the grown DPGP single crystals are well suited for NLO device fabrications.

Effect of amaranth dye on the growth and properties of conventional and SR method grown KAP single crystals

NASA Astrophysics Data System (ADS)

Babu Rao, G.; P., Rajesh; Ramasamy, P.

2018-04-01

The 0.1 mol% amaranth added KAP single crystals were grown from aqueous solutions by both slow evaporation solution technique and Sankaranarayanan-Ramasamy method. The single crystal having dimension of 45 mm length and 12 mm diameter was grown with growth rate of 1.5 mm/day using SR method. 87 % transmittance is obtained for SR method grown amaranth added KAP single crystal. The high intense luminescence at 661 nm is obtained from amaranth added conventional and SR method grown KAP single crystal. The amaranth added KAP single crystal possesses good mechanical and laser damage threshold stability.

Growth, structural, optical, mechanical and quantum chemical analysis of unidirectional grown bis(guanidinium) 5-sulfosalicylate (BGSSA) single crystal

NASA Astrophysics Data System (ADS)

Sreedevi, R.; Saravana Kumar, G.; Amarsingh Bhabu, K.; Balu, T.; Murugakoothan, P.; Rajasekaran, T. R.

2018-02-01

Bis(guanidinium) 5-sulfosalicylate single crystal was grown by using Sankaranarayanan-Ramasamy (SR) method from the solution of methanol and water in equimolar ratio. Good quality crystal with 50 mm length and 10 mm in diameter was grown. The grown crystal was subjected to single crystal X-ray diffraction analysis to confirm the crystal structure and it was found to be orthorhombic. UV-Vis-NIR spectroscopic study revealed that the SR method grown crystal had good optical transparency with wide optical band gap of 4.4 eV. The presence of the functional groups and modes of vibrations were identified by FTIR spectroscopy recorded in the range 4000-400 cm-1. The mechanical strength of the grown crystal was confirmed using Vickers microhardness tester by applying load from 25 g to 100 g. Density functional theory (DFT) method with B3LYP/6-31-G (d,p) level basis set was employed and hence the optimized molecular geometry, first order hyperpolarizability, dipole moment, thermodynamic functions, molecular electrostatic potential and frontier molecular orbital analysis of the grown BGSSA sample was computed and analysed.

Nonstoichiometry and luminescent properties of ZnSe crystals grown from the melt at high pressures

NASA Astrophysics Data System (ADS)

Khanh, Tran; Mozhevitina, Elena; Khomyakov, Andrew; Avetisov, Roman; Davydov, Albert; Chegnov, Vladimir; Antonov, Vladimir; Kobeleva, Svetlana; Zhavoronkov, Nikolai; Avetissov, Igor

2017-01-01

50 mm diameter ZnSe crystals have been grown from the melt by a vertical Bridgman technique at 100 atm argon pressure in a graphite crucible. 3D impurities concentration and nonstoichiometry mappings of the grown crystals have been defined by ICP-MS and a direct physic-chemical method, correspondingly. Photoluminescence mapping of the analyzed crystal has been done. It was found out that along the crystal height the nonstoichiometry changed from Se excess over stoichiometrical composition in the cone (bottom) part to Zn excess in the tail (upper) part passing through the stoichiometrical composition in the cylindrical part of the crystal. Metal impurities concentrated in the upper part of the crystal. The gas-forming impurities (H, C, O, N, F) had stochastic distribution but Cl impurity concentrated in the crystal peripheral part (near the crucible walls). It was found out that the as-grown crystal had a single wide PL peal with maximum of 583 nm. A proposal about complex structure luminescent center based on Cl dopant an overstoichiometric Se has been made.

Quantitative Schlieren analysis applied to holograms of crystals grown on Spacelab 3

NASA Technical Reports Server (NTRS)

Brooks, Howard L.

1986-01-01

In order to extract additional information about crystals grown in the microgravity environment of Spacelab, a quantitative schlieren analysis technique was developed for use in a Holography Ground System of the Fluid Experiment System. Utilizing the Unidex position controller, it was possible to measure deviation angles produced by refractive index gradients of 0.5 milliradians. Additionally, refractive index gradient maps for any recorded time during the crystal growth were drawn and used to create solute concentration maps for the environment around the crystal. The technique was applied to flight holograms of Cell 204 of the Fluid Experiment System that were recorded during the Spacelab 3 mission on STS 51B. A triglycine sulfate crystal was grown under isothermal conditions in the cell and the data gathered with the quantitative schlieren analysis technique is consistent with a diffusion limited growth process.

Characterization of potassium bromide crystals grown in the aqueous solution of picric acid

NASA Astrophysics Data System (ADS)

Maheswari, J. Uma; Krishnan, C.; Kalyanaraman, S.; Selvarajan, P.

2016-12-01

Potassium bromide crystals were grown in the aqueous solution of picric acid by slow evaporation technique at room temperature. X-ray Diffraction (XRD) analysis ensures that the grown sample is in Fm3m space group and FCC structure. Energy Dispersive X-ray Spectroscopy (EDX) reveals the presence of elements in the title compound. UV-Vis-NIR spectrum reveals that the grown sample is a promising nonlinear optical (NLO) material. FTIR analysis confirms the functional groups present in the sample. The thermogravimetric (TG) and differential thermogravimetric (DTA) analyses ensure that the sample material is thermally stable up to 160 °C. The second harmonic efficiency of the sample is 1.3 times greater than that of standard KDP. The mechanical strength of the grown sample is estimated by Vickers microhardness tester. The electrical properties were investigated by impedance analysis and the results of various studies of the grown crystals are discussed.

Paramagnetic resonance of LaGaO3: Mn single crystals grown by floating zone melting

NASA Astrophysics Data System (ADS)

Vazhenin, V. A.; Potapov, A. P.; Artyomov, M. Yu.; Salosin, M. A.; Fokin, A. V.; Gil'mutdinov, I. F.; Mukhamedshin, I. R.

2016-02-01

The EPR spectrum of Mn-doped lanthanum gallate single crystals grown by floating zone melting with optical heating has been studied. In contrast to the crystals grown according to the Czochralski method, no manganese is found in these crystals even after high-temperature annealing in air. The spectral characteristics of Fe3+ and Gd3+ centers in crystals prepared by various methods have been compared in the rhombohedral phase, and the fourth-rank nondiagonal parameters of the Fe3+ trigonal centers have been determined, as well.

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

DTIC Science & Technology

2015-08-28

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

Photoluminescence of vapor and solution grown ZnTe single crystals

NASA Astrophysics Data System (ADS)

Biao, Y.; Azoulay, M.; George, M. A.; Burger, A.; Collins, W. E.; Silberman, E.; Su, C.-H.; Volz, M. E.; Szofran, F. R.; Gillies, D. C.

1994-04-01

ZnTe single crystals grown by horizontal physical vapor transport (PVT) and by vertical traveling heater method (THM) from a Te solution were characterized by photoluminescence (PL) at 10.6 K and by atomic force microscopy (AFM). Copper was identified by PL as a major impurity existing in both crystals, forming a substitutional acceptor, Cu Zn. The THM ZnTe crystals were found to contain more Cu impurity than the PVT ZnTe crystals. The formation of Cu Zn-V Te complexes and the effects of annealing, oxygen contamination and intentional Cu doping were also studied. Finally, the surface morphology analyzed by AFM was correlated to the PL results.

The density and compositional analysis of titanium doped sapphire single crystal grown by the Czocharlski method

NASA Astrophysics Data System (ADS)

Kusuma, H. H.; Ibrahim, Z.; Othaman, Z.

2018-03-01

Titanium doped sapphire (Ti:Al2O3) crystal has attracted attention not only as beautiful gemstones, but also due to their applications as high power laser action. It is very important crystal for tunable solid state laser. Ti:Al2O3 crystals have been success grown using the Czocharlski method with automatic diameter control (ADC) system. The crystals were grown with different pull rates. The structure of the crystal was characterized with X-Ray Diffraction (XRD). The density of the crystal was measurement based on the Archimedes principle and the chemical composition of the crystal was confirmed by the Energy Dispersive X-ray (EDX) Spectroscopy. The XRD patterns of crystals are showed single main peak with a high intensity. Its shows that the samples are single crystal. The Ti:Al2O3 grown with different pull rate will affect the distribution of the concentration of dopant Ti3+ and densities on the sapphire crystals boules as well on the crystal growth process. The increment of the pull rate will increase the percentage distribution of Ti3+ and on the densities of the Ti:Al2O3 crystal boules. This may be attributed to the speed factor of the pull rate of the crystal that then caused changes in the heat flow in the furnace and then causes the homogeneities is changed of species distribution of atoms along crystal.

Properties of high quality GaP single crystals grown by computer controlled liquid encapsulated Czochralski technique

NASA Astrophysics Data System (ADS)

Kokubun, Y.; Washizuka, S.; Ushizawa, J.; Watanabe, M.; Fukuda, T.

1982-11-01

The properties of GaP single crystals grown by an automatically diameter controlled liquid encapsulated Czochralski technique using a computer have been studied. A dislocation density less than 5×104 cm-2 has been observed for crystal grown in a temperature gradient lower than 70 °C/cm near the solid-liquid interface. Crystals have about 10% higher electron mobility than that of commercially available coracle controlled crystals and have 0.2˜0.5 compensation ratios. Yellow light emitting diodes using computer controlled (100) substrates have shown extremely high external quantum efficiency of 0.3%.

Nucleation of insulin crystals in a wide continuous supersaturation gradient.

PubMed

Penkova, Anita; Dimitrov, Ivaylo; Nanev, Christo

2004-11-01

Modifying the classical double pulse technique, by using a supersaturation gradient along an insulin solution contained in a glass capillary tube, we found conditions appropriate for the direct measurement of nucleation parameters. The nucleation time lag has been measured. Data for the number of crystal nuclei versus the nucleation time were obtained for this hormone. Insulin was chosen as a model protein because of the availability of solubility data in the literature. A comparison with the results for hen-egg-white lysozyme, HEWL was performed.

A novel structure of gel grown strontium cyanurate crystal and its structural, optical, electrical characterization

NASA Astrophysics Data System (ADS)

Divya, R.; Nair, Lekshmi P.; Bijini, B. R.; Nair, C. M. K.; Gopakumar, N.; Babu, K. Rajendra

2017-12-01

Strontium cyanurate crystals with novel structure and unique optical property like mechanoluminescence have been grown by conventional gel method. Transparent crystals were obtained. The single crystal X-ray diffraction analysis reveals the exquisite structure of the grown crystal. The crystal is centrosymmetric and has a three dimensional polymeric structure. The powder X ray diffraction analysis confirms its crystalline nature. The functional groups present in the crystal were identified by Fourier transform infrared spectroscopy. Elemental analysis confirmed the composition of the complex. A study of thermal properties was done by thermo gravimetric analysis and differential thermal analysis. The optical properties like band gap, refractive index and extinction coefficient were evaluated from the UV visible spectral analysis. The etching study was done to reveal the dislocations in the crystal which in turn explains mechanoluminescence emission. The mechanoluminescence property exhibited by the crystal makes it suitable for stress sensing applications. Besides being a centrosymmetric crystal, it also exhibits NLO behavior. Dielectric properties were studied and theoretical calculations of Fermi energy, valence electron plasma energy, penn gap and polarisability have been done.

I222 crystal form of despentapeptide (B26-B30) insulin provides new insights into the properties of monomeric insulin.

PubMed

Whittingham, Jean L; Youshang, Zhang; Záková, Lenka; Dodson, Eleanor J; Turkenburg, Johan P; Brange, Jens; Dodson, G Guy

2006-05-01

Despentapeptide (des-B26-B30) insulin (DPI), an active modified insulin, has been crystallized in the presence of 20% acetic acid pH 2. A crystal structure analysis to 1.8 A spacing (space group I222) revealed that the DPI molecule, which is unable to make beta-strand interactions for physiological dimer formation and is apparently monomeric in solution, formed an alternative lattice-generated dimer. The formation of this dimer involved interactions between surfaces which included the B9-B19 alpha-helices (usually buried by the dimer-dimer contacts within the native hexamer). The two crystallographically independent molecules within the dimer were essentially identical and were similar in conformation to T-state insulin as seen in the T(6) insulin hexamer. An unusual feature of each molecule in the dimer was the presence of two independent conformations at the B-chain C-terminus (residues B20-B25). Both conformations were different from that of native insulin, involving a 3.5 A displacement of the B20-B23 beta-turn and a repositioning of residue PheB25 such that it made close van der Waals contact with the main body of the molecule, appearing to stabilize the B-chain C-terminus.

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.

Efficient Incorporation of Mg in Solution Grown GaN Crystals

NASA Astrophysics Data System (ADS)

Freitas, Jaime A., Jr.; Feigelson, Boris N.; Anderson, Travis J.

2013-11-01

Detailed spectrometry and optical spectroscopy studies carried out on GaN crystals grown in solution detect and identify Mg as the dominant shallow acceptor. Selective etching of crystals with higher Mg levels than that of the donor concentration background indicates that Mg acceptors incorporate preferentially in the N-polar face. Electrical transport measurements verified an efficient incorporation and activation of the Mg acceptors. These results suggest that this growth method has the potential to produce p-type doped epitaxial layers or p-type substrates characterized by high hole concentration and low defect density.

Molecular Dynamic Simulation of Space and Earth-Grown Crystal Structures of Thermostable T1 Lipase Geobacillus zalihae Revealed a Better Structure.

PubMed

Ishak, Siti Nor Hasmah; Aris, Sayangku Nor Ariati Mohamad; Halim, Khairul Bariyyah Abd; Ali, Mohd Shukuri Mohamad; Leow, Thean Chor; Kamarudin, Nor Hafizah Ahmad; Masomian, Malihe; Rahman, Raja Noor Zaliha Raja Abd

2017-09-25

Less sedimentation and convection in a microgravity environment has become a well-suited condition for growing high quality protein crystals. Thermostable T1 lipase derived from bacterium Geobacillus zalihae has been crystallized using the counter diffusion method under space and earth conditions. Preliminary study using YASARA molecular modeling structure program for both structures showed differences in number of hydrogen bond, ionic interaction, and conformation. The space-grown crystal structure contains more hydrogen bonds as compared with the earth-grown crystal structure. A molecular dynamics simulation study was used to provide insight on the fluctuations and conformational changes of both T1 lipase structures. The analysis of root mean square deviation (RMSD), radius of gyration, and root mean square fluctuation (RMSF) showed that space-grown structure is more stable than the earth-grown structure. Space-structure also showed more hydrogen bonds and ion interactions compared to the earth-grown structure. Further analysis also revealed that the space-grown structure has long-lived interactions, hence it is considered as the more stable structure. This study provides the conformational dynamics of T1 lipase crystal structure grown in space and earth condition.

DC electrical conductivity measurements for pure and titanium oxide doped KDP Crystals grown by gel medium

NASA Astrophysics Data System (ADS)

Mareeswaran, S.; Asaithambi, T.

2016-10-01

Now a day's crystals are the pillars of current technology. Crystals are applied in various fields like fiber optic communications, electronic industry, photonic industry, etc. Crystal growth is an interesting and innovative field in the subject of physics, chemistry, material science, metallurgy, chemical engineering, mineralogy and crystallography. In recent decades optically good quality of pure and metal doped KDP crystals have been grown by gel growth method in room temperature and its characterizations were studied. Gel method is a very simple and one of the easiest methods among the various crystal growth methods. Potassium dihydrogen phosphate KH2PO4 (KDP) continues to be an interesting material both academically and technologically. KDP is a delegate of hydrogen bonded materials which possess very good electrical and nonlinear optical properties in addition to interesting electro-optic properties. We made an attempt to grow pure and titanium oxide doped KDP crystals with various doping 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 crystals. The dc electrical conductivity (resistance, capacitance and dielectric constant) values of the above grown crystals were measured at two different frequencies (1KHz and 100 Hz) with a temperature range of 500C to 1200C using simple two probe setup with Q band digital LCR meter present in our lab. The electrical conductivity increases with the increase of temperature. Dielectric constants value of titanium oxide doped KDP crystal was slightly decreased compared with pure KDP crystals. Results were discussed in details.

Fabrication of optical element from unidirectional grown imidazole-imidazolium picrate monohydrate (IIP) organic crystals for nonlinear optical applications

NASA Astrophysics Data System (ADS)

Vivek, P.; Murugakoothan, P.

2014-12-01

Nonlinear optical bulk single crystal of Imidazole-imidazolium picrate monohydrate (IIP) has been grown by Sankaranarayanan-Ramasamy (SR) method using acetonitrile as solvent. First time we report the bulk growth of IIP crystal by SR method. The transparent IIP single crystal of maximum diameter 21 mm and length 46 mm was obtained by employing SR method. The grown crystal was subjected to high resolution X-ray diffraction, UV-vis-NIR transmittance, refractive index, hardness, dielectric and laser damage threshold studies. The crystalline perfection of the grown crystal was analyzed using HRXRD. Cut off wavelength and optical transmission window of the crystal was assessed by UV-vis-NIR and the refractive index of the crystal was found. The mechanical property of the crystal was estimated by Vicker's hardness test. The dielectric property of the crystal was measured as a function of frequency. The laser damage threshold value was determined. The particle size dependent second harmonic generation efficiency for IIP was evaluated with standard reference material potassium dihydrogen phosphate (KDP) by Kurtz-Perry powder method using Nd:YAG laser, which established the existence of phase matching. The second harmonic generation (SHG) of IIP crystal was investigated by the SHG Maker fringes technique. The mechanism of growth is revealed by carrying out chemical etching using acetonitrile as etchant.

Macromolecular crystallization in microgravity generated by a superconducting magnet.

PubMed

Wakayama, N I; Yin, D C; Harata, K; Kiyoshi, T; Fujiwara, M; Tanimoto, Y

2006-09-01

About 30% of the protein crystals grown in space yield better X-ray diffraction data than the best crystals grown on the earth. The microgravity environments provided by the application of an upward magnetic force constitute excellent candidates for simulating the microgravity conditions in space. Here, we describe a method to control effective gravity and formation of protein crystals in various levels of effective gravity. Since 2002, the stable and long-time durable microgravity generated by a convenient type of superconducting magnet has been available for protein crystal growth. For the first time, protein crystals, orthorhombic lysozyme, were grown at microgravity on the earth, and it was proved that this microgravity improved the crystal quality effectively and reproducibly. The present method always accompanies a strong magnetic field, and the magnetic field itself seems to improve crystal quality. Microgravity is not always effective for improving crystal quality. When we applied this microgravity to the formation of cubic porcine insulin and tetragonal lysozyme crystals, we observed no dependence of effective gravity on crystal quality. Thus, this kind of test will be useful for selecting promising proteins prior to the space experiments. Finally, the microgravity generated by the magnet is compared with that in space, considering the cost, the quality of microgravity, experimental convenience, etc., and the future use of this microgravity for macromolecular crystal growth is discussed.

The application of crystal soaking technique to study the effect of zinc and cresol on insulinotropin crystals grown from a saline solution.

PubMed

Kim, Y; Haren, A M

1995-11-01

The purpose of this study is to investigate the effect of zinc and cresol on the structure of insulinotropin crystals. Insulinotropin crystals grown from a saline solution were treated with zinc and/or m-cresol using a crystal soaking technique. The effects of these additives on the crystal structure were investigated with powder X-ray diffraction, photomicrography, and differential scanning calorimetry. The molecular interaction between insulinotropin and m-trifluorocresol in solution was also studied by 19F NMR: The data suggest that the original crystals grown from a saline solution have relatively weak lattice forces. After the addition of m-cresol to the suspension of the insulinotropin crystals, the crystals were immediately rendered amorphous. The m-cresol molecules which diffused into the crystals through solvent channels may have disturbed the lattice interactions that maintain the integrity of the crystal. In contrast, the zinc added to the suspension stabilized the crystal lattice so that the subsequent addition of m-cresol did not alter the integrity of the crystals. A marked increase in melting point (206 degrees versus 184 degrees) and heat of fusion (24.6 J/g versus 1.4 J/g) of the crystals was observed after the treatment with zinc. The solubility of the zinc treated crystals in a pH 7.1 phosphate buffered saline was 1/20 of that of the original crystals. When the insulinotropin crystals were treated with the additives using a crystal soaking method, the crystals underwent structural changes. Zinc stabilized the crystal lattice, and reduced the solubility of the peptide.

Spectroscopic study of gel grown L-Valine Zinc Glycine Thiourea Sulfate (VZGTS) crystal: A novel NLO crystal

NASA Astrophysics Data System (ADS)

Rathod, Kiran T.; Patel, I. B.

2017-05-01

In recent years, organometalic non linear optical (NLO) materials have attained immense appeal form researchers due to its range of technological applications in photonic field and optoelectronic technology. In present research work, novel semi organic NLO L-Valine Zinc Glycine Thiourea Sulfate crystals (VZGTS) with different morphologies were grown by gel method at ambient temperature. Presence and identification of functional groups were confirmed by FITR analysis. Spectroscopic studies were carried out for it. The UV-Vis spectroscopy is recorded for crystal. PL study stats that the crystal has insulating nature. Spectroscopic study shows that this crystal has good transparency in the case of fundamental wavelength of Nd : YAG laser. Second Harmonic Generation (SHG) efficiency was confirmed by Kurtz - Perry powder method. Results are discussed in the paper.

X-ray diffraction measurement of cosolvent accessible volume in rhombohedral insulin crystals

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

Soares, Alexei S.; Caspar, Donald L. D.

We report x-ray crystallographic measurement of the number of solvent electrons in the unit cell of a protein crystal equilibrated with aqueous solutions of different densities provides information about preferential hydration in the crystalline state. Room temperature and cryo-cooled rhombohedral insulin crystals were equilibrated with 1.2 M trehalose to study the effect of lowered water activity. The native and trehalose soaked crystals were isomorphous and had similar structures. Including all the low resolution data, the amplitudes of the structure factors were put on an absolute scale (in units of electrons per asymmetric unit) by constraining the integrated number of electronsmore » inside the envelope of the calculated protein density map to equal the number deduced from the atomic model. This procedure defines the value of F(0 0 0), the amplitude at the origin of the Fourier transform, which is equal to the total number of electrons in the asymmetric unit (i.e. protein plus solvent). Comparison of the F(0 0 0) values for three isomorphous pairs of room temperature insulin crystals, three with trehalose and three without trehalose, indicates that 75 ± 12 electrons per asymmetric unit were added to the crystal solvent when soaked in 1.2 M trehalose. If all the water in the crystal were available as solvent for the trehalose, 304 electrons would have been added. Thus, the co-solvent accessible volume is one quarter of the total water in the crystal. Finally, determination of the total number of electrons in a protein crystal is an essential first step for mapping the average density distribution of the disordered solvent.« less

X-ray diffraction measurement of cosolvent accessible volume in rhombohedral insulin crystals

DOE PAGES

Soares, Alexei S.; Caspar, Donald L. D.

2017-08-31

We report x-ray crystallographic measurement of the number of solvent electrons in the unit cell of a protein crystal equilibrated with aqueous solutions of different densities provides information about preferential hydration in the crystalline state. Room temperature and cryo-cooled rhombohedral insulin crystals were equilibrated with 1.2 M trehalose to study the effect of lowered water activity. The native and trehalose soaked crystals were isomorphous and had similar structures. Including all the low resolution data, the amplitudes of the structure factors were put on an absolute scale (in units of electrons per asymmetric unit) by constraining the integrated number of electronsmore » inside the envelope of the calculated protein density map to equal the number deduced from the atomic model. This procedure defines the value of F(0 0 0), the amplitude at the origin of the Fourier transform, which is equal to the total number of electrons in the asymmetric unit (i.e. protein plus solvent). Comparison of the F(0 0 0) values for three isomorphous pairs of room temperature insulin crystals, three with trehalose and three without trehalose, indicates that 75 ± 12 electrons per asymmetric unit were added to the crystal solvent when soaked in 1.2 M trehalose. If all the water in the crystal were available as solvent for the trehalose, 304 electrons would have been added. Thus, the co-solvent accessible volume is one quarter of the total water in the crystal. Finally, determination of the total number of electrons in a protein crystal is an essential first step for mapping the average density distribution of the disordered solvent.« less

Structural and optical properties of indium-doped highly conductive ZnO bulk crystals grown by the hydrothermal technique

NASA Astrophysics Data System (ADS)

Wang, Buguo; Claflin, Bruce; Look, David; Jiménez, Juan

2018-02-01

Indium-doped ZnO bulk crystals grown by the hydrothermal method are highly-conductive, with resistivity at 0.01 Ωcm at room temperature as revealed by Hall-effect measurement. In this paper we report on structural and optical properties of these crystals. The grown In:ZnO crystals have been studied by high resolution X-ray diffraction, micro-Raman scattering and low-temperature photoluminescence and cathodoluminescence. It was found that the c lattice parameter of the grown In:ZnO crystal expanded 0.06% with respect to the lithium-doped ZnO crystal seed, and the In-doped ZnO overgrew the seed crystal pseudomorphically but with high quality crystallinity; the X-ray rocking curves show the FWHM of the Zn face and O faces are only 0.05° and 0.1° ; and the indium concentration in the crystal reaches the solubility limit. Raman spectra show strain relaxation gradually from the regrowth interface as well as a weak spectral feature at 723 cm-1. The peak at 312 cm-1 noticed in hydrothermally grown In:ZnO nanostructures does not appear in our In-doped crystals, indicating that this peak may be associated with specific defects (e.g. surface related) of the nanostructures. Photoluminescence measurements show that an indium donor bound exciton peak I9 (In0X) is the dominant peak in the PL spectrum, located at 3.3586 eV on the zinc face and 3.3577 eV on the oxygen face. Both of them deviated from the consensus literature value of 3.3567 eV, probably due to strain in the crystal induced by impurities.

Thermoelectric properties of Ge 1-xSn xTe crystals grown by vertical Bridgman method

NASA Astrophysics Data System (ADS)

Wu, C. C.; Ferng, N. J.; Gau, H. J.

2007-06-01

Single crystals of Ge 1-xSn xTe compounds with x=0, 0.8, 0.9 and 1.0 were grown by vertical Bridgman method. The crystalline phase and stochiometry for these crystals were investigated by X-ray diffraction, metallographic microscope as well as electron-probe microanalysis (EPMA). Electrical property of the as-grown samples was characterized using room temperature resistivity and Hall measurements. The thermoelectric behaviors for the Ge 1-xSn xTe crystals were studied by means of thermal and carrier transport measurements. Temperature dependences of resistivity, Seebeck coefficient and thermal conductivity for the various compositions of Ge 1-xSn xTe were analyzed. A two-valence band model was proposed to describe the temperature dependence of thermoelectric property of the Ge 1-xSn xTe crystals. The dimensionless thermoelectric figure of merit ZT for the alloys was evaluated and discussed.

Temperature Dependence of Morphology and Growth Mechanism of Vapor-Grown Cd crystals as Affected by Bi Impurities

NASA Astrophysics Data System (ADS)

Yumoto, Hisami; Hasiguti, Ryukiti R.

1984-07-01

Hexagonal prismatic Cd crystals having {10\\bar{1}0} prismatic planes, or occasionally having {11\\bar{2}0} prismatic planes, were grown as high-temperature-type Cd crystals by the thin layer VLS mechanism at Ts (growth temperature) ≥ Tt (transition temperature range: 250-260°C). Pencil-shaped Cd crystals (low-temperature-type Cd crystals) were grown, having {10\\bar{1}0} and {11\\bar{2}0} prismatic planes and {10\\bar{1}1} pyramidal planes by the mixed-type VLS mechanism at Ts≤Tt. When the growth temperature was decreased below Tt, the shape of the solid-liquid interface changed from rounded to faceted. Three processes for the termination of the mixed-type VLS growth are proposed.

Sulfatide promotes the folding of proinsulin, preserves insulin crystals, and mediates its monomerization.

PubMed

Osterbye, T; Jørgensen, K H; Fredman, P; Tranum-Jensen, J; Kaas, A; Brange, J; Whittingham, J L; Buschard, K

2001-06-01

Sulfatide is a glycolipid that has been associated with insulin-dependent diabetes mellitus. It is present in the islets of Langerhans and follows the same intracellular route as insulin. However, the role of sulfatide in the beta cell has been unclear. Here we present evidence suggesting that sulfatide promotes the folding of reduced proinsulin, indicating that sulfatide possesses molecular chaperone activity. Sulfatide associates with insulin by binding to the insulin domain A8--A10 and most likely by interacting with the hydrophobic side chains of the dimer-forming part of the insulin B-chain. Sulfatide has a dual effect on insulin. It substantially reduces deterioration of insulin hexamer crystals at pH 5.5, conferring stability comparable to those in beta cell granules. Sulfatide also mediates the conversion of insulin hexamers to the biological active monomers at neutral pH, the pH at the beta-cell surface. Finally, we report that inhibition of sulfatide synthesis with chloroquine and fumonisine B1 leads to inhibition of insulin granule formation in vivo. Our observations suggest that sulfatide plays a key role in the folding of proinsulin, in the maintenance of insulin structure, and in the monomerization process.

Ferromagnetism in CVT grown tungsten diselenide single crystals with nickel doping

NASA Astrophysics Data System (ADS)

Habib, Muhammad; Muhammad, Zahir; Khan, Rashid; Wu, Chuanqiang; Rehman, Zia ur; Zhou, Yu; Liu, Hengjie; Song, Li

2018-03-01

Two dimensional (2D) single crystal layered transition materials have had extensive consideration owing to their interesting magnetic properties, originating from their lattices and strong spin-orbit coupling, which make them of vital importance for spintronic applications. Herein, we present synthesis of a highly crystalline tungsten diselenide layered single crystal grown by chemical vapor transport technique and doped with nickel (Ni) to tailor its magnetic properties. The pristine WSe2 single crystal and Ni-doped crystal were characterized and analyzed for magnetic properties using both experimental and computational aspects. It was found that the magnetic behavior of the 2D layered WSe2 crystal changed from diamagnetic to ferromagnetic after Ni-doping at all tested temperatures. Moreover, first principle density functional theory (DFT) calculations further confirmed the origin of room temperature ferromagnetism of Ni-doped WSe2, where the d-orbitals of the doped Ni atom promoted the spin moment and thus largely contributed to the magnetism change in the 2D layered material.

Studies on the growth aspects, structural, thermal, dielectric and third order nonlinear optical properties of solution grown 4-methylpyridinium p-nitrophenolate single crystal

NASA Astrophysics Data System (ADS)

Devi, S. Reena; Kalaiyarasi, S.; Zahid, I. MD.; Kumar, R. Mohan

2016-11-01

An ionic organic optical crystal of 4-methylpyridinium p-nitrophenolate was grown from methanol by slow evaporation method at ambient temperature. Powder and single crystal X-ray diffraction studies revealed the crystal system and its crystalline perfection. The rocking curve recorded from HRXRD study confirmed the crystal quality. FTIR spectral analysis confirmed the functional groups present in the title compound. UV-visible spectral study revealed the optical window and band gap of grown crystal. The thermal, electrical and surface laser damage threshold properties of harvested crystal were examined by using TGA/DTA, LCR/Impedance Analyzer and Nd:YAG laser system respectively. The third order nonlinear optical property of grown crystal was elucidated by Z-scan technique.

Optical Properties of LiNbO3 Single Crystal Grown by Czochralski Method

NASA Astrophysics Data System (ADS)

Sahar, M. R.; Naim, N. M.; Hamzah, K.

2011-03-01

Pure LiNbO3 single crystal was grown by Czochralski method using Automatic Diameter Control—Crystal Growth System (ADC-CGS). The transmission spectrum was determined by using Infrared Spectroscopy while the refractive index was determined using UV-Vis spectroscopy via the Sellmeier equation. The density was also measured using the Archimedes principle. It was found that the peak for the absorption vibrational spectrum for LiNbO3 crystal occurs at 801 cm-1, 672 cm-1, 639 cm-1 and 435 cm-1. The refractive index, ne was found to be 2.480 and the crystal density was around 4.64 g/cm3.

Homogeneity and variation of donor doping in Verneuil-grown SrTiO3:Nb single crystals

PubMed Central

Rodenbücher, C.; Luysberg, M.; Schwedt, A.; Havel, V.; Gunkel, F.; Mayer, J.; Waser, R.

2016-01-01

The homogeneity of Verneuil-grown SrTiO3:Nb crystals was investigated. Due to the fast crystal growth process, inhomogeneities in the donor dopant distribution and variation in the dislocation density are expected to occur. In fact, for some crystals optical studies show variations in the density of Ti3+ states on the microscale and a cluster-like surface conductivity was reported in tip-induced resistive switching studies. However, our investigations by TEM, EDX mapping, and 3D atom probe reveal that the Nb donors are distributed in a statistically random manner, indicating that there is clearly no inhomogeneity on the macro-, micro-, and nanoscale in high quality Verneuil-grown crystals. In consequence, the electronic transport in the bulk of donor-doped crystals is homogeneous and it is not significantly channelled by extended defects such as dislocations which justifies using this material, for example, as electronically conducting substrate for epitaxial oxide film growth. PMID:27577508

Relaxor properties of barium titanate crystals grown by Remeika method

NASA Astrophysics Data System (ADS)

Roth, Michel; Tiagunov, Jenia; Dul'kin, Evgeniy; Mojaev, Evgeny

2017-06-01

Barium titanate (BaTiO3, BT) crystals have been grown by the Remeika method using both the regular KF and mixed KF-NaF (0.6-0.4) solvents. Typical acute angle "butterfly wing" BT crystals have been obtained, and they were characterized using x-ray diffraction, scanning electron microscopy (including energy dispersive spectroscopy), conventional dielectric and acoustic emission methods. A typical wing has a triangular plate shape which is up to 0.5 mm thick with a 10-15 mm2 area. The plate has a (001) habit and an atomically smooth outer surface. Both K+ and F- solvent ions are incorporated as dopants into the crystal lattice during growth substituting for Ba2+ and O2- ions respectively. The dopants' distribution is found to be inhomogeneous, their content being almost an order of magnitude higher (up to 2 mol%) at out surface of the plate relatively to the bulk. A few μm thick surface layer is formed where a multidomain ferroelectric net is confined between two≤1 μm thick dopant-rich surfaces. The layer as a whole possess relaxor ferroelectric properties, which is apparent from the appearance of additional broad maxima, Tm, in the temperature dependence of the dielectric permittivity around the ferroelectric phase transition. Intense acoustic emission responses detected at temperatures corresponding to the Tm values allow to observe the Tm shift to lower temperatures at higher frequencies, or dispersion, typical for relaxor ferroelectrics. The outer surface of the BT wing can thus serve as a relaxor thin film for various electronic application, such as capacitors, or as a substrate for BT-based multiferroic structure. Crystals grown from KF-NaF fluxes contain sodium atoms as an additional impurity, but the crystal yield is much smaller, and while the ferroelectric transition peak is diffuse it does not show any sign of dispersion typical for relaxor behavior.

Ultra-fast scintillation properties of β-Ga2O3 single crystals grown by Floating Zone method

NASA Astrophysics Data System (ADS)

He, Nuotian; Tang, Huili; Liu, Bo; Zhu, Zhichao; Li, Qiu; Guo, Chao; Gu, Mu; Xu, Jun; Liu, Jinliang; Xu, Mengxuan; Chen, Liang; Ouyang, Xiaoping

2018-04-01

In this investigation, β-Ga2O3 single crystals were grown by the Floating Zone method. At room temperature, the X-ray excited emission spectrum includes ultraviolet and blue emission bands. The scintillation light output is comparable to the commercial BGO scintillator. The scintillation decay times are composed of the dominant ultra-fast component of 0.368 ns and a small amount of slightly slow components of 8.2 and 182 ns. Such fast component is superior to most commercial inorganic scintillators. In contrast to most semiconductor crystals prepared by solution method such as ZnO, β-Ga2O3 single crystals can be grown by traditional melt-growth method. Thus we can easily obtain large bulk crystals and mass production.

