Sample records for zeolite single crystals

  1. Synthesis of mesoporous zeolite single crystals with cheap porogens

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

    Tao Haixiang; Li Changlin; Ren Jiawen

    2011-07-15

    Mesoporous zeolite (silicalite-1, ZSM-5, TS-1) single crystals have been successfully synthesized by adding soluble starch or sodium carboxymethyl cellulose (CMC) to a conventional zeolite synthesis system. The obtained samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), nitrogen sorption analysis, {sup 27}Al magic angle spinning nuclear magnetic resonance ({sup 27}Al MAS NMR), temperature-programmed desorption of ammonia (NH{sub 3}-TPD) and ultraviolet-visible spectroscopy (UV-vis). The SEM images clearly show that all zeolite crystals possess the similar morphology with particle size of about 300 nm, the TEM images reveal that irregular intracrystalmore » pores are randomly distributed in the whole crystal. {sup 27}Al MAS NMR spectra indicate that nearly all of the Al atoms are in tetrahedral co-ordination in ZSM-5, UV-vis spectra confirm that nearly all of titanium atoms are incorporated into the framework of TS-1. The catalytic activity of meso-ZSM-5 in acetalization of cyclohexanone and meso-TS-1 in hydroxylation of phenol was also studied. The synthesis method reported in this paper is cost-effective and environmental friendly, can be easily expended to prepare other hierarchical structured zeolites. - Graphical abstract: Mesoporous zeolite single crystals were synthesized by using cheap porogens as template. Highlights: > Mesoporous zeolite (silicalite-1, ZSM-5, TS-1) single crystals were synthesized. > Soluble starch or sodium carboxymethyl cellulose (CMC) was used as porogens. > The mesoporous zeolites had connected mesopores although closed pores existed. > Higher catalytic activities were obtained.« less

  2. Development of a sorption rate technique for single zeolite crystals using an electrodynamic balance

    NASA Astrophysics Data System (ADS)

    Welegala, Mark Joseph

    Conventional means for evaluating intracrystalline diffusion in zeolites are complicated by extracrystalline mass transport resistances, crystallite size distribution, sorption heat effects, and finite instrument response times. A potentially direct means of overcoming these problems is to study sorption uptake on a single crystal suspended within a flowing gas stream in an electrodynamic balance (EDB). The objectives of this research were to design, build and investigate the viability of using such a device for obtaining diffusion coefficients from simple sorbate/zeolite systems, by computing the sorption uptake curve from the levitation voltage as a function of time. The initial electronic cell design was strongly influenced by flow mixing considerations. Accordingly, the conventional bihyperboloid electrode configuration was discarded in favor of novel four-ring (4R), and later two-ring/two-screen (2R/2S) designs with cylindrical interior geometries. A detailed numerical model based on the Method of Discrete Charges (MDC) was developed and used to aid in the design and operational understanding of these cells. Several 2R/2S designs were built and tested, including teflon/mica composite and ceramic cells capable of withstanding up to 750oF, for in situ activation of the zeolites. The diffusion of carbon dioxide in zeolite A was selected for testing due to the large differential weight change (10-20%) which occurs at ambient conditions and the availability of reliable experimental diffusion results (Yucel and Ruthven, 1980a). In addition to the carbon dioxide sorbate, water on zeolite 4A and a system relatively immune to atmospheric contamination, CO2 on activated carbon were also studied. Laboratory 4A crystals of up to 45 μm were grown using Charnell's method. These large solid particles were captured using a dry charging technique, and held during elevated temperature dehydration. Preliminary experimentation introduced externally dried crystals to the cell

  3. 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.

  4. Zeolite crystal growth in space

    NASA Technical Reports Server (NTRS)

    Sacco, Albert, Jr.; Thompson, Robert W.; Dixon, Anthony G.