Highly resistive C-doped hydride vapor phase epitaxy-GaN grown on ammonothermally crystallized GaN seeds

NASA Astrophysics Data System (ADS)

Iwinska, Malgorzata; Piotrzkowski, Ryszard; Litwin-Staszewska, Elzbieta; Sochacki, Tomasz; Amilusik, Mikolaj; Fijalkowski, Michal; Lucznik, Boleslaw; Bockowski, Michal

2017-01-01

GaN crystals were grown by hydride vapor phase epitaxy (HVPE) and doped with C. The seeds were high-structural-quality ammonothermally crystallized GaN. The grown crystals were highly resistive at 296 K and of high structural quality. High-temperature Hall effect measurements revealed p-type conductivity and a deep acceptor level in the material with an activation energy of 1 eV. This is in good agreement with density functional theory calculations based on hybrid functionals as presented by the Van de Walle group. They obtained an ionization energy of 0.9 eV when C was substituted for N in GaN and acted as a deep acceptor.

Growth and antimicrobial studies of γ-glycine crystal grown using CuSO4

NASA Astrophysics Data System (ADS)

Vijayalakshmi, V.; Dhanasekaran, P.

2018-05-01

In the current work single crystals of pure and 1M of CuSO4-added glycine were grown by slow evaporation method and its optical and antimicrobial properties were studied. The Polymorph of glycine transforms from a-glycine to γ-glycine due to the incorporation of CuSO4 on glycine was affirmed by the PXRD and FTIR studies. The impact of CuSO4 on the antimicrobial action of the grown samples was deliberate by utilizing the agar diffusion method.

Concentration and structure inhomogeneities in GaSb(Si) single crystals grown at different heat and mass transfer conditions

NASA Astrophysics Data System (ADS)

Serebryakov, Yu. A.; Prokhorov, I. A.; Vlasov, V. N.; Korobeynikova, E. N.; Zakharov, B. G.; Shul'pina, I. L.; Marchenko, M. P.; Fryazinov, I. V.

2007-06-01

Results of ground-based experiments on crystallization of gallium antimonide on the POLIZON facility carried out within the framework of space experiment preparation aboard FOTON satellite are submitted. Technical and technological opportunities of suppression of disturbing factors for improvement of quality of grown crystals in space are substantiated. Features of formation of concentration and structure inhomogeneities in GaSb:Si crystals grown under non-stationary and stationary convection conditions are investigated. Experimental data about structure and dopant distribution inhomogeneities are discussed taking into account results of numerical researches of GaSb:Si crystallization. Also earlier received results of modeling of GaSb:Te crystallization under close temperature conditions are used. Correlation between computational and experimental data is shown. The data on intensity of flows close to crystallization front are received at which non-stationary or stationary conditions of crystallization are realized. The forecast for space conditions is made. The influence of a rotating magnetic field on convection in melt for application in space experiment projected is investigated.

Analysis of Phase Separation in Czochralski Grown Single Crystal Ilmenite

NASA Technical Reports Server (NTRS)

Wilkins, R.; Powell, Kirk St. A.; Loregnard, Kieron R.; Lin, Sy-Chyi; Muthusami, Jayakumar; Zhou, Feng; Pandey, R. K.; Brown, Geoff; Hawley, M. E.

1998-01-01

Ilmenite (FeTiOs) is a wide bandgap semiconductor with an energy gap of 2.58 eV. Ilmenite has properties suited for radiation tolerant applications, as well as a variety of other electronic applications. Single crystal ilmenite has been grown from the melt using the Czochralski method. Growth conditions have a profound effect on the microstructure of the samples. Here we present data from a variety of analytical techniques which indicate that some grown crystals exhibit distinct phase separation during growth. This phase separation is apparent for both post-growth annealed and unannealed samples. Under optical microscopy, there appear two distinct areas forming a matrix with an array of dots on order of 5 pm diameter. While appearing bright in the optical micrograph, atomic force microscope (AFM) shows the dots to be shallow pits on the surface. Magnetic force microscope (MFM) shows the dots to be magnetic. Phase identification via electron microprobe analysis (EMPA) indicates two major phases in the unannealed samples and four in the annealed samples, where the dots appear to be almost pure iron. This is consistent with micrographs taken with a scanning probe microscope used in the magnetic force mode. Samples that do not exhibit the phase separation have little or no discernible magnetic structure detectable by the MFM.

High-power laser with Nd:YAG single-crystal fiber grown by the micro-pulling-down technique

NASA Astrophysics Data System (ADS)

Didierjean, Julien; Castaing, Marc; Balembois, François; Georges, Patrick; Perrodin, Didier; Fourmigué, Jean Marie; Lebbou, Kherreddine; Brenier, Alain; Tillement, Olivier

2006-12-01

We present optical characterization and laser results achieved with single-crystal fibers directly grown by the micro-pulling-down technique. We investigate the spectroscopic and optical quality of the fiber, and we present the first laser results. We achieved a cw laser power of 10 W at 1064 nm for an incident pump power of 60 W at 808 nm and 360 kW peak power for 12 ns pulses at 1 kHz in the Q-switched regime. It is, to the best of our knowledge, the highest laser power ever achieved with directly grown single-crystal fibers.

Optical characterization of single-crystal diamond grown by DC arc plasma jet CVD

NASA Astrophysics Data System (ADS)

Hei, Li-fu; Zhao, Yun; Wei, Jun-jun; Liu, Jin-long; Li, Cheng-ming; Lü, Fan-xiu

2017-12-01

Optical centers of single-crystal diamond grown by DC arc plasma jet chemical vapor deposition (CVD) were examined using a low-temperature photoluminescence (PL) technique. The results show that most of the nitrogen-vacancy (NV) complexes are present as NV- centers, although some H2 and H3 centers and B-aggregates are also present in the single-crystal diamond because of nitrogen aggregation resulting from high N2 incorporation and the high mobility of vacancies under growth temperatures of 950-1000°C. Furthermore, emissions of radiation-induced defects were also detected at 389, 467.5, 550, and 588.6 nm in the PL spectra. The reason for the formation of these radiation-induced defects is not clear. Although a Ni-based alloy was used during the diamond growth, Ni-related emissions were not detected in the PL spectra. In addition, the silicon-vacancy (Si-V)-related emission line at 737 nm, which has been observed in the spectra of many previously reported microwave plasma chemical vapor deposition (MPCVD) synthetic diamonds, was absent in the PL spectra of the single-crystal diamond prepared in this work. The high density of NV- centers, along with the absence of Ni-related defects and Si-V centers, makes the single-crystal diamond grown by DC arc plasma jet CVD a promising material for applications in quantum computing.

Pressure relaxation and diffusion of vacancies in rapidly grown helium crystals

NASA Astrophysics Data System (ADS)

Birchenko, A. P.; Mikhin, N. P.; Rudavskii, E. Ya.; Smirnov, S. N.; Fysun, Ya. Yu.

2018-04-01

An experimental study of the features of pressure relaxation in rapidly grown crystals of a diluted solid solution 3He-4He, at temperatures above 1.3 K, was performed. A cylindrical cell with capacitive pressure sensors at the ends was used for measurements. It was found that, when the helium crystals were grown at cooling rates ≳4 mK/s, the difference in pressure ΔP registered by the sensors at 1.3 K reached 2.4 bars. The ΔP value decreased with subsequent stepwise increase in temperature, but reached zero only after thorough annealing at the premelting temperatures. The kinetics of pressure changes at the sample ends at different temperatures was recorded. The results obtained were interpreted within the framework of the structural relaxation model based on the monovacancy diffusion mechanism. The proposed model made it possible to explain the dependence of ΔP on the time and temperature recorded in the experiment, as well as to determine the activation energy of the structural relaxation process and the diffusion coefficient of vacancies. The details of the vacancy model are described in the Appendix.

Investigation of inorganic nonlinear optical potassium penta borate tetra hydrate (PPBTH) single crystals grown by slow evaporation method

NASA Astrophysics Data System (ADS)

Arivuselvi, R.; Babu, P. Ramesh

2018-03-01

Borates family crystals were plays vital role in the field of non linear optics (NLO) due to needs of wide range of applications. In this report, NLO crystals (potassium penta borate tetra hydrate (KB5H8O12) are grown by slow evaporation method at room temperature (28° C) and studied their physical properties. The harvested single crystals are transparent with the dimension of 12 × 10 × 6 mm3 and colourless. X-ray diffraction of single crystals reveals that the grown crystal belongs to orthorhombic system with non-centrosymmetric space group Pba2. All the absorbed functional groups are present in the order of inorganic compounds expect 1688 cm-1 because of water (Osbnd H sbnd O blending) molecule present in the pristine. Crystals show transparent in the entire visible region with 5.9 eV optical band gap and also it shows excellence in both second and third order nonlinear optical properties. Crystals can withstand upto 154 °C without any phase changes which is observed using thermal (TGA/DTA) analysis.

Crystal Growth and Characterization of CdTe Grown by Vertical Gradient Freeze

NASA Technical Reports Server (NTRS)

Su, Ching-Hua; Lehoczky, S. L.; Raghothamachar, B.; Dudley, M.

2007-01-01

In this study, crystals of CdTe were grown from melts by the unseeded vertical gradient freeze method. The quality of grown crystal were studied by various characterization techniques including Synchrotron White Beam X-ray Topography (SWBXT), chemical analysis by glow discharge mass spectroscopy (GDMS), low temperature photoluminescence (PL), and Hall measurements. The SWBXT images from various angles show nearly strain-free grains, grains with inhomogeneous strains, as well as twinning nucleated in the shoulder region of the boule. The GDMS chemical analysis shows the contamination of Ga at a level of 3900 ppb, atomic. The low temperature PL measurement exhibits the characteristic emissions of a Ga-doped sample. The Hall measurements show a resistivity of 1 x l0(exp 7) ohm-cm at room temperature to 3 x 10(exp 9) ohm-cm at 78K with the respective hole and electron concentration of 1.7 x 10(exp 9) cm(exp -3) and 3.9 x 10(exp 7) cm(exp -3) at room temperature.

Comparison of the quality of single-crystal diamonds grown on two types of seed substrates by MPCVD

NASA Astrophysics Data System (ADS)

Zhao, Yun; Guo, Yanzhao; Lin, Liangzhen; Zheng, Yuting; Hei, Lifu; Liu, Jinlong; Wei, Junjun; Chen, Liangxian; Li, Chengming

2018-06-01

Microwave plasma chemical vapor deposition (MPCVD) was used to grow single-crystal diamonds on two types of single-crystal diamond seed substrates prepared by high-pressure, high-temperature (HPHT) and chemical vapor deposition (CVD) methods. The quality of diamonds grown on the different seed substrates was compared. Fluorescence characteristics showed that the sectors of the HPHT seed substrates were obviously partitioned. Raman and absorption spectra showed that the CVD seed substrate produced higher-quality crystals with fewer nitrogen impurities. X-ray topography showed that the HPHT seed substrate had obvious growth sector boundaries, inclusions, dislocations, and stacking faults. The polarization characteristics of HPHT seed substrate were obvious, and the stress distribution was not uniform. When etching HPHT and CVD seed substrates using the same parameters, the etching morphology and extent of different growth sectors of the two substrates differed. Although extended defects were inevitably formed at the interface and propagated in the CVD layer, the dislocation density of a 1 mm-thick CVD layer grown on a CVD seed substrate was only half that of a 1 mm-thick CVD layer grown on an HPHT seed substrate. Therefore, the use of CVD seed substrate enabled the growth of a relatively higher-quality CVD single-crystal diamond.

Large piezoelectric properties in KNN-based lead-free single crystals grown by a seed-free solid-state crystal growth method

NASA Astrophysics Data System (ADS)

Yang, Jie; Zhang, Faqiang; Yang, Qunbao; Liu, Zhifu; Li, Yongxiang; Liu, Yun; Zhang, Qiming

2016-05-01

We report lead-free single crystals with a nominal formula of (K0.45Na0.55)0.96Li0.04NbO3 grown using a simple low-cost seed-free solid-state crystal growth method (SFSSCG). The crystals thus prepared can reach maximum dimensions of 6 mm × 5 mm × 2 mm and exhibit a large piezoelectric coefficient d33 of 689 pC/N. Moreover, the effective piezoelectric coefficient d33 * , obtained under a unipolar electric field of 30 kV/cm, can reach 967 pm/V. The large piezoelectric response plus the high Curie temperature (TC) of 432 °C indicate that SFSSCG is an effective approach to synthesize high-performance lead-free piezoelectric single crystals.

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

Metal-insulator transition characteristics of VO2 thin films grown on Ge(100) single crystals

NASA Astrophysics Data System (ADS)

Yang, Z.; Ko, C.; Ramanathan, S.

2010-10-01

Phase transitions exhibited by correlated oxides could be of potential relevance to the emerging field of oxide electronics. We report on the synthesis of high-quality VO2 thin films grown on single crystal Ge(100) substrates by physical vapor deposition and their metal-insulator transition (MIT) properties. Thermally triggered MIT is demonstrated with nearly three orders of magnitude resistance change across the MIT with transition temperatures of 67 °C (heating) and 61 °C (cooling). Voltage-triggered hysteretic MIT is observed at room temperature at threshold voltage of ˜2.1 V for ˜100 nm thickness VO2 films. Activation energies for electron transport in the insulating and conducting states are obtained from variable temperature resistance measurements. We further compare the properties of VO2 thin films grown under identical conditions on Si(100) single crystals. The VO2 thin films grown on Ge substrate show higher degree of crystallinity, slightly reduced compressive strain, larger resistance change across MIT compared to those grown on Si. Depth-dependent x-ray photoelectron spectroscopy measurements were performed to provide information on compositional variation trends in the two cases. These results suggest Ge could be a suitable substrate for further explorations of switching phenomena and devices for thin film functional oxides.

Material and detector properties of cadmium manganese telluride (Cd 1-xMn xTe) crystals grown by the modified floating-zone method

DOE PAGES

Hossain, A.; Gu, G. D.; Bolotnikov, A. E.; ...

2014-12-24

We demonstrated the material- and radiation-detection properties of cadmium manganese telluride (Cd 1-xMn xTe; x=0.06), a wide-band-gap semiconductor crystal grown by the modified floating-zone method. We investigated the presence of various bulk defects, such as Te inclusions, twins, and dislocations of several as-grown indium-doped Cd 1-xMn xTe crystals using different techniques, viz., IR transmission microscopy, and chemical etching. We then fabricated four planar detectors from selected CdMnTe crystals, characterized their electrical properties, and tested their performance as room-temperature X- and gamma-ray detectors. Thus, our experimental results show that CMT crystals grown by the modified floating zone method apparently are freemore » from Te inclusions. However, we still need to optimize our growth parameters to attain high-resistivity, large-volume single-crystal CdMnTe.« less

Influence of electron irradiation on hydrothermally grown zinc oxide single crystals

NASA Astrophysics Data System (ADS)

Lu, L. W.; So, C. K.; Zhu, C. Y.; Gu, Q. L.; Li, C. J.; Fung, S.; Brauer, G.; Anwand, W.; Skorupa, W.; Ling, C. C.

2008-09-01

The resistivity of hydrothermally grown ZnO single crystals increased from ~103 Ω cm to ~106 Ω cm after 1.8 MeV electron irradiation with a fluence of ~1016 cm-2, and to ~109 Ω cm as the fluence increased to ~1018 cm-2. Defects in samples were studied by thermally stimulated current (TSC) spectroscopy and positron lifetime spectroscopy (PLS). After the electron irradiation with a fluence of 1018 cm-2, the normalized TSC signal increased by a factor of ~100. A Zn vacancy was also introduced by the electron irradiation, though with a concentration lower than expected. After annealing in air at 400 °C, the resistivity and the deep traps concentrations recovered to the levels of the as-grown sample, and the Zn vacancy was removed.

The mechanical properties of as-grown noncubic organic molecular crystals assessed by nanoindentation

DOE PAGES

Taw, Matthew R.; Yeager, John D.; Hooks, Daniel E.; ...

2017-06-19

Organic molecular crystals are often noncubic and contain significant steric hindrance within their structure to resist dislocation motion. Plastic deformation in these systems can be imparted during processing (tableting and comminution of powders), and the defect density impacts subsequent properties and performance. This paper measured the elastic and plastic properties of representative monoclinic, orthorhombic, and triclinic molecular crystalline structures using nanoindentation of as-grown sub-mm single crystals. The variation in modulus due to in-plane rotational orientation, relative to a Berkovich tip, was approximately equal to the variation of a given crystal at a fixed orientation. The onset of plasticity occurs consistentlymore » at shear stresses between 1 and 5% of the elastic modulus in all three crystal systems, and the hardness to modulus ratio suggests conventional Berkovich tips do not generate fully self-similar plastic zones in these materials. Finally, this provides guidance for mechanical models of tableting, machining, and property assessment of molecular crystals.« less

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.

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

Control of Orientation and Morphology of Crystals Grown Under Organic Templates

NASA Astrophysics Data System (ADS)

Stripe, Benjamin

Living creatures demonstrate an extraordinary ability to both grow and control the growth of inorganic crystals. These biominerals are found almost everywhere in nature from simple plants and plankton to our own teeth and bones. A great deal of research has been focused on how living creatures are able to achieve such control over the shape, size, orientation, and arrangement of these biominerals. Many studies have been done demonstrating the effects the presence of organic molecules can have on the morphology of nucleating inorganic crystals. These studies have led to the use of ordered arrays of biological molecules as templates to select the orientation of the crystals. Such experiments have had amazing success cataloging monolayers, orientations and morphologies of crystals grown beneath them. However, despite several decades of work, the exact mechanisms by which the orientation and morphology of crystals is selected by organic templates are still not known. The present study attempts to explain the complex interactions that take place at the template surface and decide the orientations and morphologies of the crystals that nucleate there. To do this, scanning electron microscopy (SEM), grazing incidence x-ray diffraction (GID), and x-ray reflectivity have been used to probe the templates and nucleating crystals in situ. The experiments described here seek to move beyond the well-studied two-component systems. In many of these two-component systems a single template and a single type of crystal are grown, and often many claims and comparisons are made about monolayer charge, crystal surface energies, stereochemical recognition, and lattice matches. However, almost all of the claims and comparisons are between systems that are different enough that assumptions about relative charge, strain, recognition, and lattice dynamics are either unfounded or poorly supported. To bridge this gap in the comparison of these different two-component systems the studies

Optical properties of bulk gallium nitride single crystals grown by chloride-hydride vapor-phase epitaxy

NASA Astrophysics Data System (ADS)

Agyekyan, V. F.; Borisov, E. V.; Serov, A. Yu.; Filosofov, N. G.

2017-12-01

A gallium nitride crystal 5 mm in thickness was grown by chloride-hydride vapor-phase epitaxy on a sapphire substrate, from which the crystal separated during cooling. At an early stage, a three-dimensional growth mode was implemented, followed by a switch to a two-dimensional mode. Spectra of exciton reflection, exciton luminescence, and Raman scattering are studied in several regions characteristic of the sample. Analysis of these spectra and comparison with previously obtained data for thin epitaxial GaN layers with a wide range of silicon doping enabled conclusions about the quality of the crystal lattice in these characteristic regions.

Optical Probing of Low-Pressure Solution Grown GaN Crystal Properties

DTIC Science & Technology

2010-04-01

observed in Mg and Si doped epitaxial films deposited by MBE and MOCVD on freestanding GaN HVPE substrates [23–25]. Considering the purity of the precursors...bands with similar energy positions here reported, a dominant deeper acceptor impurity has been assigned to Zn , a well known deep acceptor in GaN . Room...00-00-2010 to 00-00-2010 4. TITLE AND SUBTITLE Optical probing of low-pressure solution grown GaN crystal properties 5a. CONTRACT NUMBER 5b

Photoluminescence and lasing properties of MAPbBr3 single crystals grown from solution

NASA Astrophysics Data System (ADS)

Aryal, Sandip; Lafalce, Evan; Zhang, Chuang; Zhai, Yaxin; Vardeny, Z. Valy

Recent studies of solution-grown single crystals of inorganic-organic hybrid lead-trihalide perovskites have suggested that surface traps may play a significant role in their photophysics. We study electron-hole recombination in single crystal MAPbBr3 through such trap states using cw photoluminescence (PL) and ps transient photoinduced absorption (PA) spectroscopies. By varying the depth of the collecting optics we examined the contributions from surface and bulk radiative recombination. We found a surface dominated PL band at the band-edge that is similar to that observed from polycrystalline thin films, as well as a weaker red-shifted emission band that originates from the bulk crystal. The two PL bands are distinguished in their temperature, excitation intensity and polarization dependencies, as well as their ps dynamics. Additionally, amplified spontaneous emission and crystal-related cavity lasing modes were observed in the same spectral range as the PL band assigned to the surface recombination. This work was funded by AFOSR through MURI Grant RA 9550-14-1-0037.

Microgravity

NASA Image and Video Library

1994-02-01

The comparison of protein crystal, Recombiant Human Insulin; space-grown (left) and earth-grown (right). On STS-60, Spacehab II indicated that space-grown crystals are larger and of greater optical clarity than their earth-grown counterparts. Recombiant Human Insulin facilitates the incorporation of glucose into cells. In diabetics, there is either a decrease in or complete lack of insulin, thereby leading to several harmful complications. Principal Investigator is Larry DeLucas.

The effect of deuteration and doping on the phase transition temperature of grown glycine phosphite single crystals

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

Perumal, R., E-mail: perumal-cgc@yahoo.co.uk; Chandru, A. Lakshmi; Babu, S. Moorthy

The Glycinium Phosphite (GPI) compound is a representative of hydrogen-bonded ferroelectric crystals. The ordering of protons could be expected below the room temperature (225 K). Crystals grown from the milipore water as well as deuterated solvents respectively. The corresponding hydrogen bond distance was stretched out due to the effect of isotopic substitution that increase the phase transition temperature. Further to improve the phase transition temperature, GPI crystal was doped with organic complexing agent and various metals and the obtained results are presented.

High quality self-separated GaN crystal grown on a novel nanoporous template by HVPE.

PubMed

Huo, Qin; Shao, Yongliang; Wu, Yongzhong; Zhang, Baoguo; Hu, Haixiao; Hao, Xiaopeng

2018-02-16

In this study, a novel nanoporous template was obtained by a two-step etching process from MOCVD-GaN/Al 2 O 3 (MGA) with electrochemical etching sequentially followed by chemical wet etching. The twice-etched MOCVD-GaN/Al 2 O 3 (TEMGA) templates were utilized to grow GaN crystals by hydride vapor phase epitaxy (HVPE) method. The GaN crystals were separated spontaneously from the TEMGA template with the assistance of voids formed by the etched nanopores. Several techniques were utilized to characterize the quality of the free-standing GaN crystals obtained from the TEMGA template. Results showed that the quality of the as-obtained GaN crystals was improved obviously compared with those grown on the MGA. This convenient technique can be applied to grow high-quality free-standing GaN crystals.

Thermoluminescence and optically stimulated luminescence disadvantages of α-Al2O3:C crystal grown by the temperature gradient technique

NASA Astrophysics Data System (ADS)

Yang, Xin-Bo; Xu, Jun; Li, Hong-Jun; Bi, Qun-Yu; Cheng, Yan; Su, Liang-Bi; Tang, Qiang

2010-04-01

Recently, α-Al2O3:C crystal with highly sensitive thermoluminescence (TL) and optically stimulated luminescence (OSL) has been successfully grown by the temperature gradient technique. This paper investigates the heating rate dependence of TL sensitivity, light-induced fading of TL signals and thermal stability of OSL of α-Al2O3:C crystals. As the heating rate increases, the integral TL response decreases and the dosimetric glow peak shifts to higher temperatures in α-Al2O3:C crystals. Light-induced fading of TL increases with the irradiation dose, and TL response decreases as the exposure time increases, especially in the first 15 minutes. With the increasing intensity of the exposure light, the TL fading of α-Al2O3:C crystal increases sharply. The OSL response of as-grown α-Al2O3:C crystal is quite stable below 373 K and decreases sharply for higher temperatures.

Protein Crystal Growth (PCG)Insulin Crystals

NASA Technical Reports Server (NTRS)

1991-01-01

Facilitates the incorporation of glucose into cells. In diabetics, there is either a decrease in or complete lack of insulin, therby leading to several harmful complications. Principal Investigator was Charles Bugg.

Positron annihilation on the surfaces of SiO 2 films thermally grown on single crystal of Cz-Si

NASA Astrophysics Data System (ADS)

Deng, Wen; Yue, Li; Zhang, Wei; Cheng, Xu-xin; Zhu, Yan-yan; Huang, Yu-yang

2009-09-01

Two-detector coincidence system and mono-energetic slow positron beam has been applied to measure the Doppler broadening spectra for single crystals of SiO2, SiO2 films with different thickness thermally grown on single crystal of Cz-Si, and single crystal of Si without oxide film. Oxygen is recognized as a peak at about 11.85 × 10-3m0c on the ratio curves. The S parameters decrease with the increase of positron implantation energy for the single crystal of SiO2 and Si without oxide film. However, for the thermally grown SiO2-Si sample, the S parameters in near surface of the sample increase with positron implantation energy. It is due to the formation of silicon oxide at the surface, which lead to lower S value. S and W parameters vary with positron implantation depth indicate that the SiO2-Si system consist of a surface layer, a SiO2 layer, a SiO2-Si interface layer and a semi-infinite Si substrate.

The investigation of stress in freestanding GaN crystals grown from Si substrates by HVPE.

PubMed

Lee, Moonsang; Mikulik, Dmitry; Yang, Mino; Park, Sungsoo

2017-08-17

We investigate the stress evolution of 400 µm-thick freestanding GaN crystals grown from Si substrates by hydride vapour phase epitaxy (HVPE) and the in situ removal of Si substrates. The stress generated in growing GaN can be tuned by varying the thickness of the MOCVD AlGaN/AlN buffer layers. Micro Raman analysis shows the presence of slight tensile stress in the freestanding GaN crystals and no stress accumulation in HVPE GaN layers during the growth. Additionally, it is demonstrated that the residual tensile stress in HVPE GaN is caused only by elastic stress arising from the crystal quality difference between Ga- and N-face GaN. TEM analysis revealed that the dislocations in freestanding GaN crystals have high inclination angles that are attributed to the stress relaxation of the crystals. We believe that the understanding and characterization on the structural properties of the freestanding GaN crystals will help us to use these crystals for high-performance opto-electronic devices.

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

NASA Technical Reports Server (NTRS)

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

1997-01-01

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

On the Chemistry and Physical Properties of Flux and Floating Zone Grown SmB6 Single Crystals

PubMed Central

Phelan, W. A.; Koohpayeh, S. M.; Cottingham, P.; Tutmaher, J. A.; Leiner, J. C.; Lumsden, M. D.; Lavelle, C. M.; Wang, X. P.; Hoffmann, C.; Siegler, M. A.; Haldolaarachchige, N.; Young, D. P.; McQueen, T. M.

2016-01-01

Recent theoretical and experimental findings suggest the long-known but not well understood low temperature resistance plateau of SmB6 may originate from protected surface states arising from a topologically non-trivial bulk band structure having strong Kondo hybridization. Yet others have ascribed this feature to impurities, vacancies, and surface reconstructions. Given the typical methods used to prepare SmB6 single crystals, flux and floating-zone procedures, such ascriptions should not be taken lightly. We demonstrate how compositional variations and/or observable amounts of impurities in SmB6 crystals grown using both procedures affect the physical properties. From X-ray diffraction, neutron diffraction, and X-ray computed tomography experiments we observe that natural isotope containing (SmB6) and doubly isotope enriched (154Sm11B6) crystals prepared using aluminum flux contain co-crystallized, epitaxial aluminum. Further, a large, nearly stoichiometric crystal of SmB6 was successfully grown using the float-zone technique; upon continuing the zone melting, samarium vacancies were introduced. These samarium vacancies drastically alter the resistance and plateauing magnitude of the low temperature resistance compared to stoichiometric SmB6. These results highlight that impurities and compositional variations, even at low concentrations, must be considered when collecting/analyzing physical property data of SmB6. Finally, a more accurate samarium-154 coherent neutron scattering length, 8.9(1) fm, is reported. PMID:26892648

The optical properties of CdS crystal grown by the sublimation method

NASA Astrophysics Data System (ADS)

Hong, K. J.; Jeong, T. S.; Yoon, C. J.; Shin, Y. J.

2000-09-01

A cadmium sulfide (CdS) single crystal was grown by the sublimation method without a seed crystal in a two-stage vertical electric furnace. The carrier concentration and mobility obtained from Hall measurements at room temperature were 2.90 ×10 16 cm-3 and 316 cm 2/V s, respectively. The photoluminescence and the photocurrent measurement of the CdS single crystal have been performed in the temperature ranging from 20 to 293 K. From the photoluminescence measurement, the energy of the free exciton Ex(A) and Ex(B) has been obtained to be 2.5511 and 2.5707 eV, respectively. The variance of the peak position, intensity, and linewidth of the free excitons as a function of the temperature have been investigated by means of the conventional empirical relations and Toyozawa's theory. The crystal field of the CdS and its splitting energy, Δ cr, have been found to be 19.6 meV. In the photocurrent measurement, only the Ex(A) exciton peak has been observed. The energy band gap of the CdS at room temperature was determined to be 2.4749 eV by the photoluminescence and photocurrent measurement. Also, the temperature dependence of the energy band gap of the CdS, Eg( T), has been examined.

Structural characterization of bulk GaN crystals grown under high hydrostatic pressure

NASA Astrophysics Data System (ADS)

Liliental-Weber, Zuzanna; Kisielowski, C.; Ruvimov, S.; Chen, Y.; Washburn, J.; Grzegory, I.; Bockowski, M.; Jun, J.; Porowski, S.

1996-09-01

This paper describes TEM characterization of bulk GaN crystals grown at 1500-1800Kin the form of plates from a solution of atomic nitrogen in liquid gallium under high nitrogen pressure (up to 20 kbars). The x-ray rocking curves for these crystals were in the range of 20-30 arc-sec. The plate thickness along the c axis was about 100 times smaller than the nonpolar growth directions. A substantial difference in material quality was observed on the opposite sides of the plates normal to the c direction. On one side the surface was atomically flat, while on the other side the surface was rough, with pyramidal features up to 100 nm high. The polarity of the crystals was determined using convergent-beam electron diffraction. The results showed that, regarding the long bond between Ga and N along the c-axis, Ga atoms were found to be closer to the flat side of the crystal, while N atoms were found to be closer to the rough side. Near the rough side, within 1/10 to 1/4 of the plate thickness, there was a high density of planar defects (stacking faults and dislocation loops decorated by Ga/void precipitates). A model explaining the defect formation is proposed.

Characterization of Cadmium-Zinc Telluride Crystals Grown by 'Contactless' PVT Using Synchrotron White Beam Topography

NASA Technical Reports Server (NTRS)

Palosz, W.; Gillies, D.; Grasza, K.; Chung, H.; Raghothamachar, B.; Dudley, M.

1997-01-01

Crystals of Cd(1-x)Zn(x)Te grown by Physical Vapor Transport (PVT) using self-seeding 'contactless' techniques were characterized using synchrotron radiation (reflection, transmission, and Laue back-reflection X-ray topography). Crystals of low (x = 0.04) and high (up to x approx. = 0.4) ZnTe content were investigated. Twins and defects such as dislocations, precipitates, and slip bands were identified. Extensive inhomogeneous strains present in some samples were found to be generated by interaction (sticking) with the pedestal and by composition gradients in the crystals. Large (up to about 5 mm) oval strain fields were observed around some Te precipitates. Low angle grain boundaries were found only in higher ZnTe content (x greater than or equal to 0.2) samples.

On the Chemistry and Physical Properties of Flux and Floating Zone Grown SmB 6 Single Crystals

DOE PAGES

Phelan, W. A.; Koohpayeh, S. M.; Cottingham, P.; ...

2016-02-19

Recent theoretical and experimental findings suggest the long-known but not well understood low temperature resistance plateau of SmB 6 may originate from protected surface states arising from a topologically non-trivial bulk band structure having strong Kondo hybridization. Yet others have ascribed this feature to impurities, vacancies, and surface reconstructions. Given the typical methods used to prepare SmB 6 single crystals, flux and floating-zone procedures, such ascriptions should not be taken lightly. We demonstrate how compositional variations and/or observable amounts of impurities in SmB 6 crystals grown using both procedures affect the physical properties. From X-ray diffraction, neutron diffraction, and X-raymore » computed tomography experiments we observe that natural isotope containing (SmB 6) and doubly isotope enriched ( 154Sm 11B 6) crystals prepared using aluminum flux contain co-crystallized, epitaxial aluminum. Further, a large, nearly stoichiometric crystal of SmB 6 was successfully grown using the float-zone technique; upon continuing the zone melting, samarium vacancies were introduced. These samarium vacancies drastically alter the resistance and plateauing magnitude of the low temperature resistance compared to stoichiometric SmB 6. Finally, these results highlight that impurities and compositional variations, even at low concentrations, must be considered when collecting/analyzing physical property data of SmB 6. Finally, a more accurate samarium-154 coherent neutron scattering length, 8.9(1) fm, is reported.« less

Structural Characterization of Lateral-grown 6H-SiC am-plane Seed Crystals by Hot Wall CVD Epitaxy

NASA Technical Reports Server (NTRS)

Goue, Ouloide Yannick; Raghothamachar, Balaji; Dudley, Michael; Trunek, Andrew J.; Neudeck, Philip G.; Woodworth, Andrew A.; Spry, David J.

2014-01-01

The performance of commercially available silicon carbide (SiC) power devices is limited due to inherently high density of screw dislocations (SD), which are necessary for maintaining polytype during boule growth and commercially viable growth rates. The NASA Glenn Research Center (GRC) has recently proposed a new bulk growth process based on axial fiber growth (parallel to the c-axis) followed by lateral expansion (perpendicular to the c-axis) for producing multi-faceted m-plane SiC boules that can potentially produce wafers with as few as one SD per wafer. In order to implement this novel growth technique, the lateral homoepitaxial growth expansion of a SiC fiber without introducing a significant number of additional defects is critical. Lateral expansion is being investigated by hot wall chemical vapor deposition (HWCVD) growth of 6H-SiC am-plane seed crystals (0.8mm x 0.5mm x 15mm) designed to replicate axially grown SiC single crystal fibers. The post-growth crystals exhibit hexagonal morphology with approximately 1500 m (1.5 mm) of total lateral expansion. Preliminary analysis by synchrotron white beam x-ray topography (SWBXT) confirms that the growth was homoepitaxial, matching the polytype of the respective underlying region of the seed crystal. Axial and transverse sections from the as grown crystal samples were characterized in detail by a combination of SWBXT, transmission electron microscopy (TEM) and Raman spectroscopy to map defect types and distribution. X-ray diffraction analysis indicates the seed crystal contained stacking disorders and this appears to have been reproduced in the lateral growth sections. Analysis of the relative intensity for folded transverse acoustic (FTA) and optical (FTO) modes on the Raman spectra indicate the existence of stacking faults. Further, the density of stacking faults is higher in the seed than in the grown crystal. Bundles of dislocations are observed propagating from the seed in m-axis lateral directions

Structural and photoluminescence studies on europium-doped lithium tetraborate (Eu:Li2B4O7) single crystal grown by microtube Czochralski (μT-Cz) technique

NASA Astrophysics Data System (ADS)

A, Kumaresh; R, Arun Kumar; N, Ravikumar; U, Madhusoodanan; B, S. Panigrahi; K, Marimuthu; M, Anuradha

2016-05-01

Rare earth europium (Eu3+)-doped lithium tetraborate (Eu:Li2B4O7) crystal is grown from its stoichiometric melt by microtube Czochralski pulling technique (μT-Cz) for the first time. The grown crystals are subjected to powder x-ray diffraction (PXRD) analysis which reveals the tetragonal crystal structure of the crystals. UV-vis-NIR spectral analysis is carried out to study the optical characteristics of the grown crystals. The crystal is transparent in the entire visible region, and the lower cutoff is observed to be at 304 nm. The existence of BO3 and BO4 bonding structure and the molecular associations are analyzed by Fourier transform infrared (FTIR) spectroscopy. The results of excitation and emission-photoluminescence spectra of europium ion incorporated in lithium tetraborate (LTB) single crystal reveal that the observations of peaks at 258, 297, and 318 nm in the excitation spectra and peaks at 579, 591, 597, 613, and 651 nm are observed in the emission spectra. The chromaticity coordinates are calculated from the emission spectra, and the emission intensity of the grown crystal is characterized through a CIE 1931 (Commission International d’Eclairage) color chromaticity diagram. Project supported by the Department of Science and Technology-Science and Engineering Research Board (Grant No. SR/S2/LOP-0012/2011), the Government of India for Awarding Major Research Project, the University Grants Commission-Department of Atomic Research-Consortium for Scientific Research (Grant No. CSR-KN/CSR-63/2014-2015/503), and the Kalpakkam and Indore, India.

Dielectric properties of highly resistive GaN crystals grown by ammonothermal method at microwave frequencies

NASA Astrophysics Data System (ADS)

Krupka, Jerzy; Zajåc, Marcin; Kucharski, Robert; Gryglewski, Daniel

2016-03-01

Permittivity, the dielectric loss tangent and conductivity of semi-insulating Gallium Nitride crystals have been measured as functions of frequency from 10 GHz to 50 GHz and temperature from 295 to 560 K employing quasi TE0np mode dielectric resonator technique. Crystals were grown using ammonothermal method. Two kinds of doping were used to obtain high resistivity crystals; one with deep acceptors in form of transition metal ions, and the other with shallow Mg acceptors. The sample compensated with transition metal ions exhibited semi-insulating behavior in the whole temperature range. The sample doped with Mg acceptors remained semi-insulating up to 390 K. At temperatures exceeding 390 K the conductivity term in the total dielectric loss tangent of Mg compensated sample becomes dominant and it increases exponentially with activation energy of 1.14 eV. It has been proved that ammonothermal method with appropriate doping allows growth of high quality, temperature stable semi-insulating GaN crystals.

Vertically grown nanowire crystals of dibenzotetrathienocoronene (DBTTC) on large-area graphene

DOE PAGES

Kim, B.; Chiu, C. -Y.; Kang, S. J.; ...

2016-06-01

Here we demonstrate controlled growth of vertical organic crystal nanowires on single layer graphene. Using Scanning Electron Microscopy (SEM), high-resolution transition electron microscopy (TEM), and Grazing Incidence X-ray Diffraction (GIXD), we probe the microstructure and morphology of dibenzotetrathienocoronene (DBTTC) nanowires epitaxially grown on graphene. The investigation is performed at both the ensemble and single nanowire level, and as function of growth parameters, providing insight of and control over the formation mechanism. Finally, the size, density and height of the nanowires can be tuned via growth conditions, opening new avenues for tailoring three-dimensional (3-D) nanostructured architectures for organic electronics with improvedmore » functional performance.« less

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.

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.

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, structure analysis and characterisation of 2 - (1, 3 - dioxoisoindolin - 2 - yl) acetic acid single crystal

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

Sankari, R. Siva, E-mail: sivasankari.sh@act.edu.in; Perumal, Rajesh Narayana

2014-04-24

Single crystal of dielectric material 2 - (1, 3 - dioxoisoindolin - 2 - yl) acetic acid has been grown by slow evaporation solution growth method. The grown crystal was harvested in 25 days. The crystal structure was analyzed by Single crystal X - ray diffraction. UV-vis-NIR analysis was performed to examine the optical property of the grown crystal. The thermal property of the grown crystal was studied by thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The dielectric measurements were carried out and the dielectric constant was calculated and plotted at all frequencies.

Crystal growth, spectral, structural and optical studies of π-conjugated stilbazolium crystal: 4-bromobenzaldehyde-4'-N'-methylstilbazolium tosylate.

PubMed

Krishna Kumar, M; Sudhahar, S; Bhagavannarayana, G; Mohan Kumar, R

2014-05-05

Nonlinear optical (NLO) organic compound, 4-bromobenzaldehyde-4'-N'-methylstilbazolium tosylate was synthesized by reflux method. The formation of molecular complex was confirmed from (1)H NMR, FT-IR and FT-Raman spectral analyses. The single crystals were grown by slow evaporation solution growth method and the crystal structure and atomic packing of grown crystal was identified. The morphology and growth axis of grown crystal were determined. The crystal perfection was analyzed using high resolution X-ray diffraction study on (001) plane. Thermal stability, decomposition stages and melting point of the grown crystal were analyzed. The optical absorption coefficient (α) and energy band gap (E(g)) of the crystal were determined using UV-visible absorption studies. Second harmonic generation efficiency of the grown crystal was examined by Kurtz powder method with different particle size using 1064 nm laser. Laser induced damage threshold study was carried out for the grown crystal using Nd:YAG laser. Copyright © 2014 Elsevier B.V. All rights reserved.

Conformational Dynamics of Insulin

PubMed Central

Hua, Qing-Xin; Jia, Wenhua; Weiss, Michael A.

2011-01-01

We have exploited a prandial insulin analog to elucidate the underlying structure and dynamics of insulin as a monomer in solution. A model was provided by insulin lispro (the active component of Humalog®; Eli Lilly and Co.). Whereas NMR-based modeling recapitulated structural relationships of insulin crystals (T-state protomers), dynamic anomalies were revealed by amide-proton exchange kinetics in D2O. Surprisingly, the majority of hydrogen bonds observed in crystal structures are only transiently maintained in solution, including key T-state-specific inter-chain contacts. Long-lived hydrogen bonds (as defined by global exchange kinetics) exist only at a subset of four α-helical sites (two per chain) flanking an internal disulfide bridge (cystine A20–B19); these sites map within the proposed folding nucleus of proinsulin. The anomalous flexibility of insulin otherwise spans its active surface and may facilitate receptor binding. Because conformational fluctuations promote the degradation of pharmaceutical formulations, we envisage that “dynamic re-engineering” of insulin may enable design of ultra-stable formulations for humanitarian use in the developing world. PMID:22649374

Crystal orientation, crystallinity, and thermoelectric properties of Bi0.9Sr0.1CuSeO epitaxial films grown by pulsed laser deposition

NASA Astrophysics Data System (ADS)

Ishizawa, Mamoru; Fujishiro, Hiroyuki; Naito, Tomoyuki; Ito, Akihiko; Goto, Takashi

2018-02-01

We have grown Bi0.9Sr0.1CuSeO epitaxial thin films on MgO and SrTiO3 (STO) single-crystal substrates by pulsed laser deposition (PLD) under various growth conditions, and investigated the crystal orientation, crystallinity, chemical composition, and thermoelectric properties of the films. The optimization of the growth conditions was realized in the film grown on MgO at the temperature T s = 573 K and Ar pressure P Ar = 0.01 Torr in this study, in which there was no misalignment apart from the c-axis and no impurity phase. It was clearly found that the higher crystal orientation of the epitaxial film grown at a higher temperature under a lower Ar pressure mainly enhanced the thermoelectric power factor P (= S 2/ρ), where S is the Seebeck coefficient and ρ is the electrical resistivity. However, the thermoelectric properties of the films were lower than those of polycrystalline bulk because of lattice distortion from lattice mismatch, a low crystallinity caused by a lower T s, and Bi and Cu deficiencies in the films.

The Effect of the Wall Contact and Post-Growth, Cool-Down on Defects in CdTe Crystals Grown By 'Contactless' PVT

NASA Technical Reports Server (NTRS)

Palosz, W.; Grasza, K.; Dudley, M.; Raghothamachar, B.; Cai, L.; Dunrose, K.; Halliday, D.; Boyall, N. M.; Rose, M. Franklin (Technical Monitor)

2001-01-01

To take a maximum advantage of materials processing in microgravity for understanding the effects of gravity, gravity-independent effects should be minimized. In crystal growth, the quality of the grown crystals may depend, among other factors, on their interaction with the walls of the processing container during and after growth, and on the rate of the crystal cool-down at the end of the process. To investigate the above phenomena, a series of CdTe crystal growth processes was carried out. The crystals were grown by physical vapor transport without contact with the side walls of the silica glass ampoules. To eliminate the effect of the seed quality, and to reduce the number of nuclei and related crystal grains, the Low Supersaturation Nucleation technique was applied. The source temperature was 930 C, the undercooling was a few degrees. The crystals, having the diameter of 25 mm, grew at the rate of a few mm per day. The post-growth cool-down to the room temperature was conducted at different rates, and lasted from a few minutes to four days. The crystals were characterized using chemical etching, low temperature luminescence, and Synchrotron White Beam X-ray Topography techniques. The dislocation (etch pit) density was measured and its distribution was analyzed by comparison with Poisson curves and with the Normalized Radial Distribution Correlation Function. In the regions where the crystal is in contact with silica, the materials show a considerable strain field which extends for a few mm or more from the silica-crystal interface. In the reference crystal grown with contact with the ampoule walls, and when the crystals are cooled at the highest rates, the etch pit/dislocation density is in the high 10(exp 5) per square centimeter region. Typical EPD values for lower cool-down rates are in the lower 10(exp 4) per square centimeter region. In some areas the actual dislocation density was about 10(exp 3) per square centimeter or even less. No apparent effect of

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.

Evidence for graphite-like hexagonal AlN nanosheets epitaxially grown on single crystal Ag(111)

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

Tsipas, P.; Kassavetis, S.; Tsoutsou, D.

Ultrathin (sub-monolayer to 12 monolayers) AlN nanosheets are grown epitaxially by plasma assisted molecular beam epitaxy on Ag(111) single crystals. Electron diffraction and scanning tunneling microscopy provide evidence that AlN on Ag adopts a graphite-like hexagonal structure with a larger lattice constant compared to bulk-like wurtzite AlN. This claim is further supported by ultraviolet photoelectron spectroscopy indicating a reduced energy bandgap as expected for hexagonal AlN.

GaAs/Ge crystals grown on Si substrates patterned down to the micron scale

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

Taboada, A. G., E-mail: gonzalez@phys.ethz.ch; Kreiliger, T.; Falub, C. V.

Monolithic integration of III-V compounds into high density Si integrated circuits is a key technological challenge for the next generation of optoelectronic devices. In this work, we report on the metal organic vapor phase epitaxy growth of strain-free GaAs crystals on Si substrates patterned down to the micron scale. The differences in thermal expansion coefficient and lattice parameter are adapted by a 2-μm-thick intermediate Ge layer grown by low-energy plasma enhanced chemical vapor deposition. The GaAs crystals evolve during growth towards a pyramidal shape, with lateral facets composed of (111) planes and an apex formed by (137) and (001) surfaces.more » The influence of the anisotropic GaAs growth kinetics on the final morphology is highlighted by means of scanning and transmission electron microscopy measurements. The effect of the Si pattern geometry, substrate orientation, and crystal aspect ratio on the GaAs structural properties was investigated by means of high resolution X-ray diffraction. The thermal strain relaxation process of GaAs crystals with different aspect ratio is discussed within the framework of linear elasticity theory by Finite Element Method simulations based on realistic geometries extracted from cross-sectional scanning electron microscopy images.« less

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.

Crystal growth of artificial snow

NASA Technical Reports Server (NTRS)

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

1984-01-01

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

Growth, piezoelectric study and particle size dependent SHG of an 80 mm long SR grown imidazolium l-tartrate single crystals

NASA Astrophysics Data System (ADS)

Jauhar, RO MU; Era, Paavai; Murugakoothan, P.

2018-05-01

Single crystal of imidazolium l-tartrate (IMLT), an organic nonlinear optical material, was successfully grown by slow evaporation solution growth technique (SEST) and Sankaranarayanan - Ramasamy (SR) method. The crystal structure and its lattice parameters were confirmed by single crystal X-ray diffraction study. The IMLT crystal belongs to monoclinic crystal system having a = 7.579(6) Å, b = 6.911(4) Å, c = 8.9281(5) Å, β = 101.45(8)°, volume, V = 458.33 Å3. The d33 coefficient found from the the piezoelectric study is 23 pC/N. The relative second harmonic generation efficiency of IMLT was found to be 3.16 times that of reference KDP material.

Single Crystals Grown Under Unconstrained Conditions

NASA Astrophysics Data System (ADS)

Sunagawa, Ichiro

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

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.

Crystal growth and characterization of third order nonlinear optical piperazinium bis(4-hydroxybenzenesulphonate) (P4HBS) single crystal

NASA Astrophysics Data System (ADS)

Pichan, Karuppasamy; Muthu, Senthil Pandian; Perumalsamy, Ramasamy

2017-09-01

The organic single crystal of piperazinium bis(4-hydroxybenzenesulphonate) (P4HBS) was grown by slow evaporation solution technique (SEST) at room temperature. The lattice parameters of the grown crystal were confirmed by single crystal X-ray diffraction analysis. Functional groups of P4HBS crystal were confirmed by FTIR spectrum analysis. The optical quality of the grown crystal was identified by the UV-Vis NIR spectrum analysis. The grown crystal has good optical transmittance in the range of 410-1100 nm. In photoluminescence spectrum, sharp emission peaks are observed, which indicates the ultraviolet (UV) emission. The photoconductivity study reveals that the grown crystal has negative photoconductive nature. The thermal behaviour of the P4HBS crystal was investigated by thermogravimetric and differential thermal analysis (TG-DTA). The mechanical stability of grown crystal was analyzed and the indentation size effect (ISE) was explained by Hays-Kendall's (HK) approach and proportional specimen resistance model (PSRM). Chemical etching study was carried out and the etch pit density (EPD) was calculated. The dielectric constant (ε‧) and dielectric loss (tan δ) as a function of frequency were measured for the grown crystal. The solid state parameters such as valence electron, plasma energy, Penn gap and Fermi energy were evaluated theoretically for the P4HBS using the empirical relation. The estimated values are used to calculate the electronic polarizability. 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 632.8 nm using He-Ne laser.

Crystal structure and properties of tetragonal EuAg{sub 4}In{sub 8} grown by metal flux technique

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

Subbarao, Udumula; Sarkar, Sumanta; Peter, Sebastian C., E-mail: sebastiancp@jncasr.ac.in

The compound EuAg{sub 4}In{sub 8} has been obtained as single crystals in high yield from reactions run in liquid indium. X-ray diffraction on single crystals suggests that EuAg{sub 4}In{sub 8} crystallizes in the CeMn{sub 4}Al{sub 8} structure type, tetragonal space group I4/mmm with lattice constants a=b=9.7937(2) Å and c=5.7492(2) Å. Crystal structure of EuAg{sub 4}In{sub 8} is composed of pseudo Frank–Kasper cages occupied by one europium atom in each ring, which are shared through the corner along the ab plane resulting in a three dimensional network. The magnetic susceptibility of EuAg{sub 4}In{sub 8} was measured in the temperature range 2–300more » K, which obeyed Curie–Weiss law above 50 K. Magnetic moment value calculated from the fitting indicates the presence of divalent europium, which was confirmed by X-ray absorption near edge spectroscopy. Electrical resistivity measurements suggest that EuAg{sub 4}In{sub 8} is metallic in nature with a probable Fermi liquid behavior at low temperature. - Graphical abstract: The tetragonal EuAg{sub 4}In{sub 8} has been grown as single crystals from reactions run in liquid indium. Magnetic and XANES measurements suggest divalent nature of Eu and resistivity measurements suggest metallic nature. - Highlights: • EuAg{sub 4}In{sub 8} phase having tetragonal phase is grown by metal flux technique. • Magnetic and XANES measurements exhibit divalent nature of Eu in EuAg{sub 4}In{sub 8}. • Resistivity measurement suggests metallic nature and probable Fermi liquid behavior.« less

Optical spectroscopy of bulk GaN crystals grown from a Na-Ga melt

NASA Astrophysics Data System (ADS)

Skromme, B. J.; Palle, K. C.; Poweleit, C. D.; Yamane, H.; Aoki, M.; DiSalvo, F. J.

2002-11-01

Colorless transparent platelet and prismatic GaN crystals up to 3-4 mm, grown from a Na-Ga melt (0.6-0.7 mol fraction of Na) at temperatures of 700-800 °C in a modest (5 MPa) pressure of N2, are characterized using Raman scattering, room and low temperature photoluminescence, and reflectance. They exhibit sharp free and bound exciton luminescence features (down to 0.22 meV full width at half maximum), including multiple excited states. Residual Mg and Zn acceptors and a 33.6 meV donor (possibly ON) are identified. Raman spectra suggest free carrier concentrations down to the low to mid 1016 cm-3 range.

GaN Schottky diodes with single-crystal aluminum barriers grown by plasma-assisted molecular beam epitaxy

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

Tseng, H. Y.; Yang, W. C.; Lee, P. Y.

2016-08-22

GaN-based Schottky barrier diodes (SBDs) with single-crystal Al barriers grown by plasma-assisted molecular beam epitaxy are fabricated. Examined using in-situ reflection high-energy electron diffractions, ex-situ high-resolution x-ray diffractions, and high-resolution transmission electron microscopy, it is determined that epitaxial Al grows with its [111] axis coincident with the [0001] axis of the GaN substrate without rotation. In fabricated SBDs, a 0.2 V barrier height enhancement and 2 orders of magnitude reduction in leakage current are observed in single crystal Al/GaN SBDs compared to conventional thermal deposited Al/GaN SBDs. The strain induced piezoelectric field is determined to be the major source of themore » observed device performance enhancements.« less

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.

RNi2B2C (R = Ho, Dy, Tb and Pr) single crystals grown by the cold copper crucible method

NASA Astrophysics Data System (ADS)

Durán, A.; Munoz, E.; Bernès, S.; Escudero, R.

2000-08-01

Single crystals of RNi2B2C (R = Ho, Dy, Tb, Pr) have been grown on cold copper crucibles in a high-frequency induction furnace. As a result, shiny metallic and brittle platelike single crystals were obtained. They were examined by x-ray and scanning electron microscopy with WDX/EDX for local composition analysis and show a very good crystallographic structure and compositions. Resistivity and dc magnetic measurements were performed to study superconducting and magnetic properties. Besides known electronic properties of the RNi2B2C family, we report for the first time results for PrNi2B2C single crystals successfully obtained by this technique.

SEMICONDUCTOR MATERIALS: Chemical etching of a GaSb crystal incorporated with Mn grown by the Bridgman method under microgravity conditions

NASA Astrophysics Data System (ADS)

Xiaofeng, Chen; Nuofu, Chen; Jinliang, Wu; Xiulan, Zhang; Chunlin, Chai; Yude, Yu

2009-08-01

A GaSb crystal incorporated with Mn has been grown by the Bridgman method on the Polizon facility onboard the FOTON-M3 spacecraft. Structural defects and growth striations have been successfully revealed by the chemical etching method. By calculating various parameters of the convection, the striation patterns can be explained, and the critical value of the Taylor number, which characterizes the convective condition of the rotating magnetic field induced azimuthal flow, was shown. The stresses generated during crystal growth can be reflected by the observations of etch pit distribution and other structural defects. Suggestions for improving the space experiment to improve the quality of the crystal are given.

Synthesis, crystal structure, thermal and nonlinear optical properties of new metal-organic single crystal: Tetrabromo (piperazinium) zincate (II) (TBPZ)

NASA Astrophysics Data System (ADS)

Boopathi, K.; Babu, S. Moorthy; Ramasamy, P.

2018-04-01

Tetrabromo (piperazinium) zincate, a new metal-organic crystal has been synthesized and its single crystal grown by slow evaporation method. The grown crystal has characterized by structural, spectral, thermal, linear and nonlinear optical properties. Single crystal X-ray diffractions study reveals that grown crystal belongs to orthorhombic crystal system with space group P212121. The presence of functional groups is identified by FT-IR spectral analysis. Thermal stability of the crystal was ascertained by TG-DTA measurement. The second order harmonic generation efficiency was measured using Kurtz and Perry technique and it was found to be 1.5 times that of KDP.

Insulin at pH 2: structural analysis of the conditions promoting insulin fibre formation.

PubMed

Whittingham, Jean L; Scott, David J; Chance, Karen; Wilson, Ashley; Finch, John; Brange, Jens; Guy Dodson, G

2002-04-26

When insulin solutions are subjected to acid, heat and agitation, the normal pattern of insulin assembly (dimers-->tetramers-->hexamers) is disrupted; the molecule undergoes conformational changes allowing it to follow an alternative aggregation pathway (via a monomeric species) leading to the formation of insoluble amyloid fibres. To investigate the effect of acid pH on the conformation and aggregation state of the protein, the crystal structure of human insulin at pH 2.1 has been determined to 1.6 A resolution. The structure reveals that the native fold is maintained at low pH, and that the molecule is still capable of forming dimers similar to those found in hexameric insulin structures at higher pH. Sulphate ions are incorporated into the molecule and the crystal lattice where they neutralise positive charges on the protein, stabilising its structure and facilitating crystallisation. The sulphate interactions are associated with local deformations in the protein, which may indicate that the structure is more plastic at low pH. Transmission electron microscopy analysis of insulin fibres reveals that the appearance of the fibres is greatly influenced by the type of acid employed. Sulphuric acid produces distinctive highly bunched, truncated fibres, suggesting that the sulphate ions have a sophisticated role to play in fibre formation, rather as they do in the crystal structure. Analytical ultracentrifugation studies show that in the absence of heating, insulin is predominantly dimeric in mineral acids, whereas in acetic acid the equilibrium is shifted towards the monomer. Hence, the effect of acid on the aggregation state of insulin is also complex. These results suggest that acid conditions increase the susceptibility of the molecule to conformational change and dissociation, and enhance the rate of fibrillation by providing a charged environment in which the attractive forces between the protein molecules is increased. (c) 2002 Elsevier Science Ltd.

Crystallization of uric acid

NASA Astrophysics Data System (ADS)

Kalkura, S. Narayana; Vaidyan, V. K.; Kanakavel, M.; Ramasamy, P.

1993-09-01

Crystals of uric acid have been grown in tetra methoxy silane and silica gel medium. Small winged, transparent, platy crystals of uric acid of about 0.5x0.5x0.1 mm were grown and were found to be hydrated uric acid.

Influence of stress in GaN crystals grown by HVPE on MOCVD-GaN/6H-SiC substrate

PubMed Central

Zhang, Lei; Yu, Jiaoxian; Hao, Xiaopeng; Wu, Yongzhong; Dai, Yuanbin; Shao, Yongliang; Zhang, Haodong; Tian, Yuan

2014-01-01

GaN crystals without cracks were successfully grown on a MOCVD-GaN/6H-SiC (MGS) substrate with a low V/III ratio of 20 at initial growth. With a high V/III ratio of 80 at initial growth, opaque GaN polycrystals were obtained. The structural analysis and optical characterization reveal that stress has a great influence on the growth of the epitaxial films. An atomic level model is used to explain these phenomena during crystal growth. It is found that atomic mobility is retarded by compressive stress and enhanced by tensile stress. PMID:24569601

Optical, mechanical and thermal behaviors of Nitrilotriacetic acid single crystal

NASA Astrophysics Data System (ADS)

Deepa, B.; Philominathan, P.

2017-11-01

An organic nonlinear single crystal of Nitrilotriacetic acid (NTAA) was grown for the first time by employing a simple slow evaporation technique. Single crystal X-ray diffraction (XRD) analysis reveals that the grown crystal belongs to the monoclinic system with noncentrosymmetric space group CC. Fourier transform infrared (FTIR) spectral study ascertains the presence of functional groups in NTAA. The molecular structure of the grown crystal was confirmed by Nuclear Magnetic Resonance (NMR) spectral analysis. The optical parameters such as transmittance, absorption coefficient and band gap were calculated from UV-Visible and fluorescence studies. Dielectric measurements were carried out for different frequency and temperature. The mechanical strength of the grown crystal was measured using Vickers microhardness test. The high thermal stability and the melting point of the grown crystal were also estimated using thermogravimetric (TGA) and differential thermal analyses (DTA). The confirmation of the grown crystals belonging to nonlinear optical crystals was performed by Kurtz-Perry technique and found as suitable candidate for optoelectronics applications.

Zeolite Crystal Growth (ZCG) Flight on USML-2

NASA Technical Reports Server (NTRS)

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

1997-01-01

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

Crystal growth, structural, optical, mechanical and thermal properties of a new nonlinear optical single crystal: L-Ornithine monohydrochloride.

PubMed

Balakrishnan, T; Ramamurthi, K

2009-03-01

Amino acid family crystals exhibit excellent nonlinear optical and electro optical properties. l-Ornithine monohydrochloride single crystal, belongs to the amino acid group, was grown by the slow evaporation solution growth technique at room temperature. The grown crystals were characterized by single crystal and powder X-ray diffraction analysis, Fourier transform infrared (FTIR) spectroscopy, TGA, DTA and DSC analyses. UV-vis-NIR spectrum shows excellent transmission in the UV, visible and NIR region (300-1600nm). The mechanical properties of grown crystals were studied using Vickers microhardness tester. Its second harmonic generation efficiency was tested using Nd:YAG laser and is 1.25 times that of KDP.

Crystal-phase intergradation in InAs nanostructures grown by van der Waals heteroepitaxy on graphene

NASA Astrophysics Data System (ADS)

Choi, Ji Eun; Yoo, Jinkyoung; Lee, Donghwa; Hong, Young Joon; Fukui, Takashi

2018-04-01

This study demonstrates the crystal-phase intergradation of InAs nanostructures grown on graphene via van der Waals epitaxy. InAs nanostructures with diverse diameters are yielded on graphene. High-resolution transmission electron microscopy (HR-TEM) reveals two crystallographic features of (i) wurtzite (WZ)-to-zinc blende (ZB) intergradation along the growth direction of InAs nanostructures and (ii) an increased mean fraction of ZB according to diameter increment. Based on the HR-TEM observations, a crystal-phase intergradation diagram is depicted. We discuss how the formation of a WZ-rich phase during the initial growth stage is an effective way of releasing heterointerfacial stress endowed by the lattice mismatch of InAs/graphene for energy minimization in terms of less in-plane lattice mismatching between WZ-InAs and graphene. The WZ-to-ZB evolution is responsible for the attenuation of the bottom-to-top surface charge interaction as growth proceeds.

Magnetic and magnetostrictive behavior of Dy 3+ doped CoFe 2O 4 single crystals grown by flux method

NASA Astrophysics Data System (ADS)

Kambale, Rahul C.; Song, K. M.; Won, C. J.; Lee, K. D.; Hur, N.

2012-02-01

We studied the effect of Dy 3+ content on the magnetic properties of cobalt ferrite single crystal. The single crystals of CoFe 1.9Dy 0.1O 4 were grown by the flux method using Na 2B 4O 7.10 H 2O (Borax) as a solvent (flux). The black and shiny single crystals were obtained as a product. The X-ray diffraction analysis at room temperature confirmed the spinel cubic structure with lattice constant a=8.42 Å of the single crystals. The compositional analysis endorses the presence of constituents Co, Fe and Dy elements after sintering at 1300 °C within the final structure. The magnetic hysteresis measurements at various temperatures viz. 10 K, 100 K, 200 K and 300 K reveal the soft ferrimagnetic nature of the single crystal than that of for pure CoFe 2O 4. The observed saturation magnetization ( Ms) and coercivity ( Hc) are found to be lower than that of pure CoFe 2O 4 single crystal. The magnetostriction ( λ) measurement was carried out along the [001] direction. The magnetic measurements lead to conclude that the present single crystals can be used for magneto-optic recording media.

X-Ray Crystallographic Studies of Electrostatic Effects in Cubic Insulin

NASA Astrophysics Data System (ADS)

Gursky, Olga

1992-09-01

Cubic crystals of bovine insulin were obtained at pH 9 from sodium phosphate buffer. Pathway dependence of crystallization was analysed and crystallization using controlled nucleation was developed. Crystal stability and solubility were surveyed by dialysing the crystals against salt solutions varying in salt composition and ionic strength. Crystals dialysed in 0.1-0.2M Li, Na, K, Rb, NH(4) or Tl salt solutions at pH 9 diffracted to beyond 2.8A, while crystals dialysed in Cs, Mg, Ca or La rapidly lost lattice order. Change in the solvent anion did not affect crystal stability. Electron density maps calculated from X-ray data to 2.8A resolution showed two specific cation binding sites which may be occupied by monovalent cations with ionic radii <1.5A. One site lies between insulin dimers near crystallographic two-fold axis without the close involvement of protein charged groups. Cation binding at this site is important for crystal stability. The other site is alternatively occupied by B10 His in one of its two conformations. At pH 7, the Tl occupancy at both sites was decreased, at pH 9.5 the Tl occupancy of the site near B10 His was increased. The structure was refined using the refined model of cubic porcine insulin and the X-ray data collected to 2A resolution from a bovine insulin crystal at pH 9, to R = 16.1% for the data extending from 10A to 2A. High -resolution data from crystals at pH 7 and pH 10 were collected and analysed. The weights of the two B10 His conformers and the cation occupancy near B10 vary in the pH range from 7 to 10, indicating histidine titration. Shifts in the positions of B1-B4 at pH 7 suggest titration of the B-chain terminal amino groups. Co-operative conformational changes in the surface charged residues A1, A4, B21, B29, B30 at pH 10.2 suggest titration of the A-chain terminal amino groups. In several crystals treated with dichloroethane, the syn-dichloroethane was bound in the niche across the two-fold axis connecting insulin

Defect related electrical and optical properties of AlN bulk crystals grown by physical vapor transport

NASA Astrophysics Data System (ADS)

Irmscher, Klaus

AlN crystallizes thermodynamically stable in the wurtzite structure and possesses a direct band gap of about 6 eV. It is the ideal substrate for the epitaxial growth of Al-rich AlxGa1-xN films that enable deep ultraviolet (UV) emitters. Appropriate AlN bulk crystals can be grown by physical vapor transport (PVT). Besides high structural perfection, such substrate crystals should be highly UV transparent and ideally, electrically conductive. It is well known that point defects like impurities and intrinsic defects may introduce electronic energy levels within the bandgap, which lead to additional optical absorption or electrical compensation. Among the impurities, which may be incorporated into the AlN crystals during PVT growth at well above 2000 ° C, oxygen, carbon, and silicon play the major role. Based on our own experimental data as well as on experimental and theoretical results reported in literature, we discuss energy levels, charge states and possible negative-U behavior of these impurities and of vacancy-type defects. In particular, we develop a model that explains the absorption behavior of the crystals in dependence on the Fermi level that can be controlled by the growth conditions, including intentional doping. Further, we pay attention on spectroscopic investigations giving direct evidence for the chemical nature and atomic arrangement of the involved point defects. As examples local vibrational mode (LVM) spectroscopy of carbon related defects and recent reports of electron paramagnetic resonance (EPR) spectroscopy are discussed.

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.

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

NASA Astrophysics Data System (ADS)

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

2012-02-01

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

(PCG) Protein Crystal Growth HIV Reverse Transcriptase

NASA Technical Reports Server (NTRS)

1992-01-01

HIV Reverse Transcriptase crystals grown during the USML-1 (STS-50) mission using Commercial Refrigerator/Incubator Module (CR/IM) at 4 degrees C and the Vapor Diffusion Apparatus (VDA). Reverse transcriptase is an enzyme responsible for copying the nucleic acid genome of the AIDS virus from RNA to DNA. Studies indicated that the space-grown crystals were larger and better ordered (beyond 4 angstroms) than were comparable Earth-grown crystals. Principal Investigators were Charles Bugg and Larry DeLucas.

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.

Growth of propyl-p-hydroxybenzoate single crystals and its characterizations

NASA Astrophysics Data System (ADS)

Karunagaran, N.; Ramasamy, P.

2012-06-01

Single crystals of Propyl-p-hydroxybenzoate (PHB) crystals have been grown by slow evaporation solution technique (SEST) using methanol as a solvent. The PHB single crystal of dimension up to 27×16×8 mm3 has been grown in a period of 18 days at room temperature. The optical transparency of the grown PHB crystal has been measured on (212) plane by UV-Vis-NIR spectrophotometer. The crystal has 60% of transparency in the entire visible region. The thermo gravimetric analysis (TG) and differential thermal analysis (DTA) studies reveal that the crystal is thermally stable up to 99°C. The mechanical strength of the grown PHB crystal is measured using Vickers microhardness tester. The chemical etching studies were carried out on (212) plane using methanol etchant. The laser damage threshold of PHB crystal is 1.3 GW/cm2. The dielectric properties have been investigated. The birefringence value is found to be 0.10148 at the wavelength of 504 nm. The refractive index of grown PHB single crystal is 1.6753.

(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.

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

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

PubMed

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

2012-02-01

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

Toward understanding insulin fibrillation.

PubMed

Brange, J; Andersen, L; Laursen, E D; Meyn, G; Rasmussen, E

1997-05-01

Formation of insulin fibrils is a physical process by which partially unfolded insulin molecules interact with each other to form linear aggregates. Shielding of hydrophobic domains is the main driving force for this process, but formation of intermolecular beta-sheet may further stabilize the fibrillar structure. Conformational displacement of the B-chain C-terminal with exposure of nonpolar, aliphatic core residues, including A2, A3, B11, and B15, plays a crucial role in the fibrillation process. Recent crystal analyses and molecular modeling studies have suggested that when insulin fibrillates this exposed domain interacts with a hydrophobic surface domain formed by the aliphatic residues A13, B6, B14, B17, and B18, normally buried when three insulin dimers form a hexamer. In rabbit immunization experiments, insulin fibrils did not elicit an increased immune response with respect to formation of IgG insulin antibodies when compared with native insulin. In contrast, the IgE response increased with increasing content of insulin in fibrillar form. Strategies and practical approaches to prevent insulin from forming fibrils are reviewed. Stabilization of the insulin hexameric structure and blockage of hydrophobic interfaces by addition of surfactants are the most effective means of counteracting insulin fibrillation.

Advanced Protein Crystallization Facility (APCF)

NASA Technical Reports Server (NTRS)

1998-01-01

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

Shape Evolution of Detached Bridgman Crystals Grown in Microgravity

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.

2015-01-01

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

Structure and magnetic properties of flux grown single crystals of Co3-xFexSn2S2 shandites

NASA Astrophysics Data System (ADS)

Kassem, Mohamed A.; Tabata, Yoshikazu; Waki, Takeshi; Nakamura, Hiroyuki

2016-01-01

We report a successful single crystal growth of the shandite-type half-metallic ferromagnet Co3Sn2S2, and its Fe-substituted compounds, Co3-xFexSn2S2, by employing the flux method. Although Fe3Sn2S2 is unstable phase, we found that using the self Sn flux enables us to obtain single phase crystals up to x=0.53. The chemical composition of the grown plate-shaped single crystals was examined using wavelength-dispersive X-ray spectroscopy. The shandite structure with R 3 ̅m symmetry was confirmed by powder X-ray diffraction and the crystal structure parameters were refined using the Rietveld method. Magnetization measurements show suppression of the ferromagnetic order upon Fe-substitution , as well as in other substituted systems such as In- and Ni-substituted Co3Sn2S2. The almost identical magnetic phase diagrams of the Fe- and In-substituted compounds indicate that the electron number is dominantly significant to the magnetism in the Co-based shandite.