    1991-01-01

    The growth of large, uniform zeolite crystals in high yield in space can have a major impact on the chemical process industry. Large zeolite crystals will be used to improve basic understanding of adsorption and catalytic mechanisms, and to make zeolite membranes. To grow large zeolites in microgravity, it is necessary to control the nucleation event and fluid motion, and to enhance nutrient transfer. Data is presented that suggests nucleation can be controlled using chemical compounds (e.g., Triethanolamine, for zeolite A), while not adversely effecting growth rate. A three-zone furnace has been designed to perform multiple syntheses concurrently. The operating range of the furnace is 295 K to 473 K. Teflon-lined autoclaves (10 ml liquid volume) have been designed to minimize contamination, reduce wall nucleation, and control mixing of pre-gel solutions on orbit. Zeolite synthesis experiments will be performed on USML-1 in 1992.

  5. Growth of zeolite crystals in the microgravity environment of space

    NASA Technical Reports Server (NTRS)

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

    1986-01-01

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

  6. Building zeolites from pre-crystallized units: nanoscale architecture.

    PubMed

    Corma, Avelino; Li, Chengeng; Moliner, Manuel

    2018-01-24

    Since the earlier descriptions by Barrer in the 40's on converting natural minerals into synthetic zeolites, the use of pre-crystallized zeolites as crucial inorganic directing agents to synthesize other crystalline zeolites with improved physico-chemical properties, has become a very intense and relevant research field, allowing the design, particularly in the last years, of new industrial catalysts. In the present review, we will highlight how the presence of some crystalline fragments in the synthesis media, such as small secondary building units (SBUs) or layered substructures, not only favors the crystallization of other zeolites presenting similar SBUs or layers, but also permits mostly controlling important parameters affecting to their catalytic activity (i.e. chemical composition, crystal size, or porosity, among others). In this sense, the recent advances on the preparation of 3-D and 2-D related zeolites through seeding and zeolite-to-zeolite transformation processes will be extensively revised, including their preparation in presence or absence of organic structure directing agents (OSDAs), with the aim of introducing general guidelines for designing more efficient future synthesis approaches for target zeolites. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Zeolites

    NASA Technical Reports Server (NTRS)

    1992-01-01

    Zeolites are crystalline aluminosilicates that have complex framework structures. However, there are several features of zeolite crystals that make unequivocal structure determinations difficult. The acquisition of reliable structural information on zeolites is greatly facilitated by the availability of high-quality specimens. For structure determinations by conventional diffraction techniques, large single-crystal specimens are essential. Alternatively, structural determinations by powder profile refinement methods relax the constraints on crystal size, but still require materials with a high degree of crystalline perfection. Studies conducted at CAMMP (Center for Advanced Microgravity Materials Processing) have demonstrated that microgravity processing can produce larger crystal sizes and fewer structural defects relative to terrestrial crystal growth. Principal Investigator: Dr. Albert Sacco

  8. Zeolite crystal growth in space - What has been learned

    NASA Technical Reports Server (NTRS)

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

    1993-01-01

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

  9. 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.

  10. Ultrasmall Zeolite L Crystals Prepared from Highly-Interdispersed Alkali-Silicate Precursors.

    PubMed

    Li, Rui; Linares, Noemi; Sutjianto, James G; Chawla, Aseem; Garcia Martinez, Javier; Rimer, Jeffrey D

    2018-06-19

    The preparation of nanosized zeolites is critical for applications where mass transport limitations within microporous networks hinder their performance. Oftentimes the ability to generate ultrasmall zeolite crystals is dependent upon the use of expensive organics with limited commercial relevance. Here, we report the generation of zeolite L crystals with uniform sizes less than 30 nm using a facile, organic-free method. Time-resolved analysis of precursor assembly and evolution during nonclassical crystallization highlights key differences among silicon sources. Our findings reveal that a homogenous dispersion of potassium ions throughout silicate precursors is critical to enhancing the rate of nucleation and facilitating the formation of ultrasmall crystals. Intimate contact between the inorganic structure-directing agent and silica leads to the formation of a metastable nonporous phase, identified as KAlSi2O6, which undergoes an intercrystalline transformation to zeolite L. The presence of highly-interdispersed alkali-silicate precursors is seemingly integral to a reduced zeolite induction time and may facilitate the development of ultrasmall crystals. Given the general difficulty of achieving nanosized crystals in zeolite synthesis, it is likely that using well-dispersed precursors does not have the same effect on all framework types; however, in select cases it may provide an alternative strategy for optimizing zeolite synthesis. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Influence of Crystal Expansion/Contraction on Zeolite Membrane Permeation