Structural studies of a crystalline insulin analog complex with protamine by atomic force microscopy.

PubMed Central

Yip, C M; Brader, M L; Frank, B H; DeFelippis, M R; Ward, M D

2000-01-01

Crystallographic studies of insulin-protamine complexes, such as neutral protamine Hagedorn (NPH) insulin, have been hampered by high crystal solvent content, small crystal dimensions, and extensive disorder in the protamine molecules. We report herein in situ tapping mode atomic force microscopy (TMAFM) studies of crystalline neutral protamine Lys(B28)Pro(B29) (NPL), a complex of Lys(B28)Pro(B29) insulin, in which the C-terminal prolyl and lysyl residues of human insulin are inverted, and protamine that is used as an intermediate time-action therapy for treating insulin-dependent diabetes. Tapping mode AFM performed at 6 degrees C on bipyramidally tipped tetragonal rod-shaped NPL crystals revealed large micron-sized islands separated by 44-A tall steps. Lattice images obtained by in situ TMAFM phase and height imaging on these islands were consistent with the arrangement of individual insulin-protamine complexes on the P4(1)2(1)2 (110) crystal plane of NPH, based on a low-resolution x-ray diffraction structure of NPH, arguing that the NPH and NPL insulins are isostructural. Superposition of the height and phase images indicated that tip-sample adhesion was larger in the interstices between NPL complexes in the (110) crystal plane than over the individual complexes. These results demonstrate the utility of low-temperature TMAFM height and phase imaging for the structural characterization of biomolecular complexes. PMID:10620310

Bridgman growth of lead potassium niobate crystals

NASA Astrophysics Data System (ADS)

Fan, Shiji; Sun, Renying; Lin, Yafang; Wu, Jindi

1999-03-01

Lead potassium niobate Pb 2KNb 5O 15 (PKN) crystals with tetragonal tungsten bronze (TTB) structure have been grown by the modified Bridgman (BR) method. Nearly sealed Pt crucibles and small temperature gradients in the Bridgman furnace can limit volatilization of PbO and cracking of as-grown PKN crystals. Transparent PKN crystals of 1 inch diameter by ˜2 inch length with brownish color have been grown successfully at a crucible lowering rate <0.5 mm/h and a temperature gradient of 10-15°C/cm across the solid-liquid interface. Coupling between twins and growth directions of the crystal is also discussed.

Control of optical properties of YAG crystals by thermal annealing

NASA Astrophysics Data System (ADS)

Tkachenko, S.; Arhipov, P.; Gerasymov, I.; Kurtsev, D.; Vasyukov, S.; Nesterkina, V.; Shiran, N.; Mateichenko, P.; Sidletskiy, O.

2018-02-01

Optical properties of YAG crystals grown and annealed under different atmosphere conditions have been compared. Simultaneously we have registered the surface composition of crystals and content of basic admixtures in the crystals grown under the reducing conditions. Unlike YAG grown under weakly oxidizing conditions in Ir crucibles and bleached under oxidizing annealing, YAGMo crystals grown in Mo crucibles under reducing Ar + CO atmosphere can be bleached by both oxidizing and reducing thermal annealing. The bleaching of YAGMo is not reversed by further annealing under any available conditions. Mechanisms of this phenomenon have been discussed, including a possible role of admixtures in elimination of color centers in YAG grown under the reducing conditions.

Potassium-cobalt sulphate crystal growth assisted by low frequency vibrations

NASA Astrophysics Data System (ADS)

Sadovsky, A.; Ermochenkov, I.; Dubovenko, E.; Sukhanova, E.; Bebyakin, M.; Dubov, V.; Avetissov, I.

2018-02-01

Single crystals of K2Co(SO4)2·6H2O were grown from solution using the temperature reduction method enhanced by the axial low frequency vibration control technique (AVC-technique). Physical modeling of heat-mass transfer in solution under the AVC action was performed. The growth rate of the AVC grown crystal was found to be twice that of the crystal grown under natural convection conditions. Analysis of spectral characteristics (absorption and Raman spectra) as well as structural properties (dislocation density and microhardness) of the grown crystals showed the significant superiority of the AVC technique for the growth of K2Co(SO4)2·6H2O crystals.

Growth 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.

Linear, non-linear and thermal properties of single crystal of LHMHCl

NASA Astrophysics Data System (ADS)

Kulshrestha, Shobha; Shrivastava, A. K.

2018-05-01

The single crystal of amino acid of L-histidine monohydrochloride was grown by slow evaporation technique at room temperature. High optical quality and appropriate size of crystals were grown under optimized growth conditions. The grown crystals were transparent. Crystals are characterized with different characterizations such as Solubility test, UV-Visible, optical band gap (Eg). With the help of optical data to be calculate absorption coefficient (α), extinction coefficient (k), refractive index (n), dielectric constant (ɛ). These optical constants are shows favorable conditions for photonics devices. Second harmonic generation (NLO) test show the green light emission which is confirm that crystal have properties for laser application. Thermal stability of grown crystal is confirmed by TG/DTA.

Growth and characterization of diammonium copper disulphate hexahydrate single crystal

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

Siva Sankari, R.; Perumal, Rajesh Narayana, E-mail: r.shankarisai@gmail.com

2014-03-01

Graphical abstract: Diammonium copper disulphate hexahydrate (DACS) is one of the most promising inorganic dielectric crystals with exceptional mechanical properties. Good quality crystals of DACS were grown by using solution method in a period of 30 days. The grown crystals were subjected to single crystal X-ray diffraction analysis in order to establish their crystalline nature. Thermo gravimetric, differential thermal analysis, FTIR, and UV–vis–NIR analysis were performed for the crystal. Several solid state physical parameters have been determined for the grown crystals. The dielectric constant and the dielectric loss and AC conductivity of the grown crystal were studied as a functionmore » of frequency and temperature has been calculated and plotted. - Highlights: • Diammonium copper disulphate is grown for the first time and CCDC number obtained. • Thermal analysis is done to see the stability range of the crystals. • Band gap and UV cut off wavelength of the crystal are determined to be 2.4 eV and 472.86 nm, respectively. • Dielectric constant, dielectric loss and AC conductivity are plotted as a function of applied field. - Abstract: Diammonium copper disulphate hexahydrate is one of the most promising inorganic crystals with exceptional dielectric properties. A good quality crystal was harvested in a 30-day period using solution growth method. The grown crystal was subjected to various characterization techniques like single crystal X-ray diffraction analysis, thermo gravimetric, differential thermal analysis, FTIR, and UV–vis–NIR analysis. Unit cell dimensions of the grown crystal have been identified from XRD studies. Functional groups of the title compounds have been identified from FTIR studies. Thermal stability of the samples was checked by TG/DTA studies. Band gap of the crystal was calculated. The dielectric constant and dielectric loss were studied as a function of frequency of the applied field. AC conductivity was plotted as a

Microgravity

NASA Image and Video Library

2004-04-15

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.

Thermoluminescence kinetic features of Lithium Iodide (LiI) single crystal grown by vertical Bridgman technique

NASA Astrophysics Data System (ADS)

Daniel, D. Joseph; Kim, H. J.; Kim, Sunghwan; Khan, Sajid

2017-08-01

Single crystal of pure Lithium Iodide (LiI) has been grown from melt by using the vertical Bridgman technique. Thermoluminescence (TL) Measurements were carried out at 1 K/s following X-ray irradiation. The TL glow curve consists of a dominant peak at (peak-maximum Tm) 393 K and one low temperature peak of weaker intensity at 343 K. The order of kinetics (b), activation energy (E), and the frequency factor (S) for a prominent TL glow peak observed around 393 K for LiI crystals are reported for the first time. The peak shape analysis of the glow peak indicates the kinetics to be of the first order. The value of E is calculated using various standard methods such as initial rise (IR), whole glow peak (WGP), peak shape (PS), computerized glow curve deconvolution (CGCD) and Variable Heating rate (VHR) methods. An average value of 1.06 eV is obtained in this case. In order to validate the obtained parameters, numerically integrated TL glow curve has been generated using experimentally determined kinetic parameters. The effective atomic number (Zeff) for this material was determined and found to be 52. X-ray induced emission spectra of pure LiI single crystal are studied at room temperature and it is found that the sample exhibit sharp emission at 457 nm and broad emission at 650 nm.

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.

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.

Crystal-Physical Model of Ion Transport in Nonlinear Optical Crystals of KTiOPO4

NASA Astrophysics Data System (ADS)

Sorokin, N. I.; Shaldin, Yu. V.

2018-04-01

The ionic conductivity along the principal axes a, b, and c of the unit cell of the nonlinear-optical high-resistance KTiOPO4 single crystals (rhombic syngony, space group Pna21), which are as-grown and after thermal annealing in vacuum, has been investigated by the method of impedance spectroscopy. The crystals were grown from a solution-melt by the Czochralski method. The as-grown KTiOPO4 crystals possess a quasi-one-dimensional conductivity along the crystallographic c axis, which is caused by the migration of K+ cations: σ║ c = 1.0 × 10-5 S/cm at 573 K. Wherein the characteristics of the anisotropy of ionic conductivity of the crystals is equal to σ║ c /σ║ a = 3 and σ║ c /σ║ b = 24. The thermal annealing at 1000 K for 10 h in vacuum increases the magnitude of σ║ c of KTiOPO4 by a factor of 28 and leads to an increase in the ratio σ║ c /σ║ b = 2.1 × 103 at 573 K. A crystal-physical model of ionic transport in KTiOPO4 crystals has been proposed.

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.

Structural, spectral and birefringence studies of semiorganic nonlinear optical single crystal: Calcium5-sulfosalicylate

NASA Astrophysics Data System (ADS)

Shalini, D.; Kalainathan, S.; Ambika, V. Revathi; Hema, N.; Jayalakshmi, D.

2017-11-01

Semi-organic nonlinear optical crystal Calcium5-Sulfosalicylate (CA5SS) was grown by slow evaporation solution growth technique. The cell parameters and molecular structure of the grown crystal were studied by single crystal x-ray diffraction analysis. The presence of various functional groups of the grown crystal was confirmed using Fourier transform infrared (FT-IR), Fourier transform Raman (FT-Raman) analysis. UV-Visible spectrum shows that CA5SS crystals have high transmittance in the range of 330-900 nm. The refractive index, birefringence and transient photoluminescence properties of the grown crystal were analyzed. The frequency doubling of the grown crystal (CA5SS) were studied and compared with that of 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.

Crystal growth and characterization of semi-organic 2-amino-5-nitropyridinium bromide (2A5NPBr) single crystals for third-order nonlinear optical (NLO) applications

NASA Astrophysics Data System (ADS)

Vediyappan, Sivasubramani; Arumugam, Raja; Pichan, Karuppasamy; Kasthuri, Ramachandran; Muthu, Senthil Pandian; Perumal, Ramasamy

2017-12-01

Semi-organic nonlinear optical (NLO) 2-amino-5-nitropyridinium bromide (2A5NPBr) single crystals have been grown by slow evaporation solution technique (SEST) with the growth period of 60 days. The single-crystal XRD analysis confirms the unit cell parameters of the grown crystal. The crystallinity of grown 2A5NPBr was analyzed by powder X-ray diffraction (PXRD) measurement. The presence of functional groups of 2A5NPBr crystal was confirmed by Fourier transform infrared (FTIR) spectrum analysis. The optical transmittance of the grown crystal was analyzed by UV-Vis-NIR analysis. It shows good transparency in the visible and NIR region and it is favorable for nonlinear optical (NLO) device applications. The chemical etching study was carried out and it reveals that the grown crystal has less dislocation density. The photoconductivity study reveals that the grown crystal possesses positive photoconductive nature. The thermal stability of the crystal has been investigated by thermogravimetric (TG) and differential thermal analysis (DTA). The dielectric constant and dielectric loss as a function of frequency were measured. The electronic polarizability (α) of 2A5NPBr molecule has been calculated theoretically by different ways such as Penn analysis, Clausius-Mossotti relation, Lorentz-Lorenz equation, optical bandgap, and coupled dipole method (CDM). The obtained values of electronic polarizability (α) are in good agreement with each other. Laser damage threshold (LDT) of 2A5NPBr crystal has been measured using Nd:YAG laser with the wavelength of 1064 nm. Third-order nonlinear optical property of the grown crystal was studied by Z-scan technique using He-Ne laser of wavelength 632.8 nm.

Growth and characterization of high-purity SiC single crystals

NASA Astrophysics Data System (ADS)

Augustine, G.; Balakrishna, V.; Brandt, C. D.

2000-04-01

High-purity SiC single crystals with diameter up to 50 mm have been grown by the physical vapor transport method. Finite element analysis was used for thermal modeling of the crystal growth cavity in order to reduce stress in the grown crystal. Crystals are grown in high-purity growth ambient using purified graphite furniture and high-purity SiC sublimation sources. Undoped crystals up to 50 mm in diameter with micropipe density less than 100 cm -2 have been grown using this method. These undoped crystals exhibit resistivities in the 10 3 Ω cm range and are p-type due to the presence of residual acceptor impurities, mainly boron. Semi-insulating SiC material is obtained by doping the crystal with vanadium. Vanadium has a deep donor level located near the middle of the band gap, which compensates the residual acceptor resulting in semi-insulating behavior.

Synthesis, crystal structure, NLO and Hirshfeld surface analysis of 1,2,3-triazolyl chalcone single crystal

NASA Astrophysics Data System (ADS)

Shruthi, C.; Ravindrachary, V.; Guruswamy, B.; Lokanath, N. K.; Kumara, Karthik; Goveas, Janet

2018-05-01

Needle shaped brown coloured single crystal of the title compound was grown by slow evaporation technique using methanol as solvent. The grown crystal was characterized using FT-IR, Single crystal XRD, UV-visible and NLO studies. Crystal structure was confirmed by FT-IR study and the functional groups were identified. XRD study reveals that the crystal belongs to orthorhombic crystal system with pnaa space group and the corresponding cell parameters were calculated. UV-visible spectrum shows that the crystal is transparent in the entire visible region and absorption takes place in the UV-range. NLO efficiency of the crystal obtained 0.66 times that of urea was determined by SHG test. The intermolecular interaction and percentage contribution of each individual atom in the crystal lattice was quantized using Hirshfeld surface and 2D finger print analysis.

Role of Precursor-Conversion Chemistry in the Crystal-Phase Control of Catalytically Grown Colloidal Semiconductor Quantum Wires.

PubMed

Wang, Fudong; Buhro, William E

2017-12-26

Crystal-phase control is one of the most challenging problems in nanowire growth. We demonstrate that, in the solution-phase catalyzed growth of colloidal cadmium telluride (CdTe) quantum wires (QWs), the crystal phase can be controlled by manipulating the reaction chemistry of the Cd precursors and tri-n-octylphosphine telluride (TOPTe) to favor the production of either a CdTe solute or Te, which consequently determines the composition and (liquid or solid) state of the Bi x Cd y Te z catalyst nanoparticles. Growth of single-phase (e.g., wurtzite) QWs is achieved only from solid catalysts (y ≪ z) that enable the solution-solid-solid growth of the QWs, whereas the liquid catalysts (y ≈ z) fulfill the solution-liquid-solid growth of the polytypic QWs. Factors that affect the precursor-conversion chemistry are systematically accounted for, which are correlated with a kinetic study of the composition and state of the catalyst nanoparticles to understand the mechanism. This work reveals the role of the precursor-reaction chemistry in the crystal-phase control of catalytically grown colloidal QWs, opening the possibility of growing phase-pure QWs of other compositions.

Vapor Growth and Characterization of Cr-Doped ZnSe Crystals

NASA Technical Reports Server (NTRS)

Su, Ching-Hua; Feth, Shari; Volz, M. P.; Matyi, R.; George, M. A.; Chattopadhyay, K.; Burger, A.; Lehoczky, S. L.

1999-01-01

Cr-doped ZnSe single crystals were grown by a self-seeded physical vapor transport technique in both vertical (stabilized) and horizontal configurations. The source materials were mixtures of ZnSe and CrSe. Growth temperatures were in the range of 1140-1150 C and the furnace translation rates were 1.9-2.2 mm/day. The surface morphology of the as-grown crystals was examined by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Different features of the as-grown surface of the vertically and horizontally grown crystals suggest that different growth mechanisms were involved in the two growth configurations. The [Cr] doping levels were determined to be in the range of 1.8-8.3 x 10 (exp 19) cm (exp -3) from optical absorption measurements. The crystalline quality of the grown crystals were examined by high-resolution triple-crystal X-ray diffraction (HRTXD) analysis.

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

Habit modification of bis-thiourea zinc chloride (ZTC) semi organic crystals by impurities

NASA Astrophysics Data System (ADS)

Ruby Nirmala, L.; Thomas Joseph Prakash, J.

2013-06-01

Single crystals of bis-thiourea zinc chloride (ZTC) doped with metal ion (Li+) possess excellent nonlinear optical properties. These crystals were grown by slow evaporation solution growth technique. The effect of Li+ dopant on the growth and properties of ZTC single crystal were investigated and reported. The grown crystals were crystallized in orthorhombic structure with non-centro symmetric space group Pn21a through the parent compound. The amount of dopant incorporated in the parent crystal was revealed by the inductively coupled plasma (ICP-OES) studies. The FT-IR spectroscopy study was done for finding and confirming the functional groups present in the compound. The UV-Visible spectral study was carried out to find the optical behavior and transparency nature of the grown crystal. TG/DTA measurements and Vickers microhardness measurements were traced to find out the thermal and mechanical stability of the grown crystals respectively. Using Nd:YAG laser, the Second harmonic generation (SHG) for the grown crystals were confirmed.

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.

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.

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

Nucleation kinetics, crystal growth and optical studies on lithium hydrogen oxalate monohydrate single crystal

NASA Astrophysics Data System (ADS)

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

2017-06-01

Semi-organic lithium hydrogen oxalate monohydrate non-linear optical single crystals have been grown by slow evaporation solution technique at 40 °C. The nucleation parameters such as critical radius, interfacial tension, and critical free energy change have been evaluated using the experimental data. The solubility and the nucleation curve of the crystal at different temperatures have been analyzed. The crystal has a positive temperature coefficient of solubility. The metastable zone width and induction period have been determined for the aqueous solution growth of lithium hydrogen oxalate monohydrate. The UV-vis-NIR spectrum showed this crystal has high transparency. The photoconductivity studies indicate lithium hydrogen oxalate monohydrate has positive photoconductivity behaviour. The low etch pit density observed on (0 0 1) crystal surface and the high resolution x-ray difraction analysis indicate the good quality of the grown crystals

Preliminary observations of the effect of solutal convection on crystal morphology

NASA Technical Reports Server (NTRS)

Broom, M. Beth H.; Witherow, William K.; Snyder, Robert S.; Carter, Daniel C.

1988-01-01

Studies to examine the effect of solutal convection on crystal morphology using sucrose as a model system were initiated. Aspect ratios, defined as the width of the 100-plane-oriented face over the width of the 001-plane-oriented face, were determined for oriented crystals which were grown with either the 001-oriented or the 100-oriented face perpendicular to the convective flow. The dependence of the crystal morphology on orientation is much greater for crystals grown with one face occluded than for crystals grown suspended in solution. Many factors appear to interact in a complex fashion to influence crystal morphology.

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.

Growth of L-Valinium Aluminium Chloride single crystal for OLED and super-capacitor applications

NASA Astrophysics Data System (ADS)

Kalaivani, D.; Vijayalakshmi, S.; Theras, J. Elberin Mary; Jayaraman, D.; Joseph, V.

2015-12-01

L-Valinium Aluminium Chloride (LVAC), a novel semi-organic material, was grown using slow evaporation under isothermal condition. The single crystal data reveal that the grown crystal belongs to monoclinic system. The SEM micrographs give clear picture about the surface morphology. Further, they confirm the inclusion of aluminium chloride into atomic sites of L-Valine. The compositional elements present in the crystal were identified through EDAX analysis. The mass spectral analysis was carried out to determine the molecular weight of the grown crystal. The optical transparency of the grown crystal was investigated by UV-vis-NIR spectrum. FTIR spectral study was used to identify the functional groups present in the grown material. The luminescence characteristics of grown material were analysed to confirm the effect of metal ion on the ligand. This property makes the material suitable for OLED application. The supercapacitive performance of the grown crystal was finally studied using cyclic voltammetry.

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

NASA Technical Reports Server (NTRS)

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

1998-01-01

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

Bridgman growth of large-aperture yttrium calcium oxyborate crystal

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

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

2012-09-15

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

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.

Habit modification of bis-thiourea zinc chloride (ZTC) semi organic crystals by impurities.

PubMed

Ruby Nirmala, L; Thomas Joseph Prakash, J

2013-06-01

Single crystals of bis-thiourea zinc chloride (ZTC) doped with metal ion (Li(+)) possess excellent nonlinear optical properties. These crystals were grown by slow evaporation solution growth technique. The effect of Li(+) dopant on the growth and properties of ZTC single crystal were investigated and reported. The grown crystals were crystallized in orthorhombic structure with non-centro symmetric space group Pn21a through the parent compound. The amount of dopant incorporated in the parent crystal was revealed by the inductively coupled plasma (ICP-OES) studies. The FT-IR spectroscopy study was done for finding and confirming the functional groups present in the compound. The UV-Visible spectral study was carried out to find the optical behavior and transparency nature of the grown crystal. TG/DTA measurements and Vickers microhardness measurements were traced to find out the thermal and mechanical stability of the grown crystals respectively. Using Nd:YAG laser, the Second harmonic generation (SHG) for the grown crystals were confirmed. Copyright © 2013 Elsevier B.V. All rights reserved.

Brownian dynamics simulations of insulin microspheres formation

NASA Astrophysics Data System (ADS)

Li, Wei; Chakrabarti, Amit; Gunton, James

2010-03-01

Recent experiments have indicated a novel, aqueous process of microsphere insulin fabrication based on controlled phase separation of protein from water-soluble polymers. We investigate the insulin microsphere crystal formation from insulin-PEG-water systems via 3D Brownian Dynamics simulations. We use the two component Asakura-Oosawa model to simulate the kinetics of this colloid polymer mixture. We first perform a deep quench below the liquid-crystal boundary that leads to fractal formation. We next heat the system to obtain a break-up of the fractal clusters and subsequently cool the system to obtain a spherical aggregation of droplets with a relatively narrow size distribution. We analyze the structure factor S(q) to identify the cluster dimension. S(q) crosses over from a power law q dependence of 1.8 (in agreement with DLCA) to 4 as q increases, which shows the evolution from fractal to spherical clusters. By studying the bond-order parameters, we find the phase transition from liquid-like droplets to crystals which exhibit local HCP and FCC order. This work is supported by grants from the NSF and Mathers Foundation.

Electron-hole diffusion lengths >175 μm in solution-grown CH 3NH 3PbI 3 single crystals

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

Dong, Qingfeng; Fang, Yanjun; Shao, Yuchuan

Long, balanced electron and hole diffusion lengths greater than 100 nanometers in the polycrystalline organolead trihalide compound CH 3NH 3PbI 3 are critical for highly efficient perovskite solar cells. We found that the diffusion lengths in CH 3NH 3PbI 3 single crystals grown by a solution-growth method can exceed 175 micrometers under 1 sun (100 mW cm –2) illumination and exceed 3 millimeters under weak light for both electrons and holes. The internal quantum efficiencies approach 100% in 3-millimeter-thick single-crystal perovskite solar cells under weak light. These long diffusion lengths result from greater carrier mobility, longer lifetime, and much smallermore » trap densities in the single crystals than in polycrystalline thin films. As a result, the long carrier diffusion lengths enabled the use of CH 3NH 3PbI 3 in radiation sensing and energy harvesting through the gammavoltaic effect, with an efficiency of 3.9% measured with an intense cesium-137 source.« less

Electron-hole diffusion lengths >175 μm in solution-grown CH 3NH 3PbI 3 single crystals

DOE PAGES

Dong, Qingfeng; Fang, Yanjun; Shao, Yuchuan; ...

2015-02-27

Long, balanced electron and hole diffusion lengths greater than 100 nanometers in the polycrystalline organolead trihalide compound CH 3NH 3PbI 3 are critical for highly efficient perovskite solar cells. We found that the diffusion lengths in CH 3NH 3PbI 3 single crystals grown by a solution-growth method can exceed 175 micrometers under 1 sun (100 mW cm –2) illumination and exceed 3 millimeters under weak light for both electrons and holes. The internal quantum efficiencies approach 100% in 3-millimeter-thick single-crystal perovskite solar cells under weak light. These long diffusion lengths result from greater carrier mobility, longer lifetime, and much smallermore » trap densities in the single crystals than in polycrystalline thin films. As a result, the long carrier diffusion lengths enabled the use of CH 3NH 3PbI 3 in radiation sensing and energy harvesting through the gammavoltaic effect, with an efficiency of 3.9% measured with an intense cesium-137 source.« less

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

NASA Astrophysics Data System (ADS)

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

2000-09-01

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

Growth, structural, optical, thermal and mechanical properties of ammonium pentaborate single crystal.

PubMed

Balakrishnan, T; Bhagavannarayana, G; Ramamurthi, K

2008-11-15

Nonlinear optical single crystals of ammonium pentaborate (APB) were grown by the slow cooling method from aqueous solution. Grown crystal was characterized by powder X-ray diffraction (PXRD) and FT-IR spectral analysis. Perfection of the grown crystal was evaluated by high-resolution X-ray diffractometry (HRXRD). The effect of nylon threading on the perfection of the grown bigger crystal was also studied by HRXRD. The range and percentage of optical transmission was ascertained by recording UV-vis-NIR spectrum. Thermal properties were investigated by TG-DTA and DSC analyses. Its mechanical hardness was estimated by Vickers microhardness tester.

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

NASA Astrophysics Data System (ADS)

McMillen, Colin D.; Kolis, Joseph W.

2008-04-01

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

Optimization and characterization of bulk hexagonal boron nitride single crystals grown by the nickel-chromium flux method

NASA Astrophysics Data System (ADS)

Hoffman, Tim

Hexagonal boron nitride (hBN) is a wide bandgap III-V semiconductor that has seen new interest due to the development of other III-V LED devices and the advent of graphene and other 2-D materials. For device applications, high quality, low defect density materials are needed. Several applications for hBN crystals are being investigated, including as a neutron detector and interference-less infrared-absorbing material. Isotopically enriched crystals were utilized for enhanced propagation of phonon modes. These applications exploit the unique physical, electronic and nanophotonics applications for bulk hBN crystals. In this study, bulk hBN crystals were grown by the flux method using a molten Ni-Cr solvent at high temperatures (1500°C) and atmospheric pressures. The effects of growth parameters, source materials, and gas environment on the crystals size, morphology and purity were established and controlled, and the reliability of the process was greatly improved. Single-crystal domains exceeding 1mm in width and 200microm in thickness were produced and transferred to handle substrates for analysis. Grain size dependence with respect to dwell temperature, cooling rate and cooling temperature were analyzed and modeled using response surface morphology. Most significantly, crystal grain width was predicted to increase linearly with dwell temperature, with single-crystal domains exceeding 2mm in at 1700°C. Isotopically enriched 10B and 11B hBN crystal were produced using a Ni-Cr-B flux method, and their properties investigated. 10B concentration was evaluated using SIMS and correlated to the shift in the Raman peak of the E2g mode. Crystals with enrichment of 99% 10B and >99% 11B were achieved, with corresponding Raman shift peaks at 1392.0 cm-1 and 1356.6 cm-1, respectively. Peak FWHM also decreased as isotopic enrichment approached 100%, with widths as low as 3.5 cm-1 achieved, compared to 8.0 cm-1 for natural abundance samples. Defect selective etching was

Growth and characterization of divalent transition metal ions doped zinc hydrogen phosphate single crystals

NASA Astrophysics Data System (ADS)

D'Souza, Delma; Jagannatha, N.; Nagaraja, K. P.; Rohith, P. S.; Pradeepkumar, K. V.

2018-05-01

Zinc hydrogen phosphate (ZnHP) single crystal co-doped with divalent transition metal ions Cobalt (Co2+) and Cadmium (Cd2+) is grown by gel technique in silica hydro gel media. The presence of Co2+ and Cd2+ dopants in the ZnHP crystal was confirmed by Energy Dispersive X-ray Analysis (EDAX).FTIR spectra of the grown crystal depict the stretching and bending vibration of PO4 units, water of crystallization and metal-oxygen bonds. Powder XRD analysis reveals that the grown crystal belongs to monoclinic system with spacegroup P 21. The thermal stability of the grown crystal is rectified from TG-DSC studies.

Crystallization of Chicken Egg-White Lysozyme from Ammonium Sulfate

NASA Technical Reports Server (NTRS)

Forsythe, Elizabeth L.; Snell, Edward H.; Pusey, Marc L.

1997-01-01

Chicken egg-white lysozyme was crystallized from ammonium sulfate over the pH range 4.0-7.8, with protein concentrations from 100 to 150 mg/ml. Crystals were obtained by vapor-diffusion or batch-crystallization methods. The protein crystallized in two morphologies with an apparent morphology dependence on temperature and protein concentration. In general, tetragonal crystals could be grown by lowering the protein concentration or temperature. Increasing the temperature or protein concentration resulted in the growth of orthorhombic crystals. Representative crystals of each morphology were selected for X-ray analysis. The tetragonal crystals belonged to the P4(sub 3)2(sub 1)2 space group with crystals grown at ph 4.4 having unit-cell dimensions of a = b = 78.7 1, c=38.6 A and diffracting to beyond 2.0 A. The orthorhombic crystals, grown at pH 4.8, were of space group P2(sub 1)2(sub 1)2 and had unit-cell dimensions of a = 30.51, b = 56.51 and c = 73.62 A.

Characterization of high-resistivity CdTe and Cd0.9Zn0.1Te crystals grown by Bridgman method for radiation detector applications

NASA Astrophysics Data System (ADS)

Mandal, Krishna C.; Krishna, Ramesh M.; Pak, Rahmi O.; Mannan, Mohammad A.

2014-09-01

CdTe and Cd0.9Zn0.1Te (CZT) crystals have been studied extensively for various applications including x- and γ-ray imaging and high energy radiation detectors. The crystals were grown from zone refined ultra-pure precursor materials using a vertical Bridgman furnace. The growth process has been monitored, controlled, and optimized by a computer simulation and modeling program developed in our laboratory. The grown crystals were thoroughly characterized after cutting wafers from the ingots and processed by chemo-mechanical polishing (CMP). The infrared (IR) transmission images of the post-treated CdTe and CZT crystals showed average Te inclusion size of ~10 μm for CdTe and ~8 μm for CZT crystal. The etch pit density was ≤ 5×104 cm-2 for CdTe and ≤ 3×104 cm-2 for CZT. Various planar and Frisch collar detectors were fabricated and evaluated. From the current-voltage measurements, the electrical resistivity was estimated to be ~ 1.5×1010 Ω-cm for CdTe and 2-5×1011 Ω-cm for CZT. The Hecht analysis of electron and hole mobility-lifetime products (μτe and μτh) showed μτe = 2×10-3 cm2/V (μτh = 8×10-5 cm2/V) and 3-6×10-3 cm2/V (μτh = 4- 6×10-5 cm2/V) for CdTe and CZT, respectively. Detectors in single pixel, Frisch collar, and coplanar grid geometries were fabricated. Detectors in Frisch grid and guard-ring configuration were found to exhibit energy resolution of 1.4% and 2.6 %, respectively, for 662 keV gamma rays. Assessments of the detector performance have been carried out also using 241Am (60 keV) showing energy resolution of 4.2% FWHM.

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.

Growth and characterization of unidirectional benzil single crystal for photonic applications

NASA Astrophysics Data System (ADS)

Saranraj, A.; Thirupathy, J.; Dhas, S. Sahaya Jude; Jose, M.; Vinitha, G.; Dhas, S. A. Martin Britto

2018-06-01

Organic nonlinear optical benzil single crystal of fine quality with the dimensions of 168 × 14 mm2 was successfully grown in (100) plane from saturated solution by unidirectional SR method. The structural identity of the grown crystal was confirmed by powder XRD. High-resolution X-ray diffraction analysis indicates the crystalline perfection of the grown benzil crystal. The optical analysis was carried out by UV-visible spectroscopy which shows that the benzil crystal's cut off wavelength is 437 nm. The dielectric constant and dielectric loss of benzil crystal are found to be very much depending upon temperature and frequency. Ferroelectric nature of grown crystal was identified by P- E hysteresis analysis and to find the values of spontaneous polarization and coercive field. The laser damage threshold energy was studied with the help of Nd:YAG laser. The presence of third harmonic generation was identified by z-scan techniques.

Growth and properties of benzil doped benzimidazole (BMZ) single crystals

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

Babu, R. Ramesh, E-mail: rampap2k@yahoo.co.in; Crystal Growth and Crystallography Section, National Physical Laboratory, Krishnan Marg, New Delhi 110 012; Sukumar, M.

2010-09-15

In the present work, we have made an attempt to study the effect of benzil doping on the properties of benzimidazole single crystals. For this purpose we have grown pure and benzil doped benzimidazole single crystals by vertical Bridgman technique. The grown crystals were characterized by various characterization techniques. The presence of dopants confirmed by powder X-ray diffraction (XRD). Crystalline perfection of the grown crystals has been analysed by high-resolution X-ray diffraction (HRXRD). The transmittance, electrical property and mechanical strength have been analysed using UV-vis-NIR spectroscopic, dielectric and Vicker's hardness studies. The relative second harmonic generation efficiency of pure andmore » doped benzimidazole crystals measured using Kurtz powder test.« less

Liquid encapsulated crystal growth

NASA Technical Reports Server (NTRS)

Morrison, Andrew D. (Inventor)

1989-01-01

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

Liquid encapsulated crystal growth

NASA Technical Reports Server (NTRS)

Morrison, Andrew D. (Inventor)

1987-01-01

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

Macromolecule Crystal Quality Improvement in Microgravity: The Role of Impurities

NASA Technical Reports Server (NTRS)

Judge, Russell A.; Snell, Edward H.; Pusey, Marc L.; Sportiello, Michael G.; Todd, Paul; Bellamy, Henry; Borgstahl, Gloria E.; Pokros, Matt; Cassanto, John M.

2000-01-01

While macromolecule impurities may affect crystal size and morphology the over-riding question is; "How do macromolecule impurities effect crystal X-ray quality and diffraction resolution?" In the case of chicken egg white lysozyme, crystals can be grown in the presence of a number of impurities without affecting diffraction resolution. One impurity however, the lysozyme dimer, does negatively impact the X-ray crystal properties. Crystal quality improvement as a result of better partitioning of this impurity during crystallization in microgravity has been reported'. In our recent experimental work dimer partitioning was found to be not significantly different between the two environments. Mosaicity analysis of pure crystals showed a reduced mosaicity and increased signal to noise for the microgravity grown crystals. Dimer incorporation however, did greatly reduce the resolution limit in both ground and microgravity grown crystals. These results indicate that impurity effects in microgravity are complex and may rely on the conditions or techniques employed.

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.

Method for the preparation of photochromic insulating crystals

DOEpatents

Abraham, Marvin M.; Boldu, Jose L.; Chen, Yok; Orera, Victor M.

1986-01-01

A method for preparing reversible-photochromic magnesium oxide (MgO) crystals. Single crystals of MgO doped with both lithium (Li) and nickel (Ni) are grown by a conventional arc fusion method. The as-grown crystals are characterized by an amber coloration. The crystals lose the amber coloration and become photochromic when they are thermochemically reduced by heating at temperatures greater than 1000.degree. K. in a hydrogen atmosphere. Alternate irradiation with UV and visible light result in rejuvenation and bleaching of the amber coloration, respectively.