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

    Sorenson, Stephanie G; Payzant, E Andrew; Noble, Richard D

    X-ray diffraction was used to measure the unit cell parameters of B-ZSM-5, SAPO-34, and NaA zeolite powders as a function of adsorbate loading at 303 K, and in one case, at elevated temperatures. Most adsorbates expanded the zeolite crystals below saturation loading at 303 K: n-hexane and SF6 in B-ZSM-5, methanol and CO2 in SAPO-34, and methanol in NaA zeolite. As the loadings increased, the crystals expanded more. Changes in the unit cell volumes of B-ZSM-5 and SAPO-34 zeolite powders correlated with changes in permeation through zeolite membranes defects. When the zeolite crystals expanded or contracted upon adsorption, the defectmore » sizes decreased or increased. In B-ZSM-5 membranes, the fluxes through defects decreased dramatically when n-hexane or SF6 adsorbed. In contrast, i-butane adsorption at 303 K contracted B-ZSM-5 crystals at low loadings and expanded them at higher loadings. Correspondingly, the flux through B-ZSM-5 membrane defects increased at low i-butane loadings and decreased at high loading because the defects increased in size at low loading and decreased at high loadings. At 398 K and 473 K, n-hexane expanded the B-ZSM-5 unit cell more as the temperature increased from 303 to 473 K. The silicalite-1 and B-ZSM-5 unit cell volumes expanded similarly upon n-hexane adsorption at 303 K; boron substitution had little effect on volume expansion.« less

  12. Highly mesoporous single-crystalline zeolite beta synthesized using a nonsurfactant cationic polymer as a dual-function template.

    PubMed

    Zhu, Jie; Zhu, Yihan; Zhu, Liangkui; Rigutto, Marcello; van der Made, Alexander; Yang, Chengguang; Pan, Shuxiang; Wang, Liang; Zhu, Longfeng; Jin, Yinying; Sun, Qi; Wu, Qinming; Meng, Xiangju; Zhang, Daliang; Han, Yu; Li, Jixue; Chu, Yueying; Zheng, Anmin; Qiu, Shilun; Zheng, Xiaoming; Xiao, Feng-Shou

    2014-02-12

    Mesoporous zeolites are useful solid catalysts for conversion of bulky molecules because they offer fast mass transfer along with size and shape selectivity. We report here the successful synthesis of mesoporous aluminosilicate zeolite Beta from a commercial cationic polymer that acts as a dual-function template to generate zeolitic micropores and mesopores simultaneously. This is the first demonstration of a single nonsurfactant polymer acting as such a template. Using high-resolution electron microscopy and tomography, we discovered that the resulting material (Beta-MS) has abundant and highly interconnected mesopores. More importantly, we demonstrated using a three-dimensional electron diffraction technique that each Beta-MS particle is a single crystal, whereas most previously reported mesoporous zeolites are comprised of nanosized zeolitic grains with random orientations. The use of nonsurfactant templates is essential to gaining single-crystalline mesoporous zeolites. The single-crystalline nature endows Beta-MS with better hydrothermal stability compared with surfactant-derived mesoporous zeolite Beta. Beta-MS also exhibited remarkably higher catalytic activity than did conventional zeolite Beta in acid-catalyzed reactions involving large molecules.

  13. Zeolite Crystal Growth in Microgravity and on Earth

    NASA Technical Reports Server (NTRS)

    2003-01-01

    The Center for Advanced Microgravity Materials Processing (CAMMP), a NASA-sponsored Research Partnership Center, is working to improve zeolite materials for storing hydrogen fuel. CAMMP is also applying zeolites to detergents, optical cables, gas and vapor detection for environmental monitoring and control, and chemical production techniques that significantly reduce by-products that are hazardous to the environment. Shown here are zeolite crystals (top) grown in a ground control experiment and grown in microgravity on the USML-2 mission (bottom). Zeolite experiments have also been conducted aboard the International Space Station.

  14. Sub-Micrometer Zeolite Films on Gold-Coated Silicon Wafers with Single-Crystal-Like Dielectric Constant and Elastic Modulus

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

    Tiriolo, Raffaele; Rangnekar, Neel; Zhang, Han

    A low-temperature synthesis coupled with mild activation produces zeolite films exhibiting low dielectric constant (low-k) matching the theoretically predicted and experimentally measured values for single crystals. This synthesis and activation method allows for the fabrication of a device consisting of a b-oriented film of the pure-silica zeolite MFI (silicalite-1) supported on a gold-coated silicon wafer. The zeolite seeds are assembled by a manual assembly process and subjected to optimized secondary growth conditions that do not cause corrosion of the gold underlayer, while strongly promoting in-plane growth. The traditional calcination process is replaced with a non-thermal photochemical activation to ensure preservationmore » of an intact gold layer. The dielectric constant (k), obtained through measurement of electrical capacitance in a metal-insulator-metal configuration, highlights the ultralow k approximate to 1.7 of the synthetized films, which is among the lowest values reported for an MFI film. There is large improvement in elastic modulus of the film (E approximate to 54 GPa) over previous reports, potentially allowing for integration into silicon wafer processing technology.« less

  15. Commander Bowersox Tends to Zeolite Crystal Samples Aboard Space Station

    NASA Technical Reports Server (NTRS)

    2003-01-01

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

  16. Preliminary market analysis for large zeolite crystals. B.S. Thesis

    NASA Technical Reports Server (NTRS)

    Doblmaier, Thomas; Grafing, Paul; Knight, Kim

    1987-01-01

    Zeolite crystals are used in the manufacture of countless products today, which utilize their properties of absorption, ion exchange, and catalysis. It was determined that zeolites grown in space could be much larger in size than any of those currently available on Earth. The objective was to identify and examine some of the potential uses for these larger crystals. Of the several industries examined, the medical and nuclear industries offer the greatest potential.

  17. Crewmember working on the mid deck Zeolite Crystal Growth experiment.

    NASA Technical Reports Server (NTRS)

    1992-01-01

    View showing Payload Specialist Bonnie Dunbar, in the mid deck, conducting the Zeolite Crystal Growth (ZCG) Experiment in the mid deck stowage locker work area. View shows assembly of zeolite sample in the metal autoclave cylinders prior to insertion into the furnace.

  18. Reversible conversion of valence-tautomeric copper metal-organic frameworks dependent single-crystal-to-single-crystal oxidation/reduction: a redox-switchable catalyst for C-H bonds activation reaction.

    PubMed

    Huang, Chao; Wu, Jie; Song, Chuanjun; Ding, Ran; Qiao, Yan; Hou, Hongwei; Chang, Junbiao; Fan, Yaoting

    2015-06-28

    Upon single-crystal-to-single-crystal (SCSC) oxidation/reduction, reversible structural transformations take place between the anionic porous zeolite-like Cu(I) framework and a topologically equivalent neutral Cu(I)Cu(II) mixed-valent framework. The unique conversion behavior of the Cu(I) framework endowed it as a redox-switchable catalyst for the direct arylation of heterocycle C-H bonds.

  19. Probing Zeolite Crystal Architecture and Structural Imperfections using Differently Sized Fluorescent Organic Probe Molecules.

    PubMed

    Hendriks, Frank C; Schmidt, Joel E; Rombouts, Jeroen A; Lammertsma, Koop; Bruijnincx, Pieter C A; Weckhuysen, Bert M

    2017-05-05

    A micro-spectroscopic method has been developed to probe the accessibility of zeolite crystals using a series of fluorescent 4-(4-diethylaminostyryl)-1-methylpyridinium iodide (DAMPI) probes of increasing molecular size. Staining large zeolite crystals with MFI (ZSM-5) topology and subsequent mapping of the resulting fluorescence using confocal fluorescence microscopy reveal differences in structural integrity: the 90° intergrowth sections of MFI crystals are prone to develop structural imperfections, which act as entrance routes for the probes into the zeolite crystal. Polarization-dependent measurements provide evidence for the probe molecule's alignment within the MFI zeolite pore system. The developed method was extended to BEA (Beta) crystals, showing that the previously observed hourglass pattern is a general feature of BEA crystals with this morphology. Furthermore, the probes can accurately identify at which crystal faces of BEA straight or sinusoidal pores open to the surface. The results show this method can spatially resolve the architecture-dependent internal pore structure of microporous materials, which is difficult to assess using other characterization techniques such as X-ray diffraction. © 2017 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