Structural, thermal, laser damage, photoconductivity, NLO and mechanical properties of modified vertical Bridgman method grown AgGa0.5In0.5Se2 single crystal

NASA Astrophysics Data System (ADS)

Vijayakumar, P.; Ramasamy, P.

2016-08-01

AgGa0.5In0.5Se2 single crystal was grown using modified vertical Bridgman method. The structural perfection of the AgGa0.5In0.5Se2 single crystal has been analyzed by high-resolution X-ray diffraction rocking curve measurements. The structural and compositional uniformities of AgGa0.5In0.5Se2 were studied using Raman scattering spectroscopy at room temperature. The FWHM of the Γ1 (W1) and Γ5L (Γ15) measured at different regions of the crystal confirms that the composition throughout its length is fairly uniform. Thermal properties of the as-grown crystal, including specific heat, thermal diffusivity and thermal conductivity have been investigated. The multiple shot surface laser damage threshold value was measured using Nd:YAG laser. Photoconductivity measurements with different temperatures have confirmed the positive photoconducting behavior. Second harmonic generation (SHG) on powder samples has been measured using the Kurtz and Perry technique and the results display that AgGa0.5In0.5Se2 is a phase-matchable NLO material. The hardness behavior has been measured using Vickers micro hardness measurement and the indentation size effect has been observed. The classical Meyer's law, propositional resistance model and modified propositional resistance model have been used to analyse the micro hardness behavior.

Biotechnology

NASA Image and Video Library

1998-06-03

Diabetic patients may someday reduce their insulin injections and lead more normal lives because of new insights gained through innovative space research in which insulin crystals were grown on the Space Shuttle. Results from a 1994 insulin crystals growth experiment in space are leading to a new understanding of protein insulin. Lack of insulin is the cause of diabetes, a disease that accounts for one-seventh of the nation's health care costs. Champion Deivanaygam, a researcher at the Center for Macromolecular Crystallography at the University of Alabama in Birmingham, assists in this work. Photo credit: NASA/Marshall Space Flight Center (MSFC)

Influence of solvents on the habit modification of alpha lactose monohydrate single crystals

NASA Astrophysics Data System (ADS)

Parimaladevi, P.; Srinivasan, K.

2013-02-01

Restricted evaporation of solvent method was adopted for the growth of alpha lactose monohydrate single crystals from different solvents. The crystal habits of grown crystals were analysed. The form of crystallization was confirmed by powder x-ray diffraction analysis. Thermal behaviour of the grown crystals was studied by using differential scanning calorimetry.

Pressure cryocooling protein crystals

DOEpatents

Kim, Chae Un [Ithaca, NY; Gruner, Sol M [Ithaca, NY

2011-10-04

Preparation of cryocooled protein crystal is provided by use of helium pressurizing and cryocooling to obtain cryocooled protein crystal allowing collection of high resolution data and by heavier noble gas (krypton or xenon) binding followed by helium pressurizing and cryocooling to obtain cryocooled protein crystal for collection of high resolution data and SAD phasing simultaneously. The helium pressurizing is carried out on crystal coated to prevent dehydration or on crystal grown in aqueous solution in a capillary.

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.

Dielectric Spectroscopy Study of ZnSe Grown by Physical Vapor Transport

NASA Technical Reports Server (NTRS)

Kokan, J.; Gerhardt, R.; Su, Ching-Hua

1997-01-01

The dielectric properties of ZnSe samples grown by physical vapor transport were measured as a function of frequency. Differences can be seen in the dielectric properties of samples grown under different conditions. The spectra of heat treated samples were also acquired and were found to exhibit significant deviations from those of the as grown 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.

Method for the preparation of photochromic insulating crystals

DOEpatents

Abraham, M.M.; Boldu, J.L.; Chen, Y.; Orera, V.M.

1984-09-28

A method for preparing reversible-photochromic magnesium oxide (MgO) crystals is disclosed. Single crystals of MgO doped with both lithium (Li) and nickel (Ni) are grown by a conventional arc fusion method. The as-grown crystals are characterized by an amber coloration. The crystals lose the amber coloration and become photochromic when they are thermochemically reduced by heating at temperatures greater then 1000/sup 0/K in a hydrogen atmosphere. Alternate irradiation with uv and visible light result in rejuvenation and bleaching of the amber coloration, respectively.

Laser MBE-grown CoFeB epitaxial layers on MgO: Surface morphology, crystal structure, and magnetic properties

NASA Astrophysics Data System (ADS)

Kaveev, Andrey K.; Bursian, Viktor E.; Krichevtsov, Boris B.; Mashkov, Konstantin V.; Suturin, Sergey M.; Volkov, Mikhail P.; Tabuchi, Masao; Sokolov, Nikolai S.

2018-01-01

Epitaxial layers of CoFeB were grown on MgO by means of laser molecular beam epitaxy using C o40F e40B20 target. The growth was combined with in situ structural characterization by three-dimensional reciprocal space mapping obtained from reflection high energy electron diffraction (RHEED) data. High-temperature single stage growth regime was adopted to fabricate CoFeB layers. As confirmed by the atomic force microscopy, the surface of CoFeB layers consists of closely spaced nanometer sized islands with dimensions dependent on the growth temperature. As shown by RHEED and XRD analysis, the CoFeB layers grown at high-temperature on MgO(001) possess body centered cubic (bcc) crystal structure with the lattice constant a =2.87 Å close to that of the C o75F e25 alloy. It was further shown that following the same high-temperature growth technique the MgO/CoFeB/MgO(001) heterostructures can be fabricated with top and bottom MgO layers of the same crystallographic orientation. The CoFeB layers were also grown on the GaN(0001) substrates using MgO(111) as a buffer layer. In this case, the CoFeB layers crystallize in bcc crystal structure with the (111) axis perpendicular to the substrate surface. The magnetic properties of the CoFeB/MgO (001) heterostructures have been investigated by measuring magnetization curves with a vibrating sample magnetometer as well as by performing magneto-optical Kerr effect (MOKE) and ferromagnetic resonance (FMR) studies. FMR spectra were obtained for the variety of the magnetic field directions and typically consisted of a single relatively narrow resonance line. The magnetization orientations and the resonance conditions were calculated in the framework of a standard magnetic energy minimization procedure involving a single K1 c cubic term for the magnetocrystalline anisotropy. This allows a fairly accurate description of the angular dependences of the resonance fields—both in-plane and out-of-plane. It was shown that CoFeB layers exhibit

Crystal growth and piezoelectric properties of Ca3Ta(Ga0.9Sc0.1)3Si2O14 bulk single crystal

NASA Astrophysics Data System (ADS)

Igarashi, Yu; Yokota, Yuui; Ohashi, Yuji; Inoue, Kenji; Yamaji, Akihiro; Shoji, Yasuhiro; Kamada, Kei; Kurosawa, Shunsuke; Yoshikawa, Akira

2018-03-01

Ca3Ta(Ga0.9Sc0.1)3Si2O14 langasite-type single crystal with a diameter of 1 in. was grown by Czochralski (Cz) method. Obtained crystal had good crystallinity and its lattice constants exceeded those of Ca3TaGa3Si2O14 (CTGS) according to the X-ray analysis. A crack-free specimen cut from the grown crystal was used for the measurements of dielectric constant ε11T/ε0, electromechanical coupling factor k12, and piezoelectric constant d11. The accuracies of these measurements were better than those for the crystal grown by micro-pulling-down (μ-PD) method. Substitution of Ga with Sc resulted modification of these constants in the directions opposite to those observed after partial substitution of Ga (of CTGS) with Al. This suggests that increase of |d14| was most probably associated with enlargement of average size of the Ga sites. The crystal reported here had greater dimensions as compared to analogous crystals grown by the μ-PD method. As a result, accuracy of determination of acoustic constants of this material may be improved.

Doping of Czochralski-grown bulk β-Ga2O3 single crystals with Cr, Ce and Al

NASA Astrophysics Data System (ADS)

Galazka, Zbigniew; Ganschow, Steffen; Fiedler, Andreas; Bertram, Rainer; Klimm, Detlef; Irmscher, Klaus; Schewski, Robert; Pietsch, Mike; Albrecht, Martin; Bickermann, Matthias

2018-03-01

We experimentally evaluated segregation of Cr, Ce and Al in bulk β-Ga2O3 single crystals grown by the Czochralski method, as well as the impact of these dopants on optical properties. The segregation of Cr and Ce and their incorporation into the β-Ga2O3 crystal structure strongly depends on O2 concentration in the growth atmosphere which has a noticeable impact on decomposition of Ga2O3 and Cr2O3, as well as on the charge state of Cr and Ce. Effective segregation coefficients for Cr are in the range of 3.1-1.5 at 7-24 vol% O2, while for Ce they are roughly below 0.01 at 1.5-34 vol% O2. The effective segregation coefficient for Al is 1.1 at 1.5-21 vol% O2. Both dopants Ce and Al have a thermodynamically stabilizing effect on β-Ga2O3 crystal growth by supressing decomposition. While Ce has no impact on the optical transmittance in the ultraviolet and visible regions, in Cr doped crystals we observe three absorption bands due to Cr3+ on octahedral Ga sites, one in the ultraviolet merging with the band edge absorption of β-Ga2O3 and two in the visible spectrum, for which we estimate the absorption cross sections. Al doping also does not induce dopant related absorption bands but clearly shifts the absorption edge as one expects for a solid-solution crystal Ga2(1-x)Al2xO3 still in the monoclinic phase. For the highest doping concentration (Ga1.9Al0.1O3) we estimate an increase of the energy gap by 0.11 eV.

Growth, and magnetic study of Sm0.4Er0.6FeO3 single crystal grown by optical floating zone technique

NASA Astrophysics Data System (ADS)

Wu, Anhua; Zhao, Xiangyang; Man, Peiwen; Su, Liangbi; Kalashnikova, A. M.; Pisarev, R. V.

2018-03-01

Sm0.4Er0.6FeO3 single crystals were successfully grown by optical floating zone method; high quality samples with various orientations were manufactured. Based on these samples, Magnetic property of Sm0.4Er0.6FeO3 single crystals were investigated systemically by means of the temperature dependence of magnetization. It indicated that compositional variations not only alter the spin reorientation temperature, but also the compensation temperature of the orthoferrites. Unlike single rare earth orthoferrites, the reversal transition temperature point of Sm0.4Er0.6FeO3 increases as magnetic field increases, which is positive for designing novel spin switching or magnetic sensor device.

Crystal growth and scintillation properties of Pr-doped SrI2 single crystals

NASA Astrophysics Data System (ADS)

Yokota, Yuui; Ito, Tomoki; Yoshino, Masao; Yamaji, Akihiro; Ohashi, Yuji; Kurosawa, Shunsuke; Kamada, Kei; Yoshikawa, Akira

2018-04-01

Pr-doped SrI2 (Pr:SrI2) single crystals with various Pr concentrations were grown by the halide-micro-pulling-down (H-μ-PD) method, and the scintillation properties were investigated. Pr1%:SrI2 single crystal with high transparency could be grown by the H-μ-PD method while Pr2, 3 and 5%:SrI2 single crystals included some cracks and opaque parts. In the photoluminescence spectrum of the Pr1%:SrI2 single crystal, an emission peak originated from the Pr3+ ion was observed around 435 nm while the radioluminescence spectra showed an emission peak around 535 nm for the undoped SrI2 and Pr:SrI2 single crystals. Light yields of Pr1, 2, 3 and 5%:SrI2 single crystals under γ-ray irradiation were 7700, 8700, 7200 and 6700 photons/MeV, respectively. Decay times of Pr1 and 2%:SrI2 single crystals under γ-ray irradiation were 55.9 and 35.0 ns of the fast decay component, and 435 and 408 ns of the slow decay component, respectively.

Thermal, mechanical, optical and dielectric properties of piperazinium hydrogen phosphite monohydrate NLO single crystal

NASA Astrophysics Data System (ADS)

Rajkumar, R.; Praveen Kumar, P.

2018-05-01

Optical transparent crystal of piperazinium hydrogen phosphite monohydrate (PHPM) was grown by slow evaporation method. The grown crystal was characterized by single crystal X-ray diffraction analysis and the crystal belongs to monoclinic system. The functional groups present in PHPM crystal were confirmed by FTIR analysis. UV-Visible spectrum shows that the PHPM crystal is transparent in the visible region. The mechanical behavior of PHPM crystal was characterized by Vickers hardness test. Thermal stability of PHPM crystal was analyzed by thermogravimetric analysis. Dielectric studies were also carried out for the grown crystal. The third-order nonlinear parameters such as nonlinear refractive index and nonlinear absorption coefficient have been calculated using Z scan technique.

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.

Growth Defects in Biomacromolecular Crystals

NASA Technical Reports Server (NTRS)

2003-01-01

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

Human insulin polymorphism upon ligand binding and pH variation: the case of 4-ethylresorcinol.

PubMed

Fili, S; Valmas, A; Norrman, M; Schluckebier, G; Beckers, D; Degen, T; Wright, J; Fitch, A; Gozzo, F; Giannopoulou, A E; Karavassili, F; Margiolaki, I

2015-09-01

This study focuses on the effects of the organic ligand 4-ethylresorcinol on the crystal structure of human insulin using powder X-ray crystallography. For this purpose, systematic crystallization experiments have been conducted in the presence of the organic ligand and zinc ions within the pH range 4.50-8.20, while observing crystallization behaviour around the isoelectric point of insulin. High-throughput crystal screening was performed using a laboratory X-ray diffraction system. The most representative samples were selected for synchrotron X-ray diffraction measurements, which took place at the European Synchrotron Radiation Facility (ESRF) and the Swiss Light Source (SLS). Four different crystalline polymorphs have been identified. Among these, two new phases with monoclinic symmetry have been found, which are targets for the future development of microcrystalline insulin drugs.

Human insulin polymorphism upon ligand binding and pH variation: the case of 4-ethylresorcinol

PubMed Central

Fili, S.; Valmas, A.; Norrman, M.; Schluckebier, G.; Beckers, D.; Degen, T.; Wright, J.; Fitch, A.; Gozzo, F.; Giannopoulou, A. E.; Karavassili, F.; Margiolaki, I.

2015-01-01

This study focuses on the effects of the organic ligand 4-ethylresorcinol on the crystal structure of human insulin using powder X-ray crystallography. For this purpose, systematic crystallization experiments have been conducted in the presence of the organic ligand and zinc ions within the pH range 4.50–8.20, while observing crystallization behaviour around the isoelectric point of insulin. High-throughput crystal screening was performed using a laboratory X-ray diffraction system. The most representative samples were selected for synchrotron X-ray diffraction measurements, which took place at the European Synchrotron Radiation Facility (ESRF) and the Swiss Light Source (SLS). Four different crystalline polymorphs have been identified. Among these, two new phases with monoclinic symmetry have been found, which are targets for the future development of microcrystalline insulin drugs. PMID:26306195

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.

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

NASA Technical Reports Server (NTRS)

Su, Ching-Hua; Brebrick, R. F.; Burger, A.; Dudley, M.; Matyi, R.; Ramachandran, N.; Sha, Yi-Gao; Volz, M.; Shih, Hung-Dah

1999-01-01

Complete and systematic ground-based experimental and theoretical analyses on the Physical Vapor Transport (PVT) of ZnSe and related ternary compound semiconductors have been performed. The analyses included thermodynamics, mass flux, heat treatment of starting material, crystal growth, partial pressure measurements, optical interferometry, chemical analyses, photoluminescence, microscopy, x-ray diffraction and topography as well as theoretical, analytical and numerical analyses. The experimental results showed the influence of gravity orientation on the characteristics of: (1) the morphology of the as-grown crystals as well as the as-grown surface morphology of ZnSe and Cr doped ZnSe crystals; (2) the distribution of impurities and defects in ZnSe grown crystals; and (3) the axial segregation in ZnSeTe grown crystals.

Purification, crystal growth and characterization of CdSe single crystals

NASA Astrophysics Data System (ADS)

Burger, A.; Henderson, D. O.; Morgan, S. H.; Silberman, E.

1991-02-01

CdSe single crystals have been grown from the stoichiometric melt and from Se rich solutions. Here we report the first mid and far infrared spectra of CdSe crystals free of any known impurity bands. Previous studies of the lattice vibrational properties of CdSe crystals have shown the presence of two bands at 538 and 270 cm -1. Modifications in the purification and crystal growth conditions lead us to assign these two bands to a sulfur impurity. Low temperature photoluminescence spectra are also presented and discussed.

Study on structural, morphological, optical and thermal properties of guanidine carbonate doped nickel sulfate hexahydrate crystal.

PubMed

Silambarasan, A; Rajesh, P; Ramasamy, P

2015-01-05

The single crystal of guanidine carbonate doped nickel sulfate hexahydrate was grown from solution for ultraviolet filters. The single crystal XRD confirms that the grown single crystal belongs to the tetragonal system with the space group of P4₁2₁2. The crystallinity of the grown crystal was estimated by powder X-ray diffraction studies. The optical transmission and thermal stability of as-grown guanidine carbonate doped nickel sulfate single crystals have been studied. The optical transmission spectrum demonstrates the characteristics of ultraviolet filters. The TG/DTA studies confirm the thermal properties of grown crystals. Thermo-gravimetric analysis showed that the dehydration temperature of the guanidine carbonate doped nickel sulfate crystal is about 100 °C, which is much higher than that of pure nickel sulfate hexahydrate (NSH) crystals which is 72 °C. The growth behaviors and dislocation density were detected under the high resolution XRD and etching studies respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

Growth of bulk ZnO crystals by self-selecting CVT method

NASA Astrophysics Data System (ADS)

Fan, Long; Jiang, Tao; Xiao, TingTing; Chen, Jie; Peng, Liping; Wang, Xuemin; Yan, Dawei; Wu, Weidong

2018-05-01

Bulk ZnO crystals were grown by self-selecting CVT method using carbon as the transport agent. The crystal growth process took place on the top of the polycrystalline source material, and deep-red colored ZnO crystals of several millimeters were obtained. The as-grown crystals were characterized by X-ray diffraction (XRD), Energy Dispersive Spectrometer (EDS), Raman scattering (RS) spectroscopy, visible-near infrared (VIS-NIR) spectrophotometer and room temperature photoluminescence (PL) spectroscopy. XRD results indicate good crystallinity of the ZnO crystal. The EDS analysis shows that the crystal has a stoichiometry ratio Zn: O = 52: 48. The results suggest the existence of native defects of oxygen vacancies (OV) in the as-grown ZnO samples, which is caused by the stoichiometry shift to Zn-rich.

Astrocytes produce an insulin-like neurotrophic factor

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

Kadle, R.; Suksang, C.; Fellows, R.E.

1986-05-01

They have previously reported that survival of dissociated neurons from fetal rat telencephalon plated at low density in serum-free, hormone-free defined medium is enhanced in the presence of insulin. In the absence of insulin a similar effect on neuronal survival is observed if cells are grown in medium conditioned by glial cells. The present study was carried out to characterize the insulin-like neurotrophic activity present in the glial conditioned medium (GLCM). Conditioned medium from confluent cultures of astrogial cells maintained in a serum free defined medium without insulin was collected every two or three days. A 5 to 30kDa fractionmore » of this medium was obtained by filtering it sequentially through YM30 and YM5 membrane filters. Binding of /sup 125/I-insulin to high density neuronal cultures was inhibited 43% by this fraction. Radioimmunoassay for insulin indicated that 1-2 ng of immuno-reactive insulin were present per ml of GLCM. Immunosequestration of the factor by insulin antibodies bound to protein A agarose gel resulted in loss of neurotrophic activity of the 5 to 30 kDa fraction. These results indicate that cultured astrocytes produce a factor immunologically and biochemically similar to insulin. This factor enhances the survival of neurons in culture and may be important for their normal development and differentiation.« less

Structural modulation of nanowire interfaces grown over selectively disrupted single crystal surfaces

NASA Astrophysics Data System (ADS)

Garratt, E.; Nikoobakht, B.

2015-08-01

Recent breakthroughs in deterministic approaches to the fabrication of nanowire arrays have demonstrated the possibility of fabricating such networks using low-cost scalable methods. In this regard, we have developed a scalable growth platform for lateral fabrication of nanocrystals with high precision utilizing lattice match and symmetry. Using this planar architecture, a number of homo- and heterostructures have been demonstrated including ZnO nanowires grown over GaN. The latter combination produces horizontal, epitaxially formed crystals aligned in the plane of the substrate containing a very low number of intrinsic defects. We use such ordered structures as model systems in the interests of gauging the interfacial structural dynamics in relation to external stimuli. Nanosecond pulses of focused ion beams are used to slightly modify the substrate surface and selectively form lattice disorders in the path of nanowire growth to examine the nanocrystal, namely: its directionality and lattice defects. High resolution electron microscopies are used to reveal some interesting structural effects; for instance, a minimum threshold of surface defects that can divert nanowires. We also discuss data indicating formation of surface strains and show their mitigation during the growth process.

Structural, optical, mechanical and dielectric studies of pure and doped L-Prolinium trichloroacetate single crystals.

PubMed

Renuka, N; Ramesh Babu, R; Vijayan, N; Vasanthakumar, Geetha; Krishna, Anuj; Ramamurthi, K

2015-02-25

In the present work, pure and metal substituted L-Prolinium trichloroacetate (LPTCA) single crystals were grown by slow evaporation method. The grown crystals were subjected to single crystal X-ray diffraction (XRD), powder X-ray diffraction, FTIR, UV-Visible-NIR, hardness, photoluminescence and dielectric studies. The dopant concentration in the crystals was measured by inductively coupled plasma (ICP) analysis. Single crystal X-ray diffraction studies of the pure and metal substituted LPTCA revealed that the grown crystals belong to the trigonal system. Ni(2+) and Co(2+) doping slightly altered the lattice parameters of LPTCA without affecting the basic structure of the crystal. FTIR spectral analysis confirms the presence of various functional groups in the grown crystals. The mechanical behavior of pure and doped crystals was analyzed by Vickers's microhardness test. The optical transmittance, dielectric and photoluminescence properties of the pure and doped crystals were analyzed. Copyright © 2014 Elsevier B.V. All rights reserved.

Crystal Growth of Ternary Compound Semiconductors in Low Gravity Environment

NASA Technical Reports Server (NTRS)

Su, Ching-Hua

2014-01-01

A low gravity material experiment will be performed in the Material Science Research Rack (MSRR) on International Space Station (ISS). There are two sections of the flight experiment: (I) crystal growth of ZnSe and related ternary compounds, such as ZnSeS and ZnSeTe, by physical vapor transport (PVT) and (II) melt growth of CdZnTe by directional solidification. The main objective of the project is to determine the relative contributions of gravity-driven fluid flows to the compositional distribution, incorporation of impurities and defects, and deviation from stoichiometry observed in the grown crystals as results of buoyancy-driven convection and growth interface fluctuations caused by irregular fluid-flows on Earth. The investigation consists of extensive ground-based experimental and theoretical research efforts and concurrent flight experimentation. This talk will focus on the ground-based studies on the PVT crystal growth of ZnSe and related ternary compounds. The objectives of the ground-based studies are (1) obtain the experimental data and conduct the analyses required to define the optimum growth parameters for the flight experiments, (2) perfect various characterization techniques to establish the standard procedure for material characterization, (3) quantitatively establish the characteristics of the crystals grown on Earth as a basis for subsequent comparative evaluations of the crystals grown in a low-gravity environment and (4) develop theoretical and analytical methods required for such evaluations. ZnSe and related ternary compounds have been grown by vapor transport technique with real time in-situ non-invasive monitoring techniques. The grown crystals have been characterized extensively by various techniques to correlate the grown crystal properties with the growth conditions.

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.

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.

Process development and characterization of centrosymmetric semiorganic nonlinear optical crystal: 4-dimethylaminopyridine potassium chloride

NASA Astrophysics Data System (ADS)

Johnson, J.; Srineevasan, R.; Sivavishnu, D.

2018-06-01

Centrosymmetric semiorganic crystal 4-dimethylaminopyridine potassium chloride (4-DMAPKC) has been grown successfully by using slow evaporation solution growth technique. Powder x-ray diffraction shows the 4-DMAPKC crystal has good crystalline nature. Single crystal XRD shows that the grown 4-DMAPKC is cubic crystal system with cell parameters a = 3.09 Å, b = 3.09 Å, c = 3.09 Å. Investigation has been carried out to assign the Vibrational frequencies of the grown crystal by FTIR spectral studies. UVsbnd Visible NIR optical absorption spectral studies in the range of 200-1100 nm shows low absorption in UVsbnd Visible region with lower cutoff wave length at 261 nm and optical band gap energy was found as Eg = 5.52 eV. Optically transmittance spectral shows 4-DMAPKC crystal is very good transparency in UV-Visible NIR region. Thermogravimetry and differential thermal (TG-DTA) analysis were carried out. Dielectric studies of as grown crystal sample exhibit low dielectric constant and loss at higher frequencies and attests the nonlinear optical activity. Micro hardness studies of as grown crystal were discussed. Second harmonic generation (SHG) efficiency of the 4-DMAPKC is 0.69 times as that of KDP.

Growth and characterization of benzyl 4-hydroxybenzoate single crystal by vertical Bridgman technique for optical applications

NASA Astrophysics Data System (ADS)

Solanki, S. Siva Bala; Rajesh, N. P.; Suthan, T.

2018-07-01

The benzyl 4-hydroxybenzoate single crystal has been grown by vertical Bridgman technique. The grown crystal was confirmed by single crystal X-ray diffraction studies. The presence of functional groups in the crystal was confirmed by Fourier transform infrared (FTIR) spectral studies. The thermal behaviour of the grown crystal was analyzed by thermogravimetric analysis (TGA), differential thermal analysis (DTA) and differential scanning calorimetric (DSC) studies. Optical behaviour of the grown benzyl 4-hydroxybenzoate crystal was studied by UV-Vis-NIR spectral analysis. Fluorescence spectrum shows near violet light emission. The second harmonic generation behaviour of benzyl 4-hydroxybenzoate was analyzed. The laser damage threshold value of benzyl 4-hydroxybenzoate was measured as 2.16 GW/cm2. The dielectric measurements of benzyl 4-hydroxybenzoate crystal were carried out with different frequencies 1 kHz to 1 MHz versus different temperatures ranging from 313 to 353 K. Photoconductivity study shows that the grown benzyl 4-hydroxybenzoate crystal belongs to negative photoconductivity property. The mechanical strength of the crystal was calculated by Vickers microhardness study.

Habit control of deuterated potassium dihydrogen phosphate crystal for laser applications

NASA Astrophysics Data System (ADS)

Guzman, L. A.; Suzuki, M.; Fujimoto, Y.; Fujioka, K.

2016-03-01

In this study we investigate the habit of partially deuterated potassium dihydrogen phosphate (DKDP) crystals in the presence of Al3+ ions. We have grown single DKDP crystals in (50wt% and 80wt%) partially deuterated solutions and in solutions doped with Al3+ ions (2 ppm) by the point-seed rapid growth technique at controlled supercooling (ΔT=10°C). The growth length of each crystal face was measured and the aspect ratio was calculated. We found that crystals grown in partially deuterated solutions are similar in aspect ratio, while, crystals grown in deuterated solutions doped with Al3+ ions showed a relative change in aspect ratio, the crystal increased in size in the pyramidal direction (vertical axis direction). Crystal characteristics were also analyzed by X-ray diffraction, FTIR and Raman spectroscopy. We have speculated that the relative habit modification is due to a probably adsorption and inclusions of Al3+ ions in the prismatic section of the crystal.

Simulation of the temperature distribution in crystals grown by Czochralski method

NASA Technical Reports Server (NTRS)

Dudokovic, M. P.; Ramachandran, P. A.

1985-01-01

Production of perfect crystals, free of residual strain and dislocations and with prescribed dopant concentration, by the Czochralski method is possible only if the complex, interacting phenomena that affect crystal growth in a Cz-puller are fully understood and quantified. Natural and forced convection in the melt, thermocapillary effect and heat transfer in and around the crystal affect its growth rate, the shape of the crystal-melt interface and the temperature gradients in the crystal. The heat transfer problem in the crystal and between the crystal and all other surfaces present in the crystal pulling apparatus are discussed at length. A simulation and computer algorithm are used, based on the following assumptions: (1) only conduction occurs in the crystal (experimentally determined conductivity as a function of temperature is used), (2) melt temperature and the melt-crystal heat transfer coefficient are available (either as constant values or functions of radial position), (3) pseudo-steady state is achieved with respect to temperature gradients, (4) crystal radius is fixed, and (5) both direct and reflected radiation exchange occurs among all surfaces at various temperatures in the crystal puller enclosure.

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.

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

NASA Technical Reports Server (NTRS)

2003-01-01

The objective of the project is to determine the relative contributions of gravity-driven fluid flows to the compositional distribution, incorporation of impurities and defects, and deviation from stoichiometry observed in the crystals grown by vapor transport as results of buoyancy-driven convection and growth interface fluctuations caused by irregular fluid-flows. ZnSe and related ternary compounds, such as ZnSeS and ZnSeTe, were grown by vapor transport technique with real time in situ non-invasive monitoring techniques. The grown crystals were characterized extensively to correlate the grown crystal properties with the growth conditions. Significant effects of gravity vector orientation on the growth crystal morphology and point defect distribution were observed.

Insulin structure and stability.

PubMed

Brange, J; Langkjoer, L

1993-01-01

property of being able to counteract associated insulin from being disassembled. Chemical deterioration of insulin during storage of pharmaceutical preparations is mainly due to two categories of chemical reactions, hydrolysis and intermolecular transformation reactions leading to insulin HMWT products. The predominant hydrolysis reaction is deamidation of Asn residues which in acid solution takes place at residue A21, in neutral medium at residue B3. An amazing hydrolytic cleavage of the backbone A chain, presumably autocatalyzed by an adjacent insulin molecule, has been identified in insulin preparations containing rhombohedral crystals in combination with free zinc ions.(ABSTRACT TRUNCATED AT 400 WORDS)

Modified Bridgman-Stockbarger growth and characterization of LiInSe{sub 2} single crystal

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

Vijayakumar, P., E-mail: ramasamyp@ssn.edu.in; Magesh, M., E-mail: ramasamyp@ssn.edu.in; Arunkumar, A., E-mail: ramasamyp@ssn.edu.in

2014-04-24

The LiInSe{sub 2} polycrystalline materials were successfully synthesized from melt and temperature oscillation method. 8 mm diameter and 32 mm length single crystal was grown from Bridgman-Stockbarger method with steady ampoule rotation. Crystalline phase was confirmed by powder XRD pattern. Thermo gravimetric and differential thermal analysis confirms that the melting point of the grown crystal is 897°C. Rutherford backscattering analysis (RBS) gives the crystal composition as Li{sub 0.8}In{sub 1.16}Se{sub 2.04}. The crystalline perfection of the grown crystal was analyzed by High resolution X-ray diffraction measurements (HRXRD). The electrical properties of the grown crystal were analyzed by Hall effect measurements andmore » it confirms the n-type semiconducting nature.« less

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.

Structural, optical, thermal and mechanical properties of Urea tartaric acid single crystals.

PubMed

Vinothkumar, P; Rajeswari, K; Kumar, R Mohan; Bhaskaran, A

2015-06-15

Urea tartaric acid (UT) an organic nonlinear optical (NLO) material was synthesized from aqueous solution and the crystals were grown by the slow evaporation technique. The single crystal X-ray diffraction (XRD) analysis revealed that the UT crystal belongs to the orthorhombic system. The functional groups of UT have been identified by the Fourier transform infrared spectral studies. The optical transparent window in the visible and near the IR regions was investigated. The transmittance of UT has been used to calculate the refractive index (n) as a function of the wavelength. The nonlinear optical property of the grown crystal has been confirmed by the Kurtz powder second harmonic generation test. The birefringence of the crystal was determined using a tungsten halogen lamp source. The laser induced surface damage threshold for the grown crystal was measured using the Nd:YAG laser. The anisotropic in mechanical property of the grown crystals was studied using Vicker's microhardness tester at different planes. The etch pit density of UT crystals was investigated. The thermal behavior of UT was investigated using the TG-DTA and DSC studies. Copyright © 2015 Elsevier B.V. All rights reserved.

Microgravity

NASA Image and Video Library

1998-06-03

Diabetic patients may someday reduce their insulin injections and lead more normal lives because of new insights gained through irnovative space research in which insulin crystals were grown on the Space Shuttle. Results from a 1994 insulin crystal growth experiment in space are leading to a new understanding of protein insulin. Lack of insulin is the cause of diabetes, a desease that accounts for one-seventh of the nation's health care costs. Dr. Marianna Long, associate director of the Center of Macromolecular Crystallography at the University of Alabama at Birmingham, is a co-investigator on the research. Photo credit: NASA/Marshall Space Flight Center (MSFC)

Photoluminescence characteristics of ZnTe bulk crystal and ZnTe epilayer grown on GaAs substrate by MOVPE

NASA Astrophysics Data System (ADS)

Lü, Hai-Yan; Mu, Qi; Zhang, Lei; Lü, Yuan-Jie; Ji, Zi-Wu; Feng, Zhi-Hong; Xu, Xian-Gang; Guo, Qi-Xin

2015-12-01

Excitation power and temperature-dependent photoluminescence (PL) spectra of the ZnTe epilayer grown on (100) GaAs substrate and ZnTe bulk crystal are investigated. The measurement results show that both the structures are of good structural quality due to their sharp bound excitonic emissions and absence of the deep level structural defect-related emissions. Furthermore, in contrast to the ZnTe bulk crystal, although excitonic emissions for the ZnTe epilayer are somewhat weak, perhaps due to As atoms diffusing from the GaAs substrate into the ZnTe epilayer and/or because of the strain-induced degradation of the crystalline quality of the ZnTe epilayer, neither the donor-acceptor pair (DAP) nor conduction band-acceptor (e-A) emissions are observed in the ZnTe epilayer. This indicates that by further optimizing the growth process it is possible to obtain a high-crystalline quality ZnTe heteroepitaxial layer that is comparable to the ZnTe bulk crystal. Project supported by the Specialized Research Fund for the Doctoral Program of Higher Education of China (Grant No. 20120131110006), the Key Science and Technology Program of Shandong Province, China (Grant No. 2013GGX10221), the Key Laboratory of Functional Crystal Materials and Device (Shandong University, Ministry of Education), China (Grant No. JG1401), the National Natural Science Foundation of China (Grant No. 61306113), the Major Research Plan of the National Natural Science Foundation of China (Grant No. 91433112), and the Partnership Project for Fundamental Technology Researches of the Ministry of Education, Culture, Sports, Science and Technology, Japan.

Synthesis, growth, structural, spectroscopic and optical studies of a semiorganic NLO crystal: zinc guanidinium phosphate.