  20. Highly crystallized nanometer-sized zeolite a with large Cs adsorption capability for the decontamination of water.

    PubMed

    Torad, Nagy L; Naito, Masanobu; Tatami, Junichi; Endo, Akira; Leo, Sin-Yen; Ishihara, Shinsuke; Wu, Kevin C-W; Wakihara, Toru; Yamauchi, Yusuke

    2014-03-01

    Nanometer-sized zeolite A with a large cesium (Cs) uptake capability is prepared through a simple post-milling recrystallization method. This method is suitable for producing nanometer-sized zeolite in large scale, as additional organic compounds are not needed to control zeolite nucleation and crystal growth. Herein, we perform a quartz crystal microbalance (QCM) study to evaluate the uptake ability of Cs ions by zeolite, to the best of our knowledge, for the first time. In comparison to micrometer-sized zeolite A, nanometer-sized zeolite A can rapidly accommodate a larger amount of Cs ions into the zeolite crystal structure, owing to its high external surface area. Nanometer-sized zeolite is a promising candidate for the removal of radioactive Cs ions from polluted water. Our QCM study on Cs adsorption uptake behavior provides the information of adsorption kinetics (e.g., adsorption amounts and rates). This technique is applicable to other zeolites, which will be highly valuable for further consideration of radioactive Cs removal in the future. Copyright © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Crewmember in the mid deck with the Zeolite Crystal Growth experiment.

    NASA Image and Video Library

    1992-07-09

    STS50-262-004 (25 June-9 July 1992) --- Astronaut Kenneth D. Bowersox, STS-50 pilot, holds an autoclave used in the growing of zeolite crystals on the middeck of the Earth-orbiting Space Shuttle Columbia. He is standing near the Zeolite Crystal Growth (ZCG) furnace, which is housed in the space of two stowage lockers. On the 14-day U.S. Microgravity Laboratory mission, zeolite crystals were grown in 38 individual autoclaves, which were joined in pairs to be inserted into the 19 furnace orifices. While the autoclaves appear the same externally, there are several types of internal arrangements that were tested to determine which one provides the best mixing of the component solutions. The portrait of alternate payload specialist Albert Sacco, Jr. is mounted nearby. Sacco, serving as a ground controller at Marshall Space Flight Center in Alabama, worked in conjunction with the red shift crew in the science module.

  2. Cutting Materials in Half: A Graph Theory Approach for Generating Crystal Surfaces and Its Prediction of 2D Zeolites.

    PubMed

    Witman, Matthew; Ling, Sanliang; Boyd, Peter; Barthel, Senja; Haranczyk, Maciej; Slater, Ben; Smit, Berend

    2018-02-28

    Scientific interest in two-dimensional (2D) materials, ranging from graphene and other single layer materials to atomically thin crystals, is quickly increasing for a large variety of technological applications. While in silico design approaches have made a large impact in the study of 3D crystals, algorithms designed to discover atomically thin 2D materials from their parent 3D materials are by comparison more sparse. We hypothesize that determining how to cut a 3D material in half (i.e., which Miller surface is formed) by severing a minimal number of bonds or a minimal amount of total bond energy per unit area can yield insight into preferred crystal faces. We answer this question by implementing a graph theory technique to mathematically formalize the enumeration of minimum cut surfaces of crystals. While the algorithm is generally applicable to different classes of materials, we focus on zeolitic materials due to their diverse structural topology and because 2D zeolites have promising catalytic and separation performance compared to their 3D counterparts. We report here a simple descriptor based only on structural information that predicts whether a zeolite is likely to be synthesizable in the 2D form and correctly identifies the expressed surface in known layered 2D zeolites. The discovery of this descriptor allows us to highlight other zeolites that may also be synthesized in the 2D form that have not been experimentally realized yet. Finally, our method is general since the mathematical formalism can be applied to find the minimum cut surfaces of other crystallographic materials such as metal-organic frameworks, covalent-organic frameworks, zeolitic-imidazolate frameworks, metal oxides, etc.

  3. Cutting Materials in Half: A Graph Theory Approach for Generating Crystal Surfaces and Its Prediction of 2D Zeolites

    PubMed Central

    2018-01-01

    Scientific interest in two-dimensional (2D) materials, ranging from graphene and other single layer materials to atomically thin crystals, is quickly increasing for a large variety of technological applications. While in silico design approaches have made a large impact in the study of 3D crystals, algorithms designed to discover atomically thin 2D materials from their parent 3D materials are by comparison more sparse. We hypothesize that determining how to cut a 3D material in half (i.e., which Miller surface is formed) by severing a minimal number of bonds or a minimal amount of total bond energy per unit area can yield insight into preferred crystal faces. We answer this question by implementing a graph theory technique to mathematically formalize the enumeration of minimum cut surfaces of crystals. While the algorithm is generally applicable to different classes of materials, we focus on zeolitic materials due to their diverse structural topology and because 2D zeolites have promising catalytic and separation performance compared to their 3D counterparts. We report here a simple descriptor based only on structural information that predicts whether a zeolite is likely to be synthesizable in the 2D form and correctly identifies the expressed surface in known layered 2D zeolites. The discovery of this descriptor allows us to highlight other zeolites that may also be synthesized in the 2D form that have not been experimentally realized yet. Finally, our method is general since the mathematical formalism can be applied to find the minimum cut surfaces of other crystallographic materials such as metal–organic frameworks, covalent-organic frameworks, zeolitic-imidazolate frameworks, metal oxides, etc. PMID:29532024

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

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

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

    2011-01-15

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

  5. Cutting Materials in Half: A Graph Theory Approach for Generating Crystal Surfaces and Its Prediction of 2D Zeolites

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

    Witman, Matthew; Ling, Sanliang; Boyd, Peter

    Scientific interest in two-dimensional (2D) materials, ranging from graphene and other single layer materials to atomically thin crystals, is quickly increasing for a large variety of technological applications. While in silico design approaches have made a large impact in the study of 3D crystals, algorithms designed to discover atomically thin 2D materials from their parent 3D materials are by comparison more sparse. Here, we hypothesize that determining how to cut a 3D material in half (i.e., which Miller surface is formed) by severing a minimal number of bonds or a minimal amount of total bond energy per unit area canmore » yield insight into preferred crystal faces. We answer this question by implementing a graph theory technique to mathematically formalize the enumeration of minimum cut surfaces of crystals. While the algorithm is generally applicable to different classes of materials, we focus on zeolitic materials due to their diverse structural topology and because 2D zeolites have promising catalytic and separation performance compared to their 3D counterparts. We report here a simple descriptor based only on structural information that predicts whether a zeolite is likely to be synthesizable in the 2D form and correctly identifies the expressed surface in known layered 2D zeolites. The discovery of this descriptor allows us to highlight other zeolites that may also be synthesized in the 2D form that have not been experimentally realized yet. Finally, our method is general since the mathematical formalism can be applied to find the minimum cut surfaces of other crystallographic materials such as metal-organic frameworks, covalent-organic frameworks, zeolitic-imidazolate frameworks, metal oxides, etc.« less

  6. Cutting Materials in Half: A Graph Theory Approach for Generating Crystal Surfaces and Its Prediction of 2D Zeolites

    DOE PAGES

    Witman, Matthew; Ling, Sanliang; Boyd, Peter; ...

    2018-02-06

    Scientific interest in two-dimensional (2D) materials, ranging from graphene and other single layer materials to atomically thin crystals, is quickly increasing for a large variety of technological applications. While in silico design approaches have made a large impact in the study of 3D crystals, algorithms designed to discover atomically thin 2D materials from their parent 3D materials are by comparison more sparse. Here, we hypothesize that determining how to cut a 3D material in half (i.e., which Miller surface is formed) by severing a minimal number of bonds or a minimal amount of total bond energy per unit area canmore » yield insight into preferred crystal faces. We answer this question by implementing a graph theory technique to mathematically formalize the enumeration of minimum cut surfaces of crystals. While the algorithm is generally applicable to different classes of materials, we focus on zeolitic materials due to their diverse structural topology and because 2D zeolites have promising catalytic and separation performance compared to their 3D counterparts. We report here a simple descriptor based only on structural information that predicts whether a zeolite is likely to be synthesizable in the 2D form and correctly identifies the expressed surface in known layered 2D zeolites. The discovery of this descriptor allows us to highlight other zeolites that may also be synthesized in the 2D form that have not been experimentally realized yet. Finally, our method is general since the mathematical formalism can be applied to find the minimum cut surfaces of other crystallographic materials such as metal-organic frameworks, covalent-organic frameworks, zeolitic-imidazolate frameworks, metal oxides, etc.« less