PubMed

Suvitha, A; Murugakoothan, P

2012-02-01

The semi-organic nonlinear optical (NLO) crystal, zinc guanidinium phosphate (ZGuP) has been grown through synthesis between zinc sulphate, guanidine carbonate and orthophosphoric acid from its aqueous solution by slow solvent evaporation technique. Solubility of the synthesized material has been determined for various temperatures using water as solvent. The grown crystal has been characterized by powder X-ray diffraction to confirm the crystal structure. Investigation has been carried out to assign the vibrational frequencies of the grown crystals by Fourier transform infrared spectroscopy technique. (1)H and (13)C FT-NMR have been recorded to elucidate the molecular structure. The optical absorption study confirms the suitability of the crystal for device applications. The second harmonic generation (SHG) efficiency of ZGuP is found to be 1.825 times that of potassium dihydrogen phosphate (KDP). Thermal behavior of the grown crystals has been studied by thermogravimetric and differential thermal analysis. The mechanical properties of the grown crystals have been studied using Vickers microhardness tester. Copyright © 2011 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2009-08-01

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

Is it Possible to have the Similar Unit Cell in Crystals of Different form from the same Macromolecule? (A Case Study of Ribosome Crystals)

NASA Technical Reports Server (NTRS)

Karpova, E. A.; Rose, M. Franklin (Technical Monitor)

2000-01-01

Three different types of ribosome crystals were grown by the vapor diffusion technique in hanging drops as described in (1,2). The ribosome is a large asymmetric RNA-protein complex (2.3 million Da), which is protein syntheses machinery of the cell. In this poster we would like to discuss the features of ribosome crystallization. Ribosomes were purified from the thermophilic bacteria Thermus thermophilus by centrifugation (3). Three types of crystals (needle, flat tetragonal and tetragonal-like pyramid) can be grown from the same solution; furthermore, in the same drop using 10-15% 2-methyl-2,4- pentanediol as a precipitant. The crystals appeared in 5-48 hours. The crystals were stable and can co-exist in solution over long period of time. The kinetics of appearance of different crystal forms was different: first the needle crystals were grown, then the tetragonal, and finally the tetragonal pyramids. Later studies of the process of ribosome crystal growth depending on supersaturation showed that low supersaturation results in the appearance of tetragonal plates or tetragonal-like pyramids. An electron microscopy study, together with computer modeling, has shown that crystals of different forms have a high probability of having the same unit cell parameters. According to these experiments the following conclusion can be dranvn: the level of supersaturation of the macromolecule in a crystallizing solution is one of the major factors for forming three-dimensional crystals convenient for X-rays diffraction analysis. From the same macromolecule solution, crystals of different forms can be grown at approximately the same conditions by varying the concentration of macromolecule in the solution. Ion-macromolecule and water-macromolecule interactions, apparently, play the main role in the formation of the unit cell of the crystals.

Growth and characterization of struvite-Na crystals

NASA Astrophysics Data System (ADS)

Chauhan, Chetan K.; Joshi, Mihirkumar J.

2014-09-01

Sodium magnesium phosphate heptahydrate [NaMgPO4·7H2O], also known as struvite-Na, is the sodium analog to struvite. Among phosphate containing bio-minerals, struvite has attracted considerable attention, because of its common occurrence in a wide variety of environments. Struvite and family crystals were found as urinary calculi in humans and animals. Struvite-Na crystals were grown by a single diffusion gel growth technique in a silica hydro gel medium. Struvite-Na crystals with different morphologies having transparent to translucent diaphaneity were grown with different growth parameters. The phenomenon of Liesegang rings was also observed with some particular growth parameters. The powder XRD study confirmed the structural similarity of the grown struvite-Na crystals with struvite and found that struvite-Na crystallized in the orthorhombic Pmn21 space group with unit cell parameters such as a= 6.893 Å, b=6.124 Å, c=11.150 Å, and α=β=γ=90°. FT-IR spectra of struvite-Na crystals revealed the presence of functional groups. The TGA, DTA and DSC were carried out simultaneously. The kinetic and thermodynamic parameters of dehydration/decomposition process were calculated. The variation of dielectric constant with frequency of applied field was studied in the range from 400 Hz to 100 kHz.

Studies on the growth, structural, spectral and third-order nonlinear optical properties of ammonium 3-carboxy-4-hydroxy benzenesulfonate monohydrate single crystal.

PubMed

Silambarasan, A; Krishna Kumar, M; Thirunavukkarasu, A; Mohan Kumar, R; Umarani, P R

2015-01-25

An organic nonlinear optical bulk single crystal, Ammonium 3-carboxy-4-hydroxy benzenesulfonate monohydrate (ACHBS) was successfully grown by solution growth technique. Single crystal X-ray diffraction study confirms that, the grown crystal belongs to P21/c space group. Powder X-ray diffraction and high resolution X-ray diffraction analyses revealed the crystallinity of the grown crystal. Infrared spectral analysis showed the vibrational behavior of chemical bonds and its functional groups. The thermal stability and decomposition stages of the grown crystal were studied by TG-DTA analysis. UV-Visible transmittance studies showed the transparency region and cut-off wavelength of the grown crystal. The third-order nonlinear optical susceptibility of the grown crystal was estimated by Z-scan technique using He-Ne laser source. The mechanical property of the grown crystal was studied by using Vicker's microhardness test. Copyright © 2014 Elsevier B.V. All rights reserved.

Growth and characterization of CaCu3Ti4O12 single crystals

NASA Astrophysics Data System (ADS)

Kim, Hui Eun; Yang, Sang-don; Lee, Jung-Woo; Park, Hyun Min; Yoo, Sang-Im

2014-12-01

The CaCu3Ti4O12 (CCTO) single crystals could be grown from the melt with the nominal composition of Ca:Cu:Ti=1:59:20 in a platinum (Pt) crucible using a self-flux method. The flux-grown CCTO single crystals have well-developed {100} habit planes, and their compositions are close to the ratio of Ca:Cu:Ti=1:3:4. Interestingly, flux-grown CCTO single crystals exhibited two different back reflection Laue patterns; one exhibited only [100] cubic Laue patterns, and the other showed not only [100] cubic Laue patterns but also the satellite spots related to the twin boundary, implying that twin-free CCTO single crystals can be grown by the self-flux method. Both the dielectric constants and losses of twinned CCTO single crystal are significantly higher than those of untwined CCTO crystal at relatively low frequency regime (<10 kHz), suggesting that the dielectric property is sensitive to the twin boundary.

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.

Crystal growth, structural, optical, thermal, mechanical, laser damage threshold and electrical properties of triphenylphosphine oxide 4-nitrophenol (TP4N) single crystals for nonlinear optical applications

NASA Astrophysics Data System (ADS)

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

2018-05-01

The optically good quality single crystals of triphenylphosphine oxide 4-nitrophenol (TP4N) with maximum dimension of 15 × 10 × 5 mm3 were grown by slow evaporation solution technique (SEST) at room temperature. The cell dimensions of the grown TP4N crystal were confirmed by single crystal X-ray diffraction (SXRD) and the crystalline purity was confirmed and planes were indexed by powder X-ray diffraction (PXRD) analysis. Functional groups of TP4N crystal were confirmed by Fourier transform infrared (FTIR) spectral analysis. The optical transmittance of the grown crystal was determined by the UV-Vis NIR spectral analysis and it has good optical transparency in the entire visible region. The band tail (Urbach) energy of the grown crystal was analyzed and it appears to be minimum, which indicates that the TP4N has good crystallinity. The position of valence band (Ev) and conduction band (Ec) of the TP4N have been determined from the electron affinity energy (EA) and the ionization energy (EI) of its elements and using the optical band gap. The thermal behaviour of the grown crystal was investigated by thermogravimetric and differential thermal analysis (TG-DTA). Vickers microhardness analysis was carried out to identify the mechanical stability of the grown crystal and their indentation size effect (ISE) was explained by the Meyer's law (ML), Hays-Kendall's (HK) approach, proportional specimen resistance (PSR) model, modified PSR model (MPSR), elastic/plastic deformation (EPD) model and indentation induced cracking (IIC) model. Chemical etching study was carried out to find the etch pit density (EPD) of the grown crystal. Laser damage threshold (LDT) value was measured by using Nd:YAG laser (1064 nm). The dielectric permittivity (ε՛) and dielectric loss (tan δ) as a function of frequency was measured. The electronic polarizability (α) of the TP4N crystal was calculated. It is well matched to the value which was calculated from Clausius-Mossotti relation

Growth and surface topography of WSe{sub 2} single crystal

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

Dixit, Vijay, E-mail: vijdix1@gmail.com; Vyas, Chirag; Pataniya, Pratik

2016-05-06

Tungsten Di-Selenide belongs to the family of TMDCs showing their potential applications in the fields of Optoelectronics and PEC solar cells. Here in the present investigation single crystals of WSe{sub 2} were grown by Direct Vapour Transport Technique in a dual zone furnace having temperature difference of 50 K between the two zones. These single crystals were characterized by EDAX which confirms the stiochiometry of the grown crystals. Surface topography of the crystal was studied by optical micrograph showing the left handed spirals on the surface of WSe{sub 2} crystals. Single crystalline nature of the crystals was confirmed by SAED.

Spray printing of organic semiconducting single crystals

NASA Astrophysics Data System (ADS)

Rigas, Grigorios-Panagiotis; Payne, Marcia M.; Anthony, John E.; Horton, Peter N.; Castro, Fernando A.; Shkunov, Maxim

2016-11-01

Single-crystal semiconductors have been at the forefront of scientific interest for more than 70 years, serving as the backbone of electronic devices. Inorganic single crystals are typically grown from a melt using time-consuming and energy-intensive processes. Organic semiconductor single crystals, however, can be grown using solution-based methods at room temperature in air, opening up the possibility of large-scale production of inexpensive electronics targeting applications ranging from field-effect transistors and light-emitting diodes to medical X-ray detectors. Here we demonstrate a low-cost, scalable spray-printing process to fabricate high-quality organic single crystals, based on various semiconducting small molecules on virtually any substrate by combining the advantages of antisolvent crystallization and solution shearing. The crystals' size, shape and orientation are controlled by the sheer force generated by the spray droplets' impact onto the antisolvent's surface. This method demonstrates the feasibility of a spray-on single-crystal organic electronics.

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.

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

NASA Technical Reports Server (NTRS)

Su, Ching-Hua; Brebrick, R. F.; Burger, A.; Dudley, M.; Ramachandran, N.

2003-01-01

The objective of the project is to determine the relative contributions of gravity-driven fluid flows to the compositional distribution, incorporation of impurities and defects, and deviation from stoichiometry observed in the crystals grown by vapor transport as results of 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.

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

Preliminary investigations of protein crystal growth using the Space Shuttle

NASA Technical Reports Server (NTRS)

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

1986-01-01

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

Solvent minimization induces preferential orientation and crystal clustering in serial micro-crystallography on micro-meshes, in situ plates and on a movable crystal conveyor belt.

PubMed

Soares, Alexei S; Mullen, Jeffrey D; Parekh, Ruchi M; McCarthy, Grace S; Roessler, Christian G; Jackimowicz, Rick; Skinner, John M; Orville, Allen M; Allaire, Marc; Sweet, Robert M

2014-11-01

X-ray diffraction data were obtained at the National Synchrotron Light Source from insulin and lysozyme crystals that were densely deposited on three types of surfaces suitable for serial micro-crystallography: MiTeGen MicroMeshes™, Greiner Bio-One Ltd in situ micro-plates, and a moving kapton crystal conveyor belt that is used to deliver crystals directly into the X-ray beam. 6° wedges of data were taken from ∼100 crystals mounted on each material, and these individual data sets were merged to form nine complete data sets (six from insulin crystals and three from lysozyme crystals). Insulin crystals have a parallelepiped habit with an extended flat face that preferentially aligned with the mounting surfaces, impacting the data collection strategy and the design of the serial crystallography apparatus. Lysozyme crystals had a cuboidal habit and showed no preferential orientation. Preferential orientation occluded regions of reciprocal space when the X-ray beam was incident normal to the data-collection medium surface, requiring a second pass of data collection with the apparatus inclined away from the orthogonal. In addition, crystals measuring less than 20 µm were observed to clump together into clusters of crystals. Clustering required that the X-ray beam be adjusted to match the crystal size to prevent overlapping diffraction patterns. No additional problems were encountered with the serial crystallography strategy of combining small randomly oriented wedges of data from a large number of specimens. High-quality data able to support a realistic molecular replacement solution were readily obtained from both crystal types using all three serial crystallography strategies.

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.

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.

Regulation of insulin preRNA splicing by glucose

PubMed Central

Wang, Juehu; Shen, Luping; Najafi, Habiba; Kolberg, Janice; Matschinsky, Franz M.; Urdea, Mickey; German, Michael

1997-01-01

Glucose tightly regulates the synthesis and secretion of insulin by β cells in the pancreatic islets of Langerhans. To investigate whether glucose regulates insulin synthesis at the level of insulin RNA splicing, we developed a method to detect and quantify a small amount of RNA by using the branched DNA (bDNA) signal-amplification technique. This assay is both sensitive and highly specific: mouse insulin II mRNA can be detected from a single β cell (βTC3 cells or mouse islets), whereas 1 million non-insulin-producing α cells (αTC1.6 cells) give no signal. By using intron and exon sequences, oligonucleotide probes were designed to distinguish the various unspliced and partially spliced insulin preRNAs from mature insulin mRNA. Insulin RNA splicing rates were estimated from the rate of disappearance of insulin preRNA signal from β cells treated with actinomycin D to block transcription. We found that the two introns in mouse insulin II are not spliced with the same efficiency. Intron 2 is spliced out more efficiently than intron 1. As a result, some mRNA retaining intron 1 enters the cytoplasm, making up ≈2-10% of insulin mRNA in the cell. This partially spliced cytoplasmic mRNA is quite stable, with a half-life similar to the completely spliced form. When islets grown in high glucose are shifted to low glucose medium, the level of insulin preRNA and the rate of splicing fall significantly. We conclude that glucose stimulates insulin gene transcription and insulin preRNA splicing. Previous estimates of insulin transcription rates based on insulin preRNA levels that did not consider the rate of splicing may have underestimated the effect of glucose on insulin gene transcription. PMID:9113994

Growth, structural, optical and surface analysis of piperazinium tartrate: A NLO single crystal

NASA Astrophysics Data System (ADS)

Gupta, Apurva; Raseel Rahman M., K.; Nair, Lekha

2018-05-01

Single crystal of piperazinium tartrate (PPZT) was grown by the slow evaporation solution growth technique at room temperature. Crystallinity of grown crystal was examined by powder X-ray diffraction. High transparency and wide band gap were observed in the UV-Visible spectroscopic studies. Intense and broad emissions were observed in the blue region, as that is indicated by photoluminescence spectroscopy. The quality of the grown PPZT single crystals were analyzed by the etching studies using the water as the etchant.

Thermal, mechanical, optical and conductivity studies of a novel NLO active L-phenylalanine L-phenylalaninium dihydrogenphosphate single crystal

NASA Astrophysics Data System (ADS)

Sujatha, T.; Cyrac Peter, A.; Vimalan, M.; Merline Shyla, J.; Madhavan, J.

2010-08-01

An efficient, novel, semi-organic, nonlinear optical (NLO) material L-phenylalanine L-phenylalaninium dihydrogenphosphate (LPADHP), single crystal of dimension 11×5×2 mm 3, has been grown by the slow evaporation solution growth technique. Single crystal X-ray diffraction studies confirm that the grown crystal belongs to monoclinic system with the space group P2 1. The functional groups present in the crystal were confirmed by the Fourier transform infrared technique. Optical absorption spectrum shows that the material possesses very low absorption in the entire visible region. Thermal analysis confirmed that the crystal is thermally stable up to 161 °C. The frequency dependent dielectric properties of the grown crystal were studied for various temperatures. The second harmonic generation (SHG) efficiency of the grown crystal is 1.2 times greater than that of the potassium dihydrogenphosphate (KDP) single crystal. The laser induced surface damage threshold for the grown crystal was found to be 6.3 GW cm -2 with Nd:YAG laser assembly AC and DC conductivity and photoconductivity experiments are also carried out and the results are discussed.

The Effect of the Wall Contact and Post-Growth C001-Down on Defects in CdTe Crystals Grown by Contactless PVT

NASA Technical Reports Server (NTRS)

Palosz, W.; Grasza, K.; Dudley, M.; Raghothamachar, B.; Cai, L.; Durose, K.; Halliday, D.; Boyall, N. M.; Rose, M. Franklin (Technical Monitor)

2001-01-01

In crystal growth, the quality of the final material may depend, among other factors, on its interaction with the walls of the ampoule during and after the growth, and on the rate of the crystal cool-down at the end of ate the process. To investigate the above phenomena, a series of CdTe crystal growth processes was carried out, The crystals were grown by physical vapor transport without contact with the side walls of the silica glass ampoules, applying the Low Supersaturation Nucleation technique. The source temperature was 930 C, the undercooling was a few degrees. The crystals, having the diameter of 25 mm, grew at the rate of a few mm per day. The post-growth cool-down to the room temperature was conducted at different rates, and lasted from a few minutes to four days. The crystals were characterized using chemical etching low temperature luminescence, and Synchrotron White Beam X-ray Topography techniques. The dislocation (etch pit) density was measured and its distribution was analyzed by comparison with Poisson curves and with the Normalized Radial Distribution Correlation Function. It was found that the contact of the crystal with silica leads to a strain field and high (in the 105 sq cm range) dislocation (etch pit) density. Similar defect concentrations were found in crystals subjected to fast post-growth cool-down. Typical EPD values for lower cool-down rates and in regions not affected by wall interactions are in the lower 10(exp 4) sq cm range. In some areas the actual dislocation density was about 10(exp 3) sq cm or even less. No apparent effect of the cool-down rate on polygonization was observed. A fine structure could be discerned in low-temperature PL spectra of crystals with low dislocation density.

Influence of growth temperature on properties of zirconium dioxide films grown by atomic layer deposition

NASA Astrophysics Data System (ADS)

Kukli, Kaupo; Ritala, Mikko; Aarik, Jaan; Uustare, Teet; Leskela, Markku

2002-08-01

ZrO2 films were grown by atomic layer deposition from ZrCl4 and H2O or a mixture of H2O and H2O2 on Si(100) substrates in the temperature range of 180-600 degC. The films were evaluated in the as-deposited state, in order to follow the effect of deposition temperature on the film quality. The rate of crystal growth increased and the content of residual impurities decreased with increasing temperature. The zirconium-to-oxygen atomic ratio, determined by ion-beam analysis, corresponded to the stoichiometric dioxide regardless of the growth temperature. The effective permittivity of ZrO2 in Al/ZrO2/Si capacitor structures increased from 13-15 in the films grown at 180 degC to 19 in the films grown at 300-600 degC, measured at 100 kHz. The permittivity was relatively high in the crystallized films, compared to the amorphous ones, but rather insensitive to the crystal structure. The permittivity was higher in the films grown using water. The leakage current density tended to be lower and the breakdown field higher in the films grown using hydrogen peroxide.

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

DOEpatents

Zaitseva, Natalia; Carman, M Leslie; Payne, Steve

2014-10-28

An organic crystal according to one embodiment includes an organic crystal comprising diphenylacetylene and stilbene or a stilbene derivative, the crystal having physical characteristics of formation 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 comprising diphenylacetylene and stilbene or a stilbene derivative, the 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. Methods of making such crystals are also provided.

Microgravity

NASA Image and Video Library

2004-04-15

The manipulation of organic materials--cells, tissues, and even living organisms--offers many exciting possibilities for the future from organic computers to improved aquaculture. Commercial researchers are using the microgravity environment to produce large near perfect protein crystals Research on insulin has yielded crystals that far surpass the quality of insulin crystals grown on the ground. Using these crystals industry partners are working to develop new and improved treatments for diabetes. Other researchers are exploring the possibility of producing antibiotics using plant cell cultures which could lead to both orbital production and the improvement of ground-based antibiotic production.

Chemical stability of insulin. 5. Isolation, characterization and identification of insulin transformation products.

PubMed

Brange, J; Hallund, O; Sørensen, E

1992-01-01

During storage of insulin formulated for therapy, minor amounts of various degradation and covalent di- and polymerization products are formed [1-3]. The main chemical transformation products were isolated from aged preparations and characterized chemically and biologically. The most prominent products formed in neutral medium were identified as a mixture of deamidation products hydrolyzed at residue B3, namely isoAsp B3 and Asp B3 derivatives. A hydrolysis product formed only in crystals of insulin zinc suspensions containing a surplus of zinc ions in the supernatant was identified as an A8-A9 cleavage product. The small amounts of covalent insulin dimers (CID) formed in all formulations were shown to be a heterogenous mixture of 5-6 different CIDs with a composition dependent on the pharmaceutical formulation. The chemical characteristics of the CIDs indicate that they are formed through a transamidation reaction mainly between the B-chain N-terminal and one of the four amide side-chains of the A chain. GlnA15, AsnA18 and, in particular, AsnA21 participate in the formation of such isopeptide links between two insulin molecules. The covalent insulin-protamine products (CIPP) formed during storage of NPH preparations presumably originate from a similar reaction between the protamine N-terminal with an amide in insulin. Covalent polymerization products, mainly formed during storage of amorphously suspended insulin at higher temperature, were shown to be due to disulfide interactions. Biological in vivo potencies relative to native insulin were less than 2% for the split-(A8-A9)-product and for the covalent disulfide exchange polymers, 4% for the CIPP, approximately 15% for the CIDs, whereas the B3 derivatives exhibited full potency. Rabbit immunization experiments revealed that none of the insulin transformation products had significantly increased immunogenicity in rabbits.

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.

Synthesis, growth, structural, optical and thermal properties of an organic single crystal: 4-nitroaniline 4-aminobenzoic acid.

PubMed

Silambarasan, A; Rajesh, P; Ramasamy, P

2014-01-24

The organic single crystals of 4-nitroaniline 4-aminobenzoic acid (4NAABA) were grown from ethanol solvent. The lattice parameters of the grown crystal have been confirmed from single crystal XRD analysis. The powder XRD pattern shows the various planes of grown crystal. The FTIR and (1)H NMR spectral analysis confirm the presence of various functional groups and the placement of proton in 4NAABA compound respectively. The UV absorption was carried out which shows the cutoff wavelength around 459 nm. The optical band gap of the crystal has been evaluated from the transmission spectra and absorption coefficient by extrapolation technique. In addition, a fluorescence spectral analysis is carried out for 4NAABA crystals. The thermal properties of crystals were evaluated from thermogravimetrical analysis. It shows that the grown crystal is stable up to 160°C and the crystal has sharp melting point at 151°C. Copyright © 2013 Elsevier B.V. All rights reserved.

Three-dimensional evaluation of gettering ability for oxygen atoms at small-angle tilt boundaries in Czochralski-grown silicon crystals

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

Ohno, Yutaka, E-mail: yutakaohno@imr.tohoku.ac.jp; Inoue, Kaihei; Fujiwara, Kozo

2015-06-22

Three-dimensional distribution of oxygen atoms at small-angle tilt boundaries (SATBs) in Czochralski-grown p-type silicon ingots was investigated by atom probe tomography combined with transmission electron microscopy. Oxygen gettering along edge dislocations composing SATBs, post crystal growth, was observed. The gettering ability of SATBs would depend both on the dislocation strain and on the dislocation density. Oxygen atoms would agglomerate in the atomic sites under the tensile hydrostatic stress larger than about 2.0 GPa induced by the dislocations. It was suggested that the density of the atomic sites, depending on the tilt angle of SATBs, determined the gettering ability of SATBs.

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.

A novel organic nonlinear optical crystal: Creatininium succinate

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

Thirumurugan, R.; Anitha, K., E-mail: singlecerystalxrd@gmail.ciom

2015-06-24

A novel organic material complex of creatininium succinate (CS) has been synthesized and single crystals were grown by the reaction of creatinine and succinic acid from aqueous solution by employing the technique of slow evaporation at room temperature. The structure of the grown crystal has been elucidated using single crystal X-ray diffraction analysis and the structure was refined by least-squares method to R = 0.027 for 1840 reflections. FT-IR spectral investigation has been carried out to identify the various functional groups in the title compound. UV–Vis transmission was carried out which shows the crystal has a good optical transmittance inmore » the visible region with lower cutoff wavelength around 220 nm. Nonlinear optical property of the crystal was confirmed by Kurtz-Perry powder technique.« less

Solvent minimization induces preferential orientation and crystal clustering in serial micro-crystallography on micro-meshes, in situ plates and on a movable crystal conveyor belt

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

Soares, Alexei S.; Mullen, Jeffrey D.; Parekh, Ruchi M.

X-ray diffraction data were obtained at the National Synchrotron Light Source from insulin and lysozyme crystals that were densely deposited on three types of surfaces suitable for serial micro-crystallography: MiTeGen MicroMeshes™, Greiner Bio-One Ltdin situmicro-plates, and a moving kapton crystal conveyor belt that is used to deliver crystals directly into the X-ray beam. 6° wedges of data were taken from ~100 crystals mounted on each material, and these individual data sets were merged to form nine complete data sets (six from insulin crystals and three from lysozyme crystals). Insulin crystals have a parallelepiped habit with an extended flat face thatmore » preferentially aligned with the mounting surfaces, impacting the data collection strategy and the design of the serial crystallography apparatus. Lysozyme crystals had a cuboidal habit and showed no preferential orientation. Preferential orientation occluded regions of reciprocal space when the X-ray beam was incident normal to the data-collection medium surface, requiring a second pass of data collection with the apparatus inclined away from the orthogonal. In addition, crystals measuring less than 20 µm were observed to clump together into clusters of crystals. Clustering required that the X-ray beam be adjusted to match the crystal size to prevent overlapping diffraction patterns. No additional problems were encountered with the serial crystallography strategy of combining small randomly oriented wedges of data from a large number of specimens. Lastly, high-quality data able to support a realistic molecular replacement solution were readily obtained from both crystal types using all three serial crystallography strategies.« less

Solvent minimization induces preferential orientation and crystal clustering in serial micro-crystallography on micro-meshes, in situ plates and on a movable crystal conveyor belt

DOE PAGES

Soares, Alexei S.; Mullen, Jeffrey D.; Parekh, Ruchi M.; ...

2014-10-09

X-ray diffraction data were obtained at the National Synchrotron Light Source from insulin and lysozyme crystals that were densely deposited on three types of surfaces suitable for serial micro-crystallography: MiTeGen MicroMeshes™, Greiner Bio-One Ltdin situmicro-plates, and a moving kapton crystal conveyor belt that is used to deliver crystals directly into the X-ray beam. 6° wedges of data were taken from ~100 crystals mounted on each material, and these individual data sets were merged to form nine complete data sets (six from insulin crystals and three from lysozyme crystals). Insulin crystals have a parallelepiped habit with an extended flat face thatmore » preferentially aligned with the mounting surfaces, impacting the data collection strategy and the design of the serial crystallography apparatus. Lysozyme crystals had a cuboidal habit and showed no preferential orientation. Preferential orientation occluded regions of reciprocal space when the X-ray beam was incident normal to the data-collection medium surface, requiring a second pass of data collection with the apparatus inclined away from the orthogonal. In addition, crystals measuring less than 20 µm were observed to clump together into clusters of crystals. Clustering required that the X-ray beam be adjusted to match the crystal size to prevent overlapping diffraction patterns. No additional problems were encountered with the serial crystallography strategy of combining small randomly oriented wedges of data from a large number of specimens. Lastly, high-quality data able to support a realistic molecular replacement solution were readily obtained from both crystal types using all three serial crystallography strategies.« less

Solvent minimization induces preferential orientation and crystal clustering in serial micro-crystallography on micro-meshes, in situ plates and on a movable crystal conveyor belt

PubMed Central

Soares, Alexei S.; Mullen, Jeffrey D.; Parekh, Ruchi M.; McCarthy, Grace S.; Roessler, Christian G.; Jackimowicz, Rick; Skinner, John M.; Orville, Allen M.; Allaire, Marc; Sweet, Robert M.

2014-01-01

X-ray diffraction data were obtained at the National Synchrotron Light Source from insulin and lysozyme crystals that were densely deposited on three types of surfaces suitable for serial micro-crystallography: MiTeGen MicroMeshes™, Greiner Bio-One Ltd in situ micro-plates, and a moving kapton crystal conveyor belt that is used to deliver crystals directly into the X-ray beam. 6° wedges of data were taken from ∼100 crystals mounted on each material, and these individual data sets were merged to form nine complete data sets (six from insulin crystals and three from lysozyme crystals). Insulin crystals have a parallelepiped habit with an extended flat face that preferentially aligned with the mounting surfaces, impacting the data collection strategy and the design of the serial crystallography apparatus. Lysozyme crystals had a cuboidal habit and showed no preferential orientation. Preferential orientation occluded regions of reciprocal space when the X-ray beam was incident normal to the data-collection medium surface, requiring a second pass of data collection with the apparatus inclined away from the orthogonal. In addition, crystals measuring less than 20 µm were observed to clump together into clusters of crystals. Clustering required that the X-ray beam be adjusted to match the crystal size to prevent overlapping diffraction patterns. No additional problems were encountered with the serial crystallography strategy of combining small randomly oriented wedges of data from a large number of specimens. High-quality data able to support a realistic molecular replacement solution were readily obtained from both crystal types using all three serial crystallography strategies. PMID:25343789

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

NASA Astrophysics Data System (ADS)

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

1997-11-01

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

Convection effects in protein crystal growth

NASA Technical Reports Server (NTRS)

Roberts, Glyn O.

1988-01-01

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

Crystal growth of HVPE-GaN doped with germanium

NASA Astrophysics Data System (ADS)

Iwinska, M.; Takekawa, N.; Ivanov, V. Yu.; Amilusik, M.; Kruszewski, P.; Piotrzkowski, R.; Litwin-Staszewska, E.; Lucznik, B.; Fijalkowski, M.; Sochacki, T.; Teisseyre, H.; Murakami, H.; Bockowski, M.

2017-12-01

Crystallization by hydride vapor phase epitaxy method of gallium nitride single crystals doped with germanium and properties of the obtained material are described in this paper. Growth was performed in hydrogen and nitrogen carrier gas. The results were studied and compared. Influence of different flows of germanium tetrachloride, precursor of germanium, on the grown crystals was investigated. Ammonothermal GaN substrates were used as seeds for crystallization. Structural, electrical, and optical properties of HVPE-GaN doped with germanium are presented and discussed in detail. They were compared to properties of HVPE-GaN doped with silicon and also grown on native seeds of high quality.

Growth and characterization of Methyl 2-amino-5-bromobenzoate crystal for NLO applications

NASA Astrophysics Data System (ADS)

Parthasarathy, M.; Gopalakrishnan, R.

2012-11-01

Good quality single crystal of organic Methyl 2-amino-5-bromobenzoate (M2A5B) was grown using slow evaporation solution growth technique. The grown crystal was confirmed by single crystal X-ray diffraction. The functional groups and vibrational frequencies were identified using FT-IR and FT-Raman spectral analyses. The presence of hydrogen and carbon atoms in the grown sample was confirmed with proton and carbon NMR spectral studies. The optical energy band gap of the title compound is found to be 2.7 eV from the optical transmission spectra. The refractive indices nx, ny, and nz were found to be 1.569, 1.587 and 1.600, respectively using Brewster's angle method. The melting point of the material obtained with melting point apparatus is 74 °C. Thermal stability of the grown crystal was studied by thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The mechanical behaviour of the grown crystal was analyzed with Vicker's microhardness tester. The particle size dependent second harmonic generation efficiency for M2A5B was evaluated by Kurtz-Perry powder method using Nd:YAG laser, which established the existence of phase matching.

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.

Growth and characterization of a novel nonlinear optical borate crystal - Yttrium calcium borate (YCB)

NASA Astrophysics Data System (ADS)

Arun Kumar, R.; Arivanandhan, M.; Dhanasekaran, R.; Hayakawa, Y.

2013-06-01

A new nonlinear optical single crystal yttrium calcium borate Y2CaB10O19 (YCB) was grown for the first time from its melt. The starting materials were prepared by the solid-state reaction method. The melting point of the synthesized material was identified to be 967 °C. YCB crystal exhibits monoclinic crystal structure with the space group C2. The crystalline perfection of the grown YCB crystal was found to be good. From the UV-VIS-NIR studies, the lower cutoff wavelength of the crystal occurs below 200 nm. The functional groups of the grown crystal were assigned using the FTIR data. The second harmonic generation (SHG) of the YCB crystal was observed using a Nd:YAG laser with a fundamental wavelength of 1064 nm. The laser damage threshold value of the YCB crystal was found to be very high - 10.5 GW/cm2.

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.

Boost the electron mobility of solution-grown organic single crystals via reducing the amount of polar solvent residues

DOE PAGES

Xue, Guobiao; Xin, Huolin L.; Wu, Jiake; ...

2015-10-29

Enhancing electron transport to match with the development in hole transport is critical for organic electronics in the future. As electron motion is susceptible to extrinsic factors, seeking these factors and avoiding their negative effects have become the central challenge. Here, the existence of polar solvent residues in solution-grown single-crystals of 6,13-bis(triisopropylsilylethynyl)-5,7,12,14-tetraazapentacene is identified as a factor detrimental to electron motion. Field-effect transistors of the crystals exhibit electron mobility boosted by about 60% after the residues are removed. The average electron mobility reaches up to 8.0 ± 2.2 cm 2 V –1 s –1 with a highest value of 13.3more » cm 2 V –1 s –1; these results are significantly higher than those obtained previously for the same molecule (1.0–5.0 cm 2 V –1 s –1). Furthermore, the achieved mobility is also higher than the maximum reported electron mobility for organic materials (11 cm 2 V –1 s –1). As a result, this work should greatly accelerate the advancement of organic electron-transporting materials.« less

Studies on synthesis, growth, structural, thermal, linear and nonlinear optical properties of organic picolinium maleate single crystals.

PubMed

Pandi, P; Peramaiyan, G; Sudhahar, S; Chakkaravarthi, G; Mohan Kumar, R; Bhagavannarayana, G; Jayavel, R

2012-12-01

Picolinium maleate (PM), an organic material has been synthesised and single crystals were grown by slow evaporation technique. The structure of the grown crystal was elucidated by using single crystal X-ray diffraction analysis. PM crystal belongs to the monoclinic crystallographic system with space group P2(1)/c. The crystalline perfection of the grown crystals was analyzed by high-resolution X-ray diffraction rocking curve measurements. The presence of functional groups in PM was identified by FTIR and FT-NMR spectral analyses. Thermal behaviour and stability of picolinium maleate were studied by TGA/DTA analyses. UV-Vis spectral studies reveal that PM crystals are transparent in the wavelength region 327-1100 nm. The laser damage threshold value of PM crystal was found to be 4.3 GW/cm(2) using Nd:YAG laser. The Kurtz and Perry powder second harmonic generation technique confirms the nonlinear optical property of the grown crystal. Copyright © 2012 Elsevier B.V. All rights reserved.

Crystal growth, thermal and optical studies of semiorganic nonlinear optical material: L-lysine hydrochloride dihydrate

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

Kalaiselvi, D.; Mohan Kumar, R.; Jayavel, R.

2008-07-01

Single crystals of L-lysine hydrochloride dihydrate (LLHCD), a nonlinear optical material, have been grown by slow cooling technique from its aqueous solution. LLHCD was found to be highly soluble in water. The grown crystals have been subjected to single crystal X-ray diffraction to confirm the structure and to estimate the lattice parameters. The vibrational structure of the molecule is elucidated from FTIR spectra. Thermal analysis revealed the thermal stability of the grown crystals. The optical transmittance spectrum shows that the material possesses good optical transparency in the entire visible region with a UV cut-off wavelength at 228 nm. The mechanicalmore » properties of the grown crystal have been studied using Vicker's microhardness test. The laser damage threshold of 52.25 MW/cm{sup 2} has been measured by irradiating Q-switched Nd:YAG laser (1064 nm)« less

Growth, structural, thermal, linear and nonlinear optical and laser damage threshold studies of picolinium tartrate monohydrate single crystals.

PubMed

Peramaiyan, G; Pandi, P; Sornamurthy, B M; Bhagavannarayana, G; Mohan Kumar, R

2012-09-01

Picolinium tartrate monohydrate (PTM), a novel organic nonlinear optical material was synthesized and bulk crystals were grown from aqueous solution by slow cooling technique. The cell parameters of the grown crystal were found by single and powder X-ray diffraction analyses. The crystalline perfection of the grown crystals has been analyzed by high-resolution X-ray diffraction (HRXRD) rocking curve measurements. The presence of functional groups in the grown crystal was identified by FTIR and FT-Raman spectral analyses. UV-Vis spectral studies reveal PTM crystals are transparent in the wavelength region of 295-1100 nm. The thermal characteristics of PTM were analyzed by TGA/DTA studies. The dielectric and mechanical behaviours of PTM crystals were investigated. Dislocation density was estimated to be 2.89 × 10(3) cm(-2) on the flat-surface of PTM crystals from the etching studies. The laser induced surface damage threshold for the grown crystal was measured using Nd:YAG laser. Its second harmonic generation relative efficiency was measured by Kurtz and Perry powder technique and was observed to be comparable with KDP crystal. Copyright © 2012 Elsevier B.V. All rights reserved.