  7. Transport phenomena of growth-in-gel zeolite crystallization in microgravity

    NASA Technical Reports Server (NTRS)

    Zhang, H.; Ostrach, S.; Kamotani, Y.

    1993-01-01

    Secondary nucleation (SN) due to crystal sedimentation has been believed to be one of the major effects that causes smaller sizes of final zeolite crystals. The present investigation indicates that, in a reactor, this gravity-induced SN occurs only within a white opaque column termed the gel portion. Under normal gravity this portion shrinks to the bottom of the hydrothermal reactor, leaving a clear portion of solution at the top, due to depletion of the flocculated gel particles. Solution phase nucleation and crystallization is assumed and a correlation for the shrinkage is therefore derived, which shows good agreement with experimental observations. A non-dimensional parameter is suggested as a criterion for the occurrence of SN. Based on the parameter whether or not microgravity is beneficial to zeolite growth is discussed. Also, the growth mechanism and the transport phenomena in the absence of gravity are discussed.

  8. Diagnosing the Internal Architecture of Zeolite Ferrierite

    PubMed Central

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

    2017-01-01

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

  9. Adsorption of Crystal Violet Dye Using Zeolite A Synthesized From Coal Fly Ash

    NASA Astrophysics Data System (ADS)

    Jumaeri; Kusumastuti, E.; Santosa, S. J.; Sutarno

    2017-02-01

    Adsorption of Crystal Violet (CV) dye using zeolite A synthesized from coal fly ash (ZA) has been done. Effect of pH, contact time, and the initial concentration of dye adsorption was studied in this adsorption. Model experimental of adsorption isotherms and adsorption kinetics were also studied. The adsorption is done in a batch reactor at room temperature. A total of 0.01 g of zeolite A was added to the Erlenmeyer flask 50 mL containing 20 mL of the dye solution of Crystal Violet in a variety of conditions of pH, contact time and initial concentration. Furthermore, Erlenmeyer flask and its contents were shaken using an orbital shaker at a speed of 200 rpm. After a specified period of adsorption, the solution was centrifuged for 2 minutes so that the solids separated from the solution. The concentration of the dye after adsorption determined using Genesis-20 Spectrophotometer. The results showed that the Zeolite A synthesized from coal fly ash could be used as an effective adsorbent for Crystal Violet dye. The optimum adsorption occurs at pH 6, and contact time 45 minutes. At the initial concentration of 2 to 6 mg/L, adsorption is reduced from 79 to 62.8%. Crystal Violet dye adsorption in zeolite A fulfilled kinetic model of pseudo-order 2 and model of Freundlich adsorption isotherm.

  10. A facile strategy to design zeolite L crystals with tunable morphology and surface architecture.

    PubMed

    Lupulescu, Alexandra I; Kumar, Manjesh; Rimer, Jeffrey D

    2013-05-01

    Tailoring the anisotropic growth rates of materials to achieve desired structural outcomes is a pervasive challenge in synthetic crystallization. Here we discuss a method to selectively control the growth of zeolite crystals, which are used extensively in a wide range of industrial applications. This facile method cooperatively tunes crystal properties, such as morphology and surface architecture, through the use of inexpensive, commercially available chemicals with specificity for binding to crystallographic surfaces and mediating anisotropic growth. We examined over 30 molecules as potential zeolite growth modifiers (ZGMs) of zeolite L (LTL type) crystallization. ZGM efficacy was quantified through a combination of macroscopic (bulk) and microscopic (surface) investigations that identified modifiers capable of dramatically altering the cylindrical morphology of LTL crystals. We demonstrate an ability to tailor properties critical to zeolite performance, such as external porous surface area, crystal shape, and pore length, which can enhance sorbate accessibility to LTL pores, tune the supramolecular organization of guest-host composites, and minimize the diffusion path length, respectively. We report that a synergistic combination of ZGMs and the judicious adjustment of synthesis parameters produce LTL crystals with unique surface features, and a range of length-to-diameter aspect ratios spanning 3 orders of magnitude. A systematic examination of different ZGM structures and molecular compositions (i.e., hydrophobicity and binding moieties) reveal interesting physicochemical properties governing their efficacy and specificity. Results of this study suggest this versatile strategy may prove applicable for a host of framework types to produce unrivaled materials that have eluded more conventional techniques.