The Growth of Protein Crystals Using McDUCK

NASA Technical Reports Server (NTRS)

Ewing, Felicia; Wilson, Lori; Nadarajah, Arunan; Pusey, Marc

1998-01-01

Most of the current microgravity crystal growth hardware is optimized to produce crystals within the limited time available on orbit. This often results in the actual nucleation and growth process being rushed or the system not coming to equilibrium within the limited time available. Longer duration hardware exists, but one cannot readily pick out crystals grown early versus those which nucleated and grew more slowly. We have devised a long duration apparatus, the Multi-chamber Dialysis Unit for Crystallization Kinetics, or McDUCK. This apparatus-is a series of protein chambers, stacked upon a precipitant reservoir chamber. All chambers are separated by a dialysis membrane, which serves to pass small molecules while retaining the protein. The volume of the Precipitant chamber is equal to the sum of the volumes of the protein chamber. In operation, the appropriate chambers are filled with precipitant solution or protein solution, and the McDUCK is placed standing upright, with the precipitant chamber on the bottom. The precipitant diffuses upwards over time, with the time to reach equilibration a function of the diffusivity of the precipitant and the overall length of the diffusion pathway. Typical equilibration times are approximately 2-4 months, and one can readily separate rapid from slow nucleation and growth crystals. An advantage on Earth is that the vertical precipitant concentration gradient dominates that of the solute, thus dampening out solute density gradient driven convective flows. However, large Earth-grown crystals have so far tended to be more two dimensional. Preliminary X-ray diffraction analysis of lysozyme crystals grown in McDUCK have indicated that the best, and largest, come from the middle chambers, suggesting that there is an optimal growth rate. Further, the improvements in diffraction resolution have been better signal to noise ratios in the low resolution data, not an increase in resolution overall. Due to the persistently large crystals

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

NASA Technical Reports Server (NTRS)

Su, Ching-Hua; Ramachandran, N.

2013-01-01

Crystals of ZnSe and related ternary compounds, such as ZnSeS and ZnSeTe, will be grown by physical vapor transport in the Material Science Research Rack (MSRR) on International Space Station (ISS). 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 on Earth. The investigation consists of extensive ground-based experimental and theoretical research efforts and concurrent flight experimentation. The objectives of the ground-based studies are (1) obtain the experimental data and conduct the analyses required to define the optimum growth parameters for the flight experiments, (2) perfect various characterization techniques to establish the standard procedure for material characterization, (3) quantitatively establish the characteristics of the crystals grown on Earth as a basis for subsequent comparative evaluations of the crystals grown in a low-gravity environment and (4) develop theoretical and analytical methods required for such evaluations. ZnSe and related ternary compounds have been grown by vapor transport technique with real time in-situ non-invasive monitoring techniques. The grown crystals have been characterized extensively by various techniques to correlate the grown crystal properties with the growth conditions.

Electrochemical growth of linear conducting crystals in microgravity

NASA Technical Reports Server (NTRS)

Cronise, Raymond J., IV

1988-01-01

Much attention has been given to the synthesis of linear conducting materials. These inorganic, organic, and polymeric materials have some very interesting electrical and optical properties, including low temperature superconductivity. Because of the anisotropic nature of these compounds, impurities and defects strongly influences the unique physical properties of such crystals. Investigations have demonstrated that electrochemical growth has provided the most reproducible and purest crystals. Space, specifically microgravity, eliminates phenomena such as buoyancy driven convection, and could permit formation of crystals many times purer than the ones grown to date. Several different linear conductors were flown on Get Away Special G-007 on board the Space Shuttle Columbia, STS 61-C, the first of a series of Project Explorer payloads. These compounds were grown by electrochemical methods, and the growth was monitored by photographs taken throughout the mission. Due to some thermal problems, no crystals of appreciable size were grown. The experimental results will be incorporated into improvements for the next 2 missions of Project Explorer. The results and conclusions of the first mission are discussed.

A comparison of point defects in Cd1-xZnxTe1-ySey crystals grown by Bridgman and traveling heater methods

NASA Astrophysics Data System (ADS)

Gul, R.; Roy, U. N.; Camarda, G. S.; Hossain, A.; Yang, G.; Vanier, P.; Lordi, V.; Varley, J.; James, R. B.

2017-03-01

In this paper, the properties of point defects in Cd1-xZnxTe1-ySey (CZTS) radiation detectors are characterized using deep-level transient spectroscopy and compared between materials grown using two different methods, the Bridgman method and the traveling heater method. The nature of the traps was analyzed in terms of their capture cross-sections and trap concentrations, as well as their effects on the measured charge-carrier trapping and de-trapping times, and then compared for the two growth techniques. The results revealed that Se addition to CdZnTe can reduce the VCd- concentration. In Travelling Heater Method (THM) and Bridgman Method (BM) grown CZTS detectors, besides a few similarities in the shallow and medium energy traps, there were major differences in the deep traps. It was observed that the excess-Te and lower growth-temperature conditions in THM-grown CZTS led to a complete compensation of VCd- and two additional traps (attributed to Tei- and TeCd++ appearing at around Ev + 0.26 eV and Ec - 0.78 eV, respectively). The 1.1-eV deep trap related to large Te secondary phases was a dominant trap in the BM-grown CZTS crystals. In addition to i-DLTS data, the effects of point defects induced due to different processing techniques on the detector's resistivity, spectral response to gammas, and μτ product were determined.

Low Temperature Photoluminescence of PVT Grown ZnSe and ZnSeTe

NASA Technical Reports Server (NTRS)

Wang, Ling Jun; Su, Ching-Hua; Lehoczky, S. L.

1999-01-01

ZnSe and ZnSeTe single crystals were grown by physical vapor transport (PVT) technique horizontally and vertically. The grown ZnSe and ZnSeTe single crystals were characterized by low temperature photoluminescence at 5 to 10 K using the 3.4 eV emission of an argon laser. The intensity of the sharp near band edge defect lines at 2.799, 2.783 eV and the intrinsic free exciton line at 2.802 eV were mapped on various crystal surfaces with different orientations to the gravitational field. The results show the effects of gravity vector orientation on the defect segregation. Comparison of the photoluminescence spectra of the ZeSe crystal before and after annealing in the Zn vapor shows that the 2.783 eV line of ZnSe crystal is related to the zinc vacancy. The photoluminescence spectra of the ternary ZnSeTe crystal were characterized by a single broad band from 2.2 to 2.4 eV, with a Full Width at Half Maximum (FWHM) of about 100 meV. The temperature dependence of the peak position and intensity were determined from 7 to 150 K.

Investigating the Effect of Impurities on Macromolecule Crystal Growth in Microgravity

NASA Technical Reports Server (NTRS)

Snell, Edward H.; Judge, Russell A.; Crawford, Lisa; Forsythe, Elizabeth L.; Pusey, Marc L.; Sportiello, Michael; Todd, Paul; Bellamy, Henry; Lovelace, Jeff; Cassanto, John M.;

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 of NBT-BT single crystals by flux method and their structural, morphological and electrical characterizations

NASA Astrophysics Data System (ADS)

Kanuru, Sreenadha Rao; Baskar, K.; Dhanasekaran, R.; Kumar, Binay

2016-05-01

In this paper, one of the important, eco-friendly polycrystalline material, (1-x)(Na0.5Bi0.5)TiO3 (NBT) - xBaTiO3 (BT) of different compositions (x=0.07, 0.06 and 0.05 wt%) around the morphotropic phase boundary (MPB) were synthesized by solid state reaction technique. And the single crystals with 13×7×7 mm3, 12×12×7 mm3 and 10×7×4 mm3 dimensions were grown by self flux method. The morphology, crystal structure and unit-cell parameters have been studied and the monoclinic phase has been identified for 0.07 wt% of BT. Higher BT concentration changes the crystal habit and the mechanism has been studied clearly. Raman spectroscopy at room-temperature confirms the presence of functional groups. The quality of the as grown single crystals was examined by high resolution x-ray diffraction analysis. The dielectric properties of the as grown crystals were investigated in the frequency range of 20 Hz-2 MHz from room temperature to 450 °C. The broad dielectric peak and frequency dispersion demonstrates the relaxor behavior of grown crystals. The dielectric constant (εr), transition temperature (Tm), and depolarization temperature (Td) of the grown crystals are found to be comparatively good. The diffusive factor (γ) from Curie-Weiss law confirms the as grown NBT-BT single crystals are relaxor in nature.

Group III-nitride thin films grown using MBE and bismuth

DOEpatents

Kisielowski, Christian K.; Rubin, Michael

2002-01-01

The present invention comprises growing gallium nitride films in the presence of bismuth using MBE at temperatures of about 1000 K or less. The present invention further comprises the gallium nitride films fabricated using the inventive fabrication method. The inventive films may be doped with magnesium or other dopants. The gallium nitride films were grown on sapphire substrates using a hollow anode Constricted Glow Discharge nitrogen plasma source. When bismuth was used as a surfactant, two-dimensional gallium nitride crystal sizes ranging between 10 .mu.m and 20 .mu.m were observed. This is 20 to 40 times larger than crystal sizes observed when GaN films were grown under similar circumstances but without bismuth. It is thought that the observed increase in crystal size is due bismuth inducing an increased surface diffusion coefficient for gallium. The calculated value of 4.7.times.10.sup.-7 cm.sup.2 /sec. reveals a virtual substrate temperature of 1258 K which is 260 degrees higher than the actual one.

Group III-nitride thin films grown using MBE and bismuth

DOEpatents

Kisielowski, Christian K.; Rubin, Michael

2000-01-01

The present invention comprises growing gallium nitride films in the presence of bismuth using MBE at temperatures of about 1000 K or less. The present invention further comprises the gallium nitride films fabricated using the inventive fabrication method. The inventive films may be doped with magnesium or other dopants. The gallium nitride films were grown on sapphire substrates using a hollow anode Constricted Glow Discharge nitrogen plasma source. When bismuth was used as a surfactant, two-dimensional gallium nitride crystal sizes ranging between 10 .mu.m and 20 .mu.m were observed. This is 20 to 40 times larger than crystal sizes observed when GaN films were grown under similar circumstances but without bismuth. It is thought that the observed increase in crystal size is due bismuth inducing an increased surface diffusion coefficient for gallium. The calculated value of 4.7.times.10.sup.-7 cm.sup.2 /sec. reveals a virtual substrate temperature of 1258 K which is 260 degrees higher than the actual one.

Three-dimensional crystals of ribosomes and their subunits from eu- and archaebacteria.

PubMed

Glotz, C; Müssig, J; Gewitz, H S; Makowski, I; Arad, T; Yonath, A; Wittmann, H G

1987-11-01

Ordered three-dimensional crystals of 70S ribosomes as well as of 30S and 50S ribosomal subunits from various bacteria (E. coli, Bacillus stearothermophilus, Thermus thermophilus and Halobacterium marismortui) have been grown by vapour diffusion in hanging drops using mono- and polyalcohols. A new compact crystal form of 50S subunits has been obtained, and it is suitable for crystallographic studies at medium resolution. In addition, from one crystal form large crystals could be grown in X-ray capillaries. In all cases the crystals were obtained from functionally active ribosomal particles, and the particles from dissolved crystals retained their integrity and biological activity.

Sequence-specific 1H-NMR assignments for the aromatic region of several biologically active, monomeric insulins including native human insulin.

PubMed

Roy, M; Lee, R W; Kaarsholm, N C; Thøgersen, H; Brange, J; Dunn, M F

1990-06-12

The aromatic region of the 1H-FT-NMR spectrum of the biologically fully-potent, monomeric human insulin mutant, B9 Ser----Asp, B27 Thr----Glu has been investigated in D2O. At 1 to 5 mM concentrations, this mutant insulin is monomeric above pH 7.5. Coupling and amino acid classification of all aromatic signals is established via a combination of homonuclear one- and two-dimensional methods, including COSY, multiple quantum filters, selective spin decoupling and pH titrations. By comparisons with other insulin mutants and with chemically modified native insulins, all resonances in the aromatic region are given sequence-specific assignments without any reliance on the various crystal structures reported for insulin. These comparisons also give the sequence-specific assignments of most of the aromatic resonances of the mutant insulins B16 Tyr----Glu, B27 Thr----Glu and B25 Phe----Asp and the chemically modified species des-(B23-B30) insulin and monoiodo-Tyr A14 insulin. Chemical dispersion of the assigned resonances, ring current perturbations and comparisons at high pH have made possible the assignment of the aromatic resonances of human insulin, and these studies indicate that the major structural features of the human insulin monomer (including those critical to biological function) are also present in the monomeric mutant.

Flight Experiments of Physical Vapor Transport of ZnSe: Growth of Crystals in Various Convective Conditions

NASA Technical Reports Server (NTRS)

Su, Ching-Hua

2015-01-01

A low gravity material experiment will be performed in the Material Science Research Rack (MSRR) on International Space Station (ISS). The flight experiment will conduct crystal growths of ZnSe and related ternary compounds, such as ZnSeS and ZnSeTe, by physical vapor transport (PVT). The main objective of the project is to determine the relative contributions of gravity-driven fluid flows to the compositional distribution, incorporation of impurities and defects, and deviation from stoichiometry observed in the grown crystals as results of buoyancy-driven convection and growth interface fluctuations caused by irregular fluid-flows on Earth. The investigation consists of extensive ground-based experimental and theoretical research efforts and concurrent flight experimentation. The objectives of the ground-based studies are (1) obtain the experimental data and conduct the analyses required to define the optimum growth parameters for the flight experiments, (2) perfect various characterization techniques to establish the standard procedure for material characterization, (3) quantitatively establish the characteristics of the crystals grown on Earth as a basis for subsequent comparative evaluations of the crystals grown in a low-gravity environment and (4) develop theoretical and analytical methods required for such evaluations. ZnSe and related ternary compounds have been grown by vapor transport technique with real time in-situ non-invasive monitoring techniques. The grown crystals have been characterized extensively by various techniques to correlate the grown crystal properties with the growth conditions. This talk will focus on the ground-based studies on the PVT crystal growth of ZnSe and related ternary compounds, especially the effects of different growth orientations related to gravity direction on the grown crystals.

3D Micro-topography of Transferred Laboratory and Natural Ice Crystal Surfaces Imaged by Cryo and Environmental Scanning Electron Microscopy

NASA Astrophysics Data System (ADS)

Magee, N. B.; Boaggio, K.; Bancroft, L.; Bandamede, M.

2015-12-01

Recent work has highlighted micro-scale roughness on the surfaces of ice crystals grown and imaged in-situ within the chambers of environmental scanning electron microscopes (ESEM). These observations appear to align with theoretical and satellite observations that suggest a prevalence of rough ice in cirrus clouds. However, the atmospheric application of the lab observations are indeterminate because the observations have been based only on crystals grown on substrates and in pure-water vapor environments. In this work, we present details and results from the development of a transfer technique which allows natural and lab-grown ice and snow crystals to be captured, preserved, and transferred into the ESEM for 3D imaging. Ice crystals were gathered from 1) natural snow, 2) a balloon-borne cirrus particle capture device, and 3) lab-grown ice crystals from a diffusion chamber. Ice crystals were captured in a pre-conditioned small-volume (~1 cm3) cryo-containment cell. The cell was then sealed closed and transferred to a specially-designed cryogenic dewer (filled with liquid nitrogen or crushed dry ice) for transport to a new Hitachi Field Emission, Variable Pressure SEM (SU-5000). The cryo-cell was then removed from the dewer and quickly placed onto the pre-conditioned cryo transfer stage attached to the ESEM (Quorum 3010T). Quantitative 3D topographical digital elevation models of ice surfaces are reported from SEM for the first time, including a variety of objective measures of statistical surface roughness. The surfaces of the transported crystals clearly exhibit signatures of mesoscopic roughening that are similar to examples of roughness seen in ESEM-grown crystals. For most transported crystals, the habits and crystal edges are more intricate that those observed for ice grown directly on substrates within the ESEM chamber. Portions of some crystals do appear smooth even at magnification greater than 1000x, a rare observation in our ESEM-grown crystals. The

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

PubMed

Nirmala, L Ruby; Thomas Joseph Prakash, J

2013-06-01

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

Growth of high quality bulk size single crystals of inverted solubility lithium sulphate monohydrate

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

Silambarasan, A.; Rajesh, P., E-mail: rajeshp@ssn.edu.in; Ramasamy, P.

2015-06-24

The paper summarizes the processes of growing large lithium sulfate monohydrate (LSMH) single crystals. We have established a procedure to grow high quality bulk size single crystals of inverted solubility LSMH by a newly developed unidirectional crystallization technique called the Sankeranarayenan - Ramasamy (SR) method. The convective flow of crystal growth processes from solution and the conditions of growing crystals of various aspects were discussed. Good quality LSMH single crystal is grown of the size 20 mmX80 mm without cracks, localized-defects and inclusions. The as-grown crystals are suitable for piezoelectric and nonlinear optical applications.

Bulk growth of <001> organic nonlinear optical (NLO) L-arginine 4-nitrophenolate 4-nitrophenol dihydrate (LAPP) single crystals by SR method

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

Pandian, Muthu Senthil, E-mail: senthilpandianm@ssn.edu.in; Sivasubramani, V.; Ramasamy, P.

2015-06-24

A transparent uniaxial L-arginine 4-nitrophenolate 4-nitrophenol dehydrate (LAPP) single crystal having dimension of 20 mm diameter and 45 mm length was grown by Sankaranarayanan-Ramasamy (SR) method with a growth rate of 1 mm per day. Using an identical solution the conventional crystal grown to a dimension of 8×5×5 mm{sup 3} was obtained over a period of 30 days. The crystal structure has been confirmed by single crystal X-ray diffraction measurement. The crystalline perfection of LAPP crystals grown by slow evaporation solution technique (SEST) and SR method were characterized using Vickers microhardness, UV-Vis NIR, chemical etching, dark and photo current measurements. The above study indicatesmore » that the crystal quality of the Sankaranarayanan-Ramasamy (SR) method grown LAPP is good compared to the conventional method grown crystal.« less

Studies on 2-amino-5-nitropyridinium nitrate (2A5NPN): A semi-organic third order nonlinear optical single crystal

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

Sivasubramani, V.; Pandian, Muthu Senthil, E-mail: senthilpandianm@ssn.edu.in; Ramasamy, P.

2016-05-23

2-amino-5-nitropyridinium nitrate (2A5NPN) is a semi-organic nonlinear optical crystal and optically good quality 2A5NPN single crystals were successfully grown by slow evaporation solution growth technique (SEST) at ambient temperature. The crystallographic structure of the grown crystal was determined by single crystal X-Ray diffraction analysis and it belongs to Monoclinic crystal system with centro symmetric crystalline nature. The crystallinity of the grown crystal was confirmed by powder X-ray diffraction analysis. The other physical properties of grown crystals are also characterized using TG-DTA, UV-Visible NIR, chemical etching, photoconductivity and Z-scan measurements. The Z-scan method reveals that the 2A5NPN crystal possesses multi photonmore » absorption behaviour and the significantly higher third order susceptibility and it is a promising potential NLO material.« less

Synthesis, growth and characterization of L-Phenylalaninium methanesulfonate nonlinear optical single crystal

NASA Astrophysics Data System (ADS)

Mangaiyarkarasi, K.; Ravichandran, A. T.; Anitha, K.; Manivel, A.

2018-03-01

The titled compound, L-Phenylalaninium methanesulfonate (LPA-MS) was synthesized and grown into single crystals by slow solvent evaporation solution growth technique in aqueous solution containing equimolar concentrations of L-phenylalanine and methanesulfonic acid at room temperature. The grown crystals were subjected to single crystal X-ray diffraction studies. It crystallizes in the monoclinic crystal structure with P21 space group and the unit cell parameters are a = 5.312 (10) Å, b = 8.883 (2) Å and c = 25.830 (7) Å. The functional groups of the LPA-MS crystal were confirmed with FT-IR and FT-Raman analysis. The carbon-hydrogen skeleton was confirmed with 1H NMR and 13C NMR analysis. TG-DTG and DSC studies were carried out to determine the thermal stability of the crystals. The optical transparency ranges were studied through UV-vis-spectroscopy and the crystal was found to be transparent in the visible region. The second Harmonic generation (SHG) efficiency of the grown LPA-MS crystal was measured by the Kurtz-Perry powder technique. The dipolar nature of the L-phenylalaninium methanesulfonate and the presence of the intermolecular hydrogen bonding between the molecules are the vital factors responsible for the existence of SHG activity in the crystal.

Thaumatin crystallization aboard the International Space Station using liquid-liquid diffusion in the Enhanced Gaseous Nitrogen Dewar (EGN).

PubMed

Barnes, Cindy L; Snell, Edward H; Kundrot, Craig E

2002-05-01

This paper reports results from the first biological crystal-growth experiment on the International Space Station (ISS). Crystals of thaumatin were grown using liquid-liquid diffusion in Tygon tubing transported in the Enhanced Gaseous Nitrogen Dewar (EGN). Different volume ratios and concentrations of protein and precipitant were used to test different adaptations of the vapor-diffusion crystallization recipe to the liquid-liquid diffusion method. The EGN warmed up from 77 to 273 K in about 4 d, about the same time it took to warm from 273 to 293 K. The temperature within the EGN was 293-297 K for the majority of the experiment. Air gaps that blocked liquid-liquid diffusion formed in the tubes. Nonetheless, crystals were grown. Synchrotron diffraction data collected from the best space-grown crystal extended to 1.28 A, comparable to previous studies of space-grown thaumatin crystals. The resolution of the best ground-control crystal was only 1.47 A. It is not clear if the difference in diffraction limit arises from factors other than crystal size. Improvements in temperature control and the elimination of air gaps are needed, but the results show that the EGN on the ISS can be used to produce space-grown crystals that diffract to high resolution.

Thaumatin Crystallization Aboard the International Space Station Using Liquid-Liquid Diffusion in the Enhanced Gaseous Nitrogen Dewar (EGN)

NASA Technical Reports Server (NTRS)

Kundrot, Craig; Barnes, Cindy L.; Snell, Edward H.; Stinson, Thomas N. (Technical Monitor)

2002-01-01

This paper reports results from the first biological crystal growth experiment on the International Space Station (ISS). Crystals of thaumatin were grown using liquid-liquid diffusion in Tygon tubing transported in the Enhanced Gaseous Nitrogen Dewar (EGN). Different Volume ratios and concentrations of protein and precipitant were used to test different adaptations of the vapor diffusion crystallization recipe to the liquid-liquid diffusion method. The EGN warmed up from -196 C to 0 C in about four days, about the same time it took to warm from 0 C to 20 C. The temperature within the EGN was 20 - 24 C for the majority of the experiment. Air gaps that blocked liquid-liquid diffusion formed in the tubes. Nonetheless, crystals were grown. Synchrotron diffraction data collected from the best space grown crystal extended to 1.28 Angstroms, comparable to previous studies of space-grown thaumatin crystals. The resolution of the best ground control crystal was only 1.47 Angstroms. It is not clear if the difference in diffraction limit is due to factors other than crystal size. Improvements in temperature control and the elimination of air gaps are needed, but the results show that EGN on the ISS can be used to produce space grown crystals that diffract to high resolution.

Characterizing the effect of growth conditions and crystal habit on the distribution of imperfections amongst populations of crystals

NASA Astrophysics Data System (ADS)

Price, C. J.

1993-03-01

The distribution of gross imperfections amongst populations of copper sulphate pentahydrate crystals grown under different conditions of purity and temperature are examined. The frequency of imperfection increases with decreasing crystal size. The nature of the imperfections vary with growth temperature and impurities present.

A Review of the Security of Insulin Pump Infusion Systems

PubMed Central

Paul, Nathanael; Kohno, Tadayoshi; Klonoff, David C

2011-01-01

Insulin therapy has enabled patients with diabetes to maintain blood glucose control to lead healthier lives. Today, rather than injecting insulin manually using syringes, a patient can use a device such as an insulin pump to deliver insulin programmatically. This allows for more granular insulin delivery while attaining blood glucose control. Insulin pump system features have increasingly benefited patients, but the complexity of the resulting system has grown in parallel. As a result, security breaches that can negatively affect patient health are now possible. Rather than focus on the security of a single device, we concentrate on protecting the security of the entire system. In this article, we describe the security issues as they pertain to an insulin pump system that includes an embedded system of components, which include the insulin pump, continuous glucose management system, blood glucose monitor, and other associated devices (e.g., a mobile phone or personal computer). We detail not only the growing wireless communication threat in each system component, but also describe additional threats to the system (e.g., availability and integrity). Our goal is to help create a trustworthy infusion pump system that will ultimately strengthen pump safety, and we describe mitigating solutions to address identified security issues. PMID:22226278

A review of the security of insulin pump infusion systems.

PubMed

Paul, Nathanael; Kohno, Tadayoshi; Klonoff, David C

2011-11-01

Insulin therapy has enabled patients with diabetes to maintain blood glucose control to lead healthier lives. Today, rather than injecting insulin manually using syringes, a patient can use a device such as an insulin pump to deliver insulin programmatically. This allows for more granular insulin delivery while attaining blood glucose control. Insulin pump system features have increasingly benefited patients, but the complexity of the resulting system has grown in parallel. As a result, security breaches that can negatively affect patient health are now possible. Rather than focus on the security of a single device, we concentrate on protecting the security of the entire system. In this article, we describe the security issues as they pertain to an insulin pump system that includes an embedded system of components, which include the insulin pump, continuous glucose management system, blood glucose monitor, and other associated devices (e.g., a mobile phone or personal computer). We detail not only the growing wireless communication threat in each system component, but also describe additional threats to the system (e.g., availability and integrity). Our goal is to help create a trustworthy infusion pump system that will ultimately strengthen pump safety, and we describe mitigating solutions to address identified security issues. © 2011 Diabetes Technology Society.

Synthesis, growth and characterization of a nonlinear optical crystal: Bis l-proline hydrogen nitrate.

PubMed

Selvaraju, K; Kirubavathi, K

2013-11-01

The single crystals of bis l-proline hydrogen nitrate (BLPHN) belonging to non-centrosymmetric space group were successfully grown by the slow evaporation solution growth technique. The BLPHN crystals of size 10×7×3mm(3) were obtained in 35days. Initially, the solubility tests were carried out for two solvents such as deionized water and mixed of deionized water-acetone. Among the two solvents, the solubility of BLPHN was found to be the highest in deionized water, so crystallization of BLPHN was done from its aqueous solution. As grown, crystals were characterized by single crystal X-ray diffraction studies and optical transmission spectral studies. Infrared spectroscopy, thermo gravimetric analysis and differential thermal analysis measurements were performed to study the molecular vibration and thermal behavior of the grown BLPHN crystals. Nonlinear optical (NLO) behavior of BLPHN crystal was studied by Kurtz and Perry powder method. Copyright © 2013 Elsevier B.V. All rights reserved.

Growth of NH4Cl Single Crystal from Vapor Phase in Vertical Furnace

NASA Astrophysics Data System (ADS)

Nigara, Yutaka; Yoshizawa, Masahito; Fujimura, Tadao

1983-02-01

A pure and internally stress-free single crystal of NH4Cl was grown successfully from the vapor phase. The crystal measured 1.6 cmφ× 2 cm and had the disordered CsCl structure, which was stable below 184°C. The crystal was grown in an ampoule in a vertical furnace, in which the vapor was efficiently transported both by diffusion and convection. In line with the growth mechanism of a single crystal, the temperature fluctuation (°C/min) on the growth interface was kept smaller than the product of the temperature gradient (°C/cm) and the growth rate (cm/min). The specific heat of the crystal was measured around -31°C (242 K) during cooling and heating cycles by AC calorimetry. The thermal hysteresis (0.4 K) obtained here was smaller than that (0.89 K) of an NH4Cl crystal grown from its aqueous solution with urea added as a habit modifier.

Insulin microcrystal suspension as a long-acting formulation for pulmonary delivery.

PubMed

Kwon, Jai-Hyun; Lee, Byung-Ha; Lee, Jae-Jeong; Kim, Chan-Wha

2004-06-01

Pulmonary delivery provides the most promising non-parenteral route of insulin administration. Insulin was used as a model protein to demonstrate the feasibility of using protein crystals for the pulmonary delivery of a sustained-release protein drug formulation. Insulin microcrystals with a mean diameter of 3 microm were prepared using a seed zone method. The yield of crystallization was very high (95.8 +/- 0.97%), and the microcrystals were recovered with high efficiency (>98%) by centrifugation. Morphological examination using scanning electron microphotography showed the microcrystals to be of a homogeneous rhombohedral shape, with some rhombus forms, without aggregates. After the administration of 32 U/kg of the microcrystal suspension to STZ-induced diabetic SD rats by intratracheal instillation, the blood glucose levels were reduced and hypoglycemia was prolonged over 13 h, as compared to the insulin solution. The percent minimum reductions of the blood glucose concentration (% MRBG) produced by the microcrystal suspension and insulin solution reached 36.5 and 37.2%, respectively, of the initial level, and the percent total reductions in blood glucose (% TRBG(13 h)) were 34.4 and 25.0%, respectively. In the case of inhalation using a sieve-type ultrasonic nebulizer, the % MRBG produced by the microcrystal suspension and insulin solution were 21.7 and 26.3%, respectively, of the initial level, and the % TRBG(13 h) were 66.7 and 58.4%, respectively. However, the hypoglycemic effects of the microcrystal suspension were prolonged over 7 h, which compares favorably with the insulin solution (P<0.5 by unpaired t-test). These results could be attributed to the sustained-release of insulin from the microcrystals, which were deposited widely throughout the entire lung.

Optical and dielectric studies of KH2PO4 crystal influenced by organic ligand of citric acid and L-valine: A single crystal growth and comparative study

NASA Astrophysics Data System (ADS)

Anis, Mohd; Hakeem, D. A.; Muley, G. G.

In the present study pure, citric acid (CA) and L-valine (LV) doped potassium dihydrogen phosphate (KDP) crystals have been grown with the aim to investigate the nonlinear optical applications facilitated by UV-visible, third order nonlinear optical (TONLO) and dielectric properties. The structural parameters of grown crystals have been confirmed by single crystal X-ray diffraction analysis. The enhancement in optical transparency of KDP crystal due to addition of CA and LV has been examined within 200-900 nm by means of UV-visible spectral analysis. In addition, the transmittance data have been used to evaluate the effect of dopants on reflectance, refractive index and extinction coefficient of grown crystals in the visible region. The Z-scan analysis has been performed at 632.8 nm to identify the nature of photoinduced nonlinear refraction and nonlinear absorption in doped KDP crystals. The influence of π-bonded ligand of dopant CA and LV on TONLO susceptibility (χ3), refractive index (n2) and absorption coefficient (β) of KDP crystals has been evaluated to discuss laser assisted device applications. The decrease in dielectric constant and dielectric loss of KDP crystal due to addition of CA and LV has been explored using the temperature dependent dielectric studies.

Structural, thermal and optical properties of a semiorganic nonlinear optical single crystal: glycine zinc sulphate.

PubMed

Balakrishnan, T; Ramamurthi, K

2007-10-01

Glycine zinc sulphate salt was synthesized and the solubility and metastable zonewidth were estimated from the aqueous solution. Single crystals of glycine zinc sulphate were grown by solvent evaporation method from aqueous solution. Grown crystals were characterized by X-ray diffraction and FT-IR spectral analyses. The range and percentage of optical transmission was ascertained by recording UV-vis-NIR spectrum. Thermal properties of the crystal were investigated by thermogravimetric analysis. Microhardness study was carried out on (01-1) face of the grown crystal. Its powder second harmonic generation efficiency was measured using Nd:YAG laser and the value was observed to be 0.7 times that of potassium dihydrogen orthophosphate.

Protein crystal growth aboard the U.S. Space Shuttle flights STS-31 and STS-32

NASA Technical Reports Server (NTRS)

Delucas, Lawrence J.; Smith, Craig D.; Carter, Daniel C.; Twigg, Pam; He, Xiao-Min; Snyder, Robert S.; Weber, Patricia C.; Schloss, J. V.; Einspahr, H. M.; Clancy, L. L.

1992-01-01

Results obtained from the Shuttle flight STS-32 flown in January 1990, and preliminary results from the most recent Shuttle flight, STS-31, flown in April 1990, are presented. Crystals grown in microgravity environment include Canavalin, isocitrate lyase, human serum albumin, and Anti-HPr Fab. It is concluded that about 20 percent of proteins flown exhibit better morphologies or better quality data than their earth-grown counterparts. About 40 percent do not yield crystals at all and the remaining 40 percent yield crystals that are either too small for X-ray analysis or produce data of poorer quality than the best earth-grown crystals.

Growth and dielectric, mechanical, thermal and etching studies of an organic nonlinear optical L-arginine trifluoroacetate (LATF) single crystal

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

Arjunan, S.; Department of Physics, Presidency College, Chennai 600005; Mohan Kumar, R.

2008-08-04

L-arginine trifluoroacetate, an organic nonlinear optical material, has been synthesized from aqueous solution. Bulk single crystal of dimension 57 mm x 5 mm x 3 mm has been grown by temperature lowering technique. Powder X-ray diffraction studies confirmed the monoclinic structure of the grown L-arginine trifluoroacetate crystal. Linear optical property of the grown crystal has been studied by UV-vis spectrum. Dielectric response of the L-arginine trifluoroacetate crystal was analysed for different frequencies and temperatures in detail. Microhardness study on the sample reveals that the crystal possesses relatively higher hardness compared to many organic crystals. Thermal analyses confirmed that the L-argininemore » trifluoroacetate material is thermally stable upto 212 deg. C. The etching studies have been performed to assess the perfection of the L-arginine trifluoroacetate crystal. Kurtz powder second harmonic generation test confirms the nonlinear optical properties of the as-grown L-arginine trifluoroacetate crystal.« 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

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

NASA Technical Reports Server (NTRS)

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

2003-01-01

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

Growth, nonlinear optical, thermal, dielectric and laser damage threshold studies of semiorganic crystal: monohydrate piperazine hydrogen phosphate.

PubMed

Krishnan, P; Gayathri, K; Bhagavannarayana, G; Gunasekaran, S; Anbalagan, G

2013-02-01

Monohydrate piperazine hydrogen phosphate (MPHP), a semi organic nonlinear optical material has been synthesized and single crystals were grown from aqueous solution by slow evaporation technique. Single crystal X-ray diffraction study on grown crystal reveals that they belong to monoclinic crystal system with space group P2(1)/c; (a=6.39Å; b=12.22Å; c=11.16Å; β=97.14°; V=864Å(3)). The structural perfection of the grown crystal was analyzed by high-resolution X-ray diffraction (HRXRD) rocking curve measurements. FTIR spectrum confirms the presence of the functional groups in synthesized material. UV-Vis spectrum indicates that the crystal is transparent in the entire visible region with a lower cut off wavelength of 387 nm. The variation of dielectric properties of the grown crystal with respect to frequency has been investigated at different temperatures. Thermal analysis carried out on the MPHP crystal shows that the crystal is stable up to 135°C. Relative powder second harmonic generation efficiency tested by Kurtz-Perry powder technique, which was about 0.638 times that of Potassium dihydrogen phosphate. Copyright © 2012 Elsevier B.V. All rights reserved.

Growth and characterization of pure and glycine doped cadmium thiourea sulphate (GCTS) crystals

NASA Astrophysics Data System (ADS)

Lawrence, M.; Thomas Joseph Prakash, J.

2012-06-01

The pure and glycine doped cadmium thiourea sulphate (GCTS) single crystals were grown successfully by slow evaporation method at room temperature. The concentration of dopant in the mother solution was 1 mol%. There is a change in unit cell. The Fourier transform infrared spectroscopy study confirms the incorporation of glycine into CTS crystal. The doped crystals are optically better and more transparent than the pure ones. The dopant increases the hardness value of the material. The grown crystals were also subjected to thermal and NLO studies.

Lysozyme Crystal

NASA Technical Reports Server (NTRS)

2004-01-01

To the crystallographer, this may not be a diamond but it is just as priceless. A Lysozyme crystal grown in orbit looks great under a microscope, but the real test is X-ray crystallography. The colors are caused by polarizing filters. Proteins can form crystals generated by rows and columns of molecules that form up like soldiers on a parade ground. Shining X-rays through a crystal will produce a pattern of dots that can be decoded to reveal the arrangement of the atoms in the molecules making up the crystal. Like the troops in formation, uniformity and order are everything in X-ray crystallography. X-rays have much shorter wavelengths than visible light, so the best looking crystals under the microscope won't necessarily pass muster under the X-rays. In order to have crystals to use for X-ray diffraction studies, crystals need to be fairly large and well ordered. Scientists also need lots of crystals since exposure to air, the process of X-raying them, and other factors destroy them. Growing protein crystals in space has yielded striking results. Lysozyme's structure is well known and it has become a standard in many crystallization studies on Earth and in space.

Growth and characterization of KDP crystals doped with L-aspartic acid.

PubMed

Krishnamurthy, R; Rajasekaran, R; Samuel, Bincy Susan

2013-03-01

Potassium Dihydrogen Phosphate (KDP) doped with L-aspartic acid has been grown by solvent slow evaporation technique from a mixture of aqueous solution of KDP and 0.7% of L-aspartic acid at room temperature. The grown crystals were characterized by powder X-ray diffraction, UV-visible, FTIR analysis. The doping of aspartic acid was confirmed by FTIR spectrum. The Nonlinear optical property (SHG) of L-aspartic acid doped KDP has been confirmed. Microhardness studies were carried out on the grown crystal. Copyright © 2012 Elsevier B.V. All rights reserved.

Powder XRD and dielectric studies of gel grown calcium pyrophosphate crystals

NASA Astrophysics Data System (ADS)

Parekh, Bharat; Parikh, Ketan; Joshi, Mihir

2013-06-01

Formation of calcium pyrophosphate dihydrate (CPPD) crystals in soft tissues such as cartilage, meniscus and synovial tissue leads to CPPD deposition diseases. The appearance of these crystals in the synovial fluid can give rise to an acute arthritic attack with pain and inflammation of the joints, a condition called pseudo-gout. The growth of CPP crystals has been carried out, in the present study, using the single diffusion gel growth technique, which can broadly mimic in vitro the condition in soft tissues. The crystals were characterized by different techniques. The FTIR study revealed the presence of various functional groups. Powder XRD study was also carried out to verify the crystal structure. The dielectric study was carried out at room temperature by applying field of different frequency from 500 Hz to 1 MHz. The dielectric constant, dielectric loss and a.c. resistivity decreased as frequency increased, whereas the a.c. conductivity increased as frequency increased.

Crystallization of Chicken Egg White Lysozyme from Assorted Sulfate Salts

NASA Technical Reports Server (NTRS)

Forsythe, Elizabeth L.; Snell, Edward H.; Malone, Christine C.; Pusey, Marc L.

1999-01-01

Chicken egg white lysozyme has been found to crystallize from ammonium, sodium, potassium, rubidium, magnesium, and manganese sulfates at acidic and basic pH, with protein concentrations from 60 to 190 mg/ml. Crystals have also been grown at 4 C in the absence of any other added salts using isoionic lysozyme which was titrated to pH 4.6 with dilute sulfuric acid. Four different crystal forms have been obtained, depending upon the temperature, protein concentration, and precipitating salt employed. Crystals grown at 15 C were generally tetragonal, with space group P4(sub 3)2(sub 1)2. Crystallization at 20 C typically resulted in the formation of orthorhombic crystals, space group P2(sub 1)2(sub 1)2(sub 1). The tetragonal reversible reaction orthorhombic transition appeared to be a function of both the temperature and protein concentration, occurring between 15 and 20 C and between 100 and 125 mg/ml protein concentration. Crystallization from 1.2 M magnesium sulfate at pH 7.8 gave a trigonal crystal, space group P3(sub 1)2(sub 1), a = b = 87.4, c = 73.7, gamma = 120 deg, which diffracted to 2.8 A. Crystallization from ammonium sulfate at pH 4.6, generally at lower temperatures, was also found to result in a monoclinic form. space group C2, a = 65.6, b = 95.0, c = 41.2, beta = 119.2 deg. A crystal of approximately 0.2 x 0.2 x 0.5 mm grown from bulk solution diffracted to approximately 3.5 A.

Crystallization of chicken egg white lysozyme from assorted sulfate salts

NASA Astrophysics Data System (ADS)

Forsythe, Elizabeth L.; Snell, Edward H.; Malone, Christine C.; Pusey, Marc L.

1999-01-01

Chicken egg white lysozyme has been found to crystallize from ammonium, sodium, potassium, rubidium, magnesium, and manganese sulfates at acidic and basic pH, with protein concentrations from 60 to 190 mg/ml. Crystals have also been grown at 4°C in the absence of any other added salts using isoionic lysozyme which was titrated to pH 4.6 with dilute sulfuric acid. Four different crystal forms have been obtained, depending upon the temperature, protein concentration, and precipitating salt employed. Crystals grown at 15°C were generally tetragonal, with space group P4 32 12. Crystallization at 20°C typically resulted in the formation of orthorhombic crystals, space group P2 12 12 1. The tetragonal ↔ orthorhombic transition appeared to be a function of both the temperature and protein concentration, occurring between 15 and 20°C and between 100 and 125 mg/ml protein concentration. Crystallization from 1.2 M magnesium sulfate at pH 7.8 gave a trigonal crystal, space group P3 12 1, a= b=87.4, c=73.7, γ=120°, which diffracted to 2.8 Å. Crystallization from ammonium sulfate at pH 4.6, generally at lower temperatures, was also found to result in a monoclinic form, space group C2, a=65.6, b=95.0, c=41.2, β=119.2°. A crystal of ˜0.2×0.2×0.5 mm grown from bulk solution diffracted to ˜3.5 Å.

Size-controllable nanopyramids photonic crystal selectively grown on p-GaN for enhanced light-extraction of light-emitting diodes.

PubMed

Du, Chengxiao; Wei, Tongbo; Zheng, Haiyang; Wang, Liancheng; Geng, Chong; Yan, Qingfeng; Wang, Junxi; Li, Jinmin

2013-10-21

Size-controllable p-GaN hexagonal nanopyramids (HnPs)-photonic crystal (PhC) structures were selectively grown on flat p-GaN layer for the elimination of total internal reflection of light-emitting diodes (LEDs). The LEDs with HnPs-PhC of 46.3% bottom fill factor (PhC lattice constant is 730 nm) showed an improved light output power by 99.9% at forward current of 350 mA compared to the reference LEDs with flat p-GaN layer. We confirmed the effect of HnPs-PhC with different bottom fill factors and the effect of nanopyramid-shaped and nanocolumn-shaped PhC on the light-extraction of LEDs was also investigated by using three-dimensional finite-difference time-domain simulations.

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

NASA Astrophysics Data System (ADS)

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

2002-06-01

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

Single-crystal silicon optical fiber by direct laser crystallization

DOE PAGES

Ji, Xiaoyu; Lei, Shiming; Yu, Shih -Ying; ...

2016-12-05

Semiconductor core optical fibers with a silica cladding are of great interest in nonlinear photonics and optoelectronics applications. Laser crystallization has been recently demonstrated for crystallizing amorphous silicon fibers into crystalline form. Here we explore the underlying mechanism by which long single-crystal silicon fibers, which are novel platforms for silicon photonics, can be achieved by this process. Using finite element modeling, we construct a laser processing diagram that reveals a parameter space within which single crystals can be grown. Utilizing this diagram, we illustrate the creation of single-crystal silicon core fibers by laser crystallizing amorphous silicon deposited inside silica capillarymore » fibers by high-pressure chemical vapor deposition. The single-crystal fibers, up to 5.1 mm long, have a very welldefined core/cladding interface and a chemically pure silicon core that leads to very low optical losses down to ~0.47-1dB/cm at the standard telecommunication wavelength (1550 nm). Furthermore, tt also exhibits a photosensitivity that is comparable to bulk silicon. Creating such laser processing diagrams can provide a general framework for developing single-crystal fibers in other materials of technological importance.« less

Growth, optical, luminescence, thermal and mechanical behavior of an organic single crystal: 3-Acetyl-2-methyl-4-phenylquinolin-1-ium chloride.

PubMed

Nirosha, M; Kalainathan, S; Sarveswari, S; Vijayakumar, V

2014-04-05

A single crystal of 3-acetyl-2-methyl-4-phenylquinolin-1-ium chloride has grown by slow evaporation solution growth technique using ethanol as solvent. The structural, thermal, optical and mechanical property has studied for the grown crystal. Single crystal XRD revealed that the crystal belongs to monoclinic system with space group P21/c. The presences of Functional groups in the crystallized material have confirmed using the FTIR vibrational spectrum. The optical absorbance spectrum recorded from 190 to 1100nm shows the cut-off wavelength occurs at 371nm. The material shows its transparency in the entire region of the visible spectrum. The photoluminescence spectrum shows the ultraviolet and blue emission in the crystal. Thermogravimetric and differential thermal analysis reveal the thermal stability of the grown crystal. Etching study shows the grown mechanism and surface features of the crystal. Vickers microhardness studies have carried out on the (01-1) plane to understand the mechanical properties of the grown crystal. The hardness of the title compound increases on increasing the load. The Meyer's index number (n), and the stiffness constants for different loads has calculated and reported. Copyright © 2013 Elsevier B.V. All rights reserved.

R6 Hexameric Insulin Complexed with m-Cresol or Rescorcinol

NASA Technical Reports Server (NTRS)

Smith, G. David; Ciszak, Ewa; Magrum, Lucy A.; Rose, M. Franklin (Technical Monitor)

2000-01-01

The structures of three R6 human insulin hexamers have been determined. Crystals of monoclinic m-cresol/insulin, monoclinic resorcinol/insulin, and rhombohedral m-cresol/insulin crystals diffracted to 1.9, 1.9 and 1,78 Angstroms, respectively, and have been refined to residuals of 0.195, 0.179, and 0.200, respectively. In all three structures, a phenolic derivative is found to occupy the phenolic binding site where it forms hydrogen bonds to the carbonyl oxygen of A6 Cys and the nitrogen of A11 Cys. Two additional phenolic derivative binding sites were identified within or between hexamers. The structures of all three hexamers are nearly identical although a large displacement of the N-terminus of one B-chain in both monoclinic structures results from coordination to a sodium ion which is located between symmetry related hexamers. Other minor differences in structure are a consequence of differences in packing in the monoclinic cell as compared to the rhombohedral cell. Based upon the differences in conformation of the B13 Glu side chains in T6, T3R3, and R6 hexamers, the deprotonation of these side chains appears to be associated with the T (right arrow) R conformational transition.

Influence of carbon on the thermoluminescence and optically stimulated luminescence of α-Al2O3:C crystals

NASA Astrophysics Data System (ADS)

Yang, Xin-Bo; Li, Hong-Jun; Bi, Qun-Yu; Cheng, Yan; Tang, Qiang; Xu, Jun

2008-12-01

α-Al2O3:C crystal shows excellent thermoluminescence (TL) and optically stimulated luminescence (OSL) properties but the real role carbon plays in this crystal is still not clearly understood so far. In this work, α-Al2O3:C crystal doping with different amounts of carbon were grown by the temperature gradient technique, and TL and OSL properties of as-grown crystals were investigated. Additionally, a mechanism was proposed to explain the role of carbon in forming the TL and OSL properties of α-Al2O3:C. TL and OSL intensities of as-grown crystals increase with the increasing amount of carbon doping in the crystal, but no shift is found in the glow peak location at 465 K. As the amount of carbon doping in the crystals decreases, OSL decay rate becomes faster. With the increase in heating rate, the integral TL response of as-grown crystals decreases and glow peak shifts to higher temperatures. TL response decrease rate increases with the increasing amount of carbon doping in the crystals. All the TL and OSL response curves of as-grown crystals show linear-sublinear-saturation characteristic, and OSL dose response exhibits higher sensitivity and wider linear dose range than that of TL. The crystal doping with 5000 ppm carbon shows the best dosimetric properties. Carbon plays the role of a dopant in α-Al2O3:C crystal and four-valent carbon anions replace the two-valent anions of oxygen during the crystal growth process, and large amounts of oxygen vacancies were formed, which corresponds to the high absorption coefficient of F and F+ centers in the crystals.

Crystal growth, characterization and theoretical studies of 4-aminopyridinium picrate

NASA Astrophysics Data System (ADS)

Aditya Prasad, A.; Muthu, K.; Rajasekar, M.; Meenatchi, V.; Meenakshisundaram, S. P.

2015-01-01

Single crystals of 4-aminopyridinium picrate (APP) were grown by slow evaporation of a mixed solvent system methanol-acetone (1:1, v/v) containing equimolar quantities of 4-aminopyridine and picric acid. Structure is elucidated by single crystal XRD analysis and the crystal belongs to monoclinic system with four molecules in the unit cell (space group P21/c) and the cell parameter values are, a = 8.513 Å (±0.015), b = 11.33 Å (±0.02), c = 14.33 Å (±0.03) and β = 104.15° (±0.019), V = 1340 A3 (±6) with refined R factors R1 = 0.0053 and wR2 = 0.0126. The electron density mapping is interpreted to find coordinates for each atom in the crystallized molecules. The various functional groups present in the molecule are confirmed by FT-IR analysis. UV-visible spectral analysis was used to determine the band gap energy of 4-aminopyridinium picrate. Powder X-ray diffraction pattern reveals the crystallinity of the as-grown crystal and it closely resembles the simulated XRD from the single crystal XRD analysis. Scanning electron microscopy reveals the surface morphology of the grown crystal. Optimized geometry is derived by Hartree-Fock theory calculations and the first-order molecular hyperpolarizability (β), theoretically calculated bond length, bond angles and excited state energy from theoretical UV-vis spectrum were estimated.

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

NASA Astrophysics Data System (ADS)

Sadhasivam, S.; Rajesh, N. P.

2017-12-01

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

Crystallization of Chicken Egg White Lysozyme from Assorted Sulfate Salts

NASA Technical Reports Server (NTRS)

Forsythe, Elizabeth L.; Snell, Edward H.; Malone, Christine C.; Pusey, Marc L.

1998-01-01

Chicken egg white lysozyme has been found to crystallize from ammonium, sodium, potassium, rubidium, magnesium, and manganese sulfates at acidic and basic pH, with protein concentrations from 60 to 190 mg/ml. Four different crystal morphologies have been obtained, depending upon the temperature, protein concentration, and precipitating salt employed, Crystals grown at 15 C were generally tetragonal, with space group P43212. Crystallization at 20 C typically resulted in the formation of orthorhombic crystals, space group P21212 1. The tetragonal much less than orthorhombic morphology transition appeared to be a function of both the temperature and protein concentration, occurring between 15 and 20 C and between 100 and 125 mg/ml protein concentration. Crystallization from 0.8 -1.2M magnesium sulfate at pH 7.6 - 8.0 gave a hexagonal (trigonal) crystal form, space group P3121, which diffracted to 2.8 A. Ammonium sulfate was also found to result in a monoclinic form, space group C2. Small twinned monoclinic crystals of approx. 0.2 mm on edge were grown by dialysis followed by seeded sitting drop crystallization.

Fabrication of graded index single crystal in glass

PubMed Central

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

2017-01-01

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

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

NASA Technical Reports Server (NTRS)

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

1998-01-01

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

Point defects in CdTe xSe 1-x crystals grown from a Te-rich solution for applications in detecting radiation

DOE PAGES

Gul, R.; Roy, U. N.; Bolotnikov, A. E.; ...

2015-04-15

We investigated cadmium telluride selenide (CdTeSe) crystals, newly grown by the Traveling Heater Method (THM), for the presence and abundance of point defects. Deep Level Transient spectroscopy (I-DLTS) was used to determine the energies of the traps, their capture cross sections, and densities. The bias across the detectors was varied from (1–30) V. Four types of point defects were identified, ranging from 10 meV to 0.35 eV. Two dominant traps at energies of 0.18 eV and 0.14 eV were studied in depth. Cd vacancies are found at lower concentrations than other point defects present in the material.

Influence of bis-thiourea nickel nitrate on the structural, optical, electrical, thermal and mechanical behavior of a KDP single crystal for NLO applications

NASA Astrophysics Data System (ADS)

Rasal, Y. B.; Shaikh, R. N.; Shirsat, M. D.; Kalainathan, S.; Hussaini, S. S.

2017-03-01

A single crystal of bis-thiourea nickel nitrate (BTNN) doped potassium dihydrogen phosphate (KDP) has been grown from solution at room temperature by a slow evaporation technique. The cell parameters of the grown crystals were determined using single crystal x-ray diffraction analysis. The different functional groups of the grown crystal were confirmed using Fourier transform infrared analysis. The improved optical parameters of the grown crystal have been evaluated in the range of 200-900 nm using UV-visible spectral analysis. The grown crystal was transparent in the entire visible region and the band gap value was found to be 4.96 eV. The influence of BTNN on the third order nonlinear optical properties of KDP crystal has been investigated by means of the Z-scan technique. The second harmonic generation (SHG) efficiency of grown crystal measured using a Nd-YAG laser is 1.98 times higher than that of pure KDP. The third order nonlinear optical susceptibility (χ 3) and nonlinear absorption coefficient (β) of BTNN doped KDP crystal is found to be 1.77  ×  10-5 esu and 5.57  ×  10-6 cm W-1 respectively. The laser damage threshold (LDT) energy for the grown crystal has been measured by using a Q-switched Nd:YAG laser source. The bis-thiourea nickel nitrate shows authoritative impact on the dielectric properties of doped crystal. The influence of bis-thiourea nickel nitrate on the mechanical behavior of KDP crystal has been investigated using Vickers microhardness intender. The thermal behavior of BTNN doped KDP crystal has been analyzed by TGA/DTA analysis.

Thermoelectric Behavior of PbSe Single Crystals

DOE PAGES

Kogo, Gilbert; Pradhan, Aswini K.; Roy, Utpal N.

2016-12-05

The electrical conductivity and Seebeck coefficient of PbSe single crystals grown by the Bridgman technique display metallic behavior. The Seebeck coefficient increases linearly with increasing temperature and showed positive Seebeck values, typically valid for a p-type PbSe crystal. The electronic thermal conductivity decreases with increase in temperature. The power factor increases gradually with temperature until the maximum value of 6.51 × 10 -3 W/mK2 at 260 K, other values are 5.95 × 10 -3 W/mK 2 at 300 K, and 5.40 × 10 -3 W/mK 2 at 320 K. Our results demonstrate that as-grown PbSe crystal is generically p-type duemore » to excess in Pb and can be a potential candidate for thermoelectric power generation.« less

Growth and characterization of SrI2:Eu2+ single crystal for gamma ray detector applications

NASA Astrophysics Data System (ADS)

Raja, A.; Daniel, D. Joseph; Ramasamy, P.; Singh, S. G.; Sen, S.; Gadkari, S. C.

2018-04-01

Europium activated Strontium Iodide single crystal was grown by vertical Bridgman-stockbarger technique. The melting point and freezing point of SrI2:Eu2+ crystal was analyzed by TG/DTA. The Radioluminescence emission was recorded. The scintillation measurement was carried out for the grown SrI2:Eu2+ crystal under 137Cs gamma energy source.

Investigation on the growth and characterization of 4-aminobenzophenone single crystal by the vertical dynamic gradient freeze technique

NASA Astrophysics Data System (ADS)

Prabhakaran, SP.; Ramesh Babu, R.; Sukumar, M.; Bhagavannarayana, G.; Ramamurthi, K.

2014-03-01

Growth of bulk single crystal of 4-Aminobenzophenone (4-ABP) from the vertical dynamic gradient freeze (VDGF) setup designed with eight zone furnace was investigated. The experimental parameters for the growth of 4-ABP single crystal with respect to the design of VDGF setup are discussed. The eight zones were used to generate multiple temperature gradients over the furnace, and video imaging system helped to capture the real time growth and solid-liquid interface. 4-ABP single crystal with the size of 18 mm diameter and 40 mm length was grown from this investigation. Structural and optical quality of grown crystal was examined by high resolution X-ray diffraction and UV-visible spectral analysis, respectively and the blue emission was also confirmed from the photoluminescence spectrum. Microhardness number of the crystal was estimated at different loads using Vicker's microhardness tester. The size and quality of single crystal grown from the present investigation are compared with the vertical Bridgman grown 4-ABP.

Growth of Solid Solution Crystals

NASA Technical Reports Server (NTRS)

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

1985-01-01

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

Mapping crystal defects with a digital scanning ultramicroscope

NASA Astrophysics Data System (ADS)

Springer, John M., Jr.; Silberman, Enrique; Kroes, Roger L.; Reiss, Don

1991-12-01

A computer controlled scanning ultramicroscope has been built to assist in the characterization of transparent crystals. The device measures the scattering of a focused He-Ne laser beam by crystalline defects. As an XYZ translation table moves the crystal under the ultramicroscope, the scattered light is measured by a photodetector whose output is digitized and recorded. From this data, contour maps or 3-D perspective plots of the scattering regions of the crystal can be generated to assist in finding patterns of defects which might be correlated with perturbations in the growth process. The verified resolution of the present instrument is about 1 micrometers , which is limited by the minimum step of the stepper-motor driven translation stages, optical diffraction effects, and the sensitivity of the detector at the laser light frequency. The instrument was used to build a database of defects patterns in commercial laboratory grown triglycine sulphate (TGS) crystals, and to map defects in a TGS crystal grown from aqueous solution during the flight of Spacelab 3. This crystal shows indications of a reduction both in the generation of defects at the seed-new growth interface and in their propagation into the new crystal.

Mapping crystal defects with a digital scanning ultramicroscope

NASA Astrophysics Data System (ADS)

Springer, J. M.; Silberman, E.; Kroes, Roger; Reiss, D.

A computer controlled scanning ultramicroscope has been built to assist in the characterization of transparent crystals. The device measures the scattering of a focused He-Ne laser beam by crystalline defects. As an XYZ translation table moves the crystal under the ultramicroscope, the scattered light is measured by a photodetector whose output is digitized and recorded. From this data, contour maps or three dimensional perspective plots of the scattering regions of the crystal can be generated to assist in finding patterns of defects which might be correlated with perturbations in the growth process. The verified resolution of the present instrument is about 1 micrometer, which is limited by the minimum step of the stepper-motor driven translation stages, optical diffraction effects and the sensitivity of the detector at the laser light frequency. The instrument was used to build a database of defects patterns in commercial laboratory grown triglycine sulphate (TGS) crystals, and to map defects in a TGS crystal grown from aqueous solution during the flight of Spacelab 3. This crystal shows indications of a reduction both in the generation of defects at the seed-new growth interface and in their propagation into the new crystal.

Mapping crystal defects with a digital scanning ultramicroscope

NASA Technical Reports Server (NTRS)

Springer, J. M.; Silberman, E.; Kroes, Roger; Reiss, D.

1991-01-01

A computer controlled scanning ultramicroscope has been built to assist in the characterization of transparent crystals. The device measures the scattering of a focused He-Ne laser beam by crystalline defects. As an XYZ translation table moves the crystal under the ultramicroscope, the scattered light is measured by a photodetector whose output is digitized and recorded. From this data, contour maps or three dimensional perspective plots of the scattering regions of the crystal can be generated to assist in finding patterns of defects which might be correlated with perturbations in the growth process. The verified resolution of the present instrument is about 1 micrometer, which is limited by the minimum step of the stepper-motor driven translation stages, optical diffraction effects and the sensitivity of the detector at the laser light frequency. The instrument was used to build a database of defects patterns in commercial laboratory grown triglycine sulphate (TGS) crystals, and to map defects in a TGS crystal grown from aqueous solution during the flight of Spacelab 3. This crystal shows indications of a reduction both in the generation of defects at the seed-new growth interface and in their propagation into the new crystal.

Growth, structural, spectral, optical, and thermal studies on amino acid based new NLO single crystal: L-phenylalanine-4-nitrophenol.

PubMed

Prakash, M; Lydia Caroline, M; Geetha, D

2013-05-01

A new organic nonlinear optical single crystal, L-phenylalanine-4-nitrophenol (LPAPN) belonging to the amino acid group has been successfully grown by slow evaporation technique. The lattice parameters of the grown crystal have been determined by X-ray diffraction studies. FT-IR spectrum was recorded to identify the presence of functional group and molecular structure was confirmed by NMR spectrum. Thermal strength of the grown crystal has been studied using TG-DTA analyses. The grown crystals were found to be transparent in the entire visible region. The existence of second harmonic generation signals was observed using Nd:YAG laser with fundamental wavelength of 1064 nm. Copyright © 2013 Elsevier B.V. All rights reserved.

Growth and physicochemical properties of organometallic (DL)-trithioureatartrato-O1,O2,O3-cadmium(II) single crystals

NASA Astrophysics Data System (ADS)

Sathyamoorthy, K.; Vinothkumar, P.; Irshad Ahamed, J.; Murali Manohar, P.; Priya, M.; Liu, Jinghe

2018-04-01

Single crystals of organometallic (DL)-trithioureatartrato-O1,O2,O3-cadmium(II) (TUDLC) have been grown from methanol solution by using the slow evaporation of solvent growth technique. The lattice structure and crystalline perfection have been determined by carrying out single crystal X-ray diffraction and high resolution X-ray diffraction measurements. The grown crystal was characterized thermally and mechanically by carrying out thermo-gravimetric and micro hardness measurements. The linear and nonlinear optical characterizations were made by carrying out optical transmittance, surface laser damage threshold, particle size-dependent second harmonic generation (SHG) efficiency and photo conductivity measurements. The grown crystal was electrically characterized by carrying out frequency-dependent dielectric measurements. Chemical etching study was also carried out and the dislocation density was estimated. Results obtained in the present study indicate that the grown TUDLC crystal is optically transparent with lower cut-off wavelength 304 nm, mechanically soft, thermally stable up to 101 °C and NLO active with SHG efficiency 2.13 (in KDP unit). The grown crystal is found to have considerably large size, good crystalline perfection, large specific heat capacity, higher surface laser damage threshold and negative photoconductivity.

Growth, structural, optical, piezoelectric and etching analysis of L-lysine p-nitrophenolate monohydrate single crystals

NASA Astrophysics Data System (ADS)

Alexandar, A.; Lakshmanan, A.; Sakthy Priya, S.; Surendran, P.; Rameshkumar, P.

2017-09-01

Nonlinear optical single crystals of L-lysine p-nitrophenolate monohydrate (LLPNP) were grown in aqueous solution by the slow evaporation solution technique (SEST). The grown crystals were subjected to powder X-ray diffraction analysis, (PXRD) and it was found that the title compound was crystallized in the orthorhombic crystal system with noncentrosymmetric space group of P212121. The vibrational frequencies of various functional groups present in the crystal were analyzed using the FTIR spectrum with a wavenumber range between 450 cm-1 and 4000 cm-1. The microhardness analysis of the sample revealed that the crystal belongs to the soft material category. Piezoelectric analysis was performed to measure the value of the piezoelectric (d33) coefficient. Blue light emission of the material was confirmed using the photoluminescence spectrum. Thermal stability of the grown crystal was analyzed using a melting point apparatus and it was found that the LLPNP is stable upto 175∘C. Etching analysis was performed at various durations, in order to identify the surface properties of the LLPNP crystal.

Point Defect Distributions in ZnSe Crystals: Effects of Gravity Vector Orientation During Physical Vapor Transport Growth

NASA Technical Reports Server (NTRS)

Su, Ching-Hua; Feth, S.; Hirschfeld, D.; Smith, T. M.; Wang, Ling Jun; Volz, M. P.; Lehoczky, S. L.

1999-01-01

ZnSe crystals were grown by the physical vapor transport technique under horizontal and vertical (stabilized and destabilized) configurations. Secondary ion mass spectroscopy and photoluminescence measurements were performed on the grown ZnSe samples to map the distributions of [Si], [Fe], [Cu], [Al] and [Li or Na] impurities as well as Zn vacancy, [V (sub Zn)]. Annealings of ZnSe under controlled Zn pressures were studied to correlate the measured photoluminescence emission intensity to the equilibrium Zn partial pressure. In the horizontal grown crystals the segregations of [Si], [Fe], [Al] and [V (sub Zn)] were observed along the gravity vector direction whereas in the vertically stabilized grown crystal the segregation of these point defects was radially symmetrical. No apparent pattern was observed on the measured distributions in the vertically destabilized grown crystal. The observed segregations in the three growth configurations were interpreted based on the possible buoyancy-driven convection in the vapor phase.

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

NASA Technical Reports Server (NTRS)

Ma, Nancy

2003-01-01

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

Synthesis, characterization and anti-microbial activity of pure, Cu2+ and Cd2+ doped organic NLO l-arginine trifluoroacetate single crystals

NASA Astrophysics Data System (ADS)

Prasanyaa, T.; Haris, M.; Jayaramakrishnan, V.; Amgalan, M.; Mathivanan, V.

2013-10-01

Optically transparent Cu2+ and Cd2+ doped l-arginine trifluoroacetate (LATF) single crystals were grown from its aqueous solution using the slow solvent evaporation technique. The grown crystals were characterized by powder x-ray diffraction to confirm the monoclinic crystal structure. The percentage of transmittance measured using the ultraviolet-visible-near infrared spectrophotometer was found to be more than 80% for doped crystals. The functional group analysis of the grown crystals has been made by Fourier transform infrared spectroscopy. Thermogravimetric/differential thermal analysis was performed for the grown crystals. An atomic absorption study was carried out to determine the presence of Cu2+ and Cd2+. The hardness of the grown crystals was assessed and the results show a significant variation in the hardness value between the pure and doped LATF crystals. The second harmonic generation measurements show that Cu2+ doped LATF is 2.8 times greater and Cd2+ doped is 2.6 times greater than KDP. The anti-bacterial and anti-fungal activities of the title compound were performed using the disc diffusion method against standard bacteria Escherichia coli, Xanthomonas oryzae and against the fungus Aspergillus niger and Aspergillus flavus.

Second harmonic generation and crystal growth of new chalcone derivatives

NASA Astrophysics Data System (ADS)

Patil, P. S.; Dharmaprakash, S. M.; Ramakrishna, K.; Fun, Hoong-Kun; Sai Santosh Kumar, R.; Narayana Rao, D.

2007-05-01

We report on the synthesis, crystal structure and optical characterization of chalcone derivatives developed for second-order nonlinear optics. The investigation of a series of five chalcone derivatives with the second harmonic generation powder test according to Kurtz and Perry revealed that these chalcones show efficient second-order nonlinear activity. Among them, high-quality single crystals of 3-Br-4'-methoxychalcone (3BMC) were grown by solvent evaporation solution growth technique. Grown crystals were characterized by X-ray powder diffraction (XRD), laser damage threshold, UV-vis-NIR and refractive index measurement studies. Infrared spectroscopy, thermogravimetric analysis and differential thermal analysis measurements were performed to study the molecular vibration and thermal behavior of 3BMC crystal. Thermal analysis does not show any structural phase transition.

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

NASA Astrophysics Data System (ADS)

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

2015-06-01

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

Growth and spectroscopic, thermodynamic and nonlinear optical studies of L-threonine phthalate crystal

NASA Astrophysics Data System (ADS)

Theras, J. Elberin Mary; Kalaivani, D.; Jayaraman, D.; Joseph, V.

2015-10-01

L-threonine phthalate (LTP) single crystal has been grown using a solution growth technique at room temperature. Single crystal X-ray diffraction analysis reveals that LTP crystallizes in monoclinic crystal system with space group C2/c. The optical absorption studies show that the crystal is transparent in the entire visible region with a cut-off wavelength 309 nm. The optical band gap is found to be 4.05 eV. The functional groups of the synthesized compound have been identified by FTIR spectral analysis. The functional groups present in the material were also confirmed by FT-RAMAN spectroscopy. Surface morphology and the presence of various elements were studied by SEM-EDAX analysis. The thermal stability of LTP single crystal has been analyzed by TGA/DTA studies. The thermodynamic parameters such as activation energy, entropy, enthalpy and Gibbs free energy were determined for the grown material using TG data and Coats-Redfern relation. Since the grown crystal is centrosymmetric, Z-Scan studies were carried out for analyzing the third order nonlinear optical property. The nonlinear absorption coefficient, nonlinear refractive index and susceptibility have been measured using Z-Scan technique.

Crystal growth and characterization of Ce:Gd3(Ga,Al)5O12 single crystal using floating zone method in different O2 partial pressure

NASA Astrophysics Data System (ADS)

Yoshikawa, Akira; Fujimoto, Yutaka; Yamaji, Akihiro; Kurosawa, Shunsuke; Pejchal, Jan; Sugiyama, Makoto; Wakahara, Shingo; Futami, Yoshisuke; Yokota, Yuui; Kamada, Kei; Yubuta, Kunio; Shishido, Toetsu; Nikl, Martin

2013-09-01

Multicomponent garnet Ce:Gd3(Ga,Al)5O12 (Ce:GAGG) single crystals show very high light yield with reasonably fast scintillation response. Therefore, they can be promising scintillators for gamma-ray detection. However, in the decay curve a very slow component does exist. Therefore, it is necessary to optimize further the crystal growth technology of Ce:GAGG. In this study, Ce:GAGG single crystals were grown by the floating zone (FZ) method under atmospheres of various compositions such as Ar 100%, Ar 80% + O2 20%, Ar 60% + O2 40% and O2 100%. Radioluminescence spectra are dominated by the band at about 540 nm due to Ce3+ 5d1-4f transition. The Ce:GAGG single crystal grown under Ar atmosphere shows an intense slower decay component. It can be related to the processes of the delayed radiative recombination and thermally induced ionization of 5d1 level of Ce3+ center possibly further affected by oxygen vacancies. This slower decay process is significantly suppressed in the samples grown under the O2 containing atmosphere.

Conversion of broadband thermal radiation in lithium niobate crystals of various compositions

NASA Astrophysics Data System (ADS)

Syuy, A. V.; Litvinova, M. N.; Goncharova, P. S.; Sidorov, N. V.; Palatnikov, M. N.; Krishtop, V. V.; Likhtin, V. V.

2013-05-01

The conversion of the broadband thermal radiation in stoichiometric ( R = 1) lithium niobate single crystals that are grown from melt with 58.6 mol % of LiO2, congruent ( R = Li/Nb = 0.946) melt with the K2O flux admixture (4.5 and 6.0 wt %), and congruent melt and in congruent single crystals doped with the Zn2+, Gd3+, and Er3+ cations is studied. It is demonstrated that the conversion efficiency of the stoichiometric crystal that is grown from the melt with 58.6 mol % of LiO2 is less than the conversion efficiency of congruent crystal. In addition, the stoichiometric and almost stoichiometric crystals and the doped congruent crystals exhibit the blue shift of the peak conversion intensity in comparison with a nominally pure congruent crystal. For the congruent crystals, the conversion intensities peak at 520 and 495 nm, respectively.