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

    PubMed

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

    2012-03-07

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

  12. Diagram of Zeolite Crystals

    NASA Technical Reports Server (NTRS)

    2003-01-01

    The Center for Advanced Microgravity Materials Processing (CAMMP) in Cambridge, MA, a NASA-sponsored Commercial Space Center, is working to improve zeolite materials for storing hydrogen fuel. CAMMP is also applying zeolites to detergents, optical cables, gas and vapor detection for environmental monitoring and control, and chemical production techniques that significantly reduce by-products that are hazardous to the environment. Depicted here is one of the many here complex geometric shapes which make them highly absorbent. Zeolite experiments have also been conducted aboard the International Space Station

  13. The assessment of pore connectivity in hierarchical zeolites using positron annihilation lifetime spectroscopy: instrumental and morphological aspects.

    PubMed

    Zubiaga, Asier; Warringham, Robbie; Boltz, Marilyne; Cooke, David; Crivelli, Paolo; Gidley, David; Pérez-Ramírez, Javier; Mitchell, Sharon

    2016-04-07

    Recent studies demonstrated the power of positron annihilation lifetime spectroscopy (PALS) to characterise the connectivity and corresponding effectiveness of hierarchical pore networks in zeolites. This was based on the fractional escape of ortho-positronium (Ps), formed within the micropore framework, to vacuum. To further develop this technique, here we assess the impact of the positron implantation energy and of the zeolite crystal size and the particle morphology. Conventional measurements using fast positrons and beam measurements applying moderated positrons both readily distinguish purely microporous ZSM-5 zeolites comprised of single crystals or crystal aggregates. Unlike beam measurements, however, conventional measurements fail to discriminate model hierarchical zeolites with open or constricted mesopore architectures. Several steps are taken to rationalise these observations. The dominant contribution of Ps diffusion to the PALS response is confirmed by capping the external surface of the zeolite crystals with tetraethylorthosilicate, which greatly enhances the sensitivity to the micropore network. A one-dimensional model is constructed to predict the out-diffusion of Ps from a zeolite crystal, which is validated experimentally by comparing coffin-shaped single crystals of varying size. Calculation of the trends expected on the application of fast or moderated positrons indicates that the distinctions in the initial distribution of Ps at the crystal level cannot explain the limited sensitivity of the former to the mesopore architecture. Instead, we propose that the greater penetration of fast positrons within the sample increases the probability of Ps re-entry from intercrystalline voids into mesopores connected with the external surface of zeolite crystals, thereby reducing their fractional escape.

  14. Growth of large zeolite crystals in space

    NASA Technical Reports Server (NTRS)

    Sacco, A., Jr.; Dixon, A.; Thompson, R.; Scott, G.; Ditr, J.

    1988-01-01

    Synthesis studies performed using close analogs of triethanolamine (TEA) have shown that all three hydroxyl groups and the amine group in this molecule are necessary to provide nucleation suppression. Studies using C-13 nuclear magnetic resonance (NMR) revealed that the hydroxyl ions and the amine group are involved in the formation of an aluminum complex. It was also shown that silicate species fo not interact this way with TEA in an alkaline solution. These results suggest that successful aluminum complexation leads to nucleation in zeolite-A crystallization.

  15. Expedition Six Commander Bowersox working with Zeolite Crystal Growth in U.S. Lab

    NASA Image and Video Library

    2002-12-05

    ISS006-E-07127 (5 December 2002) --- Astronaut Kenneth D. Bowersox, Expedition Six mission commander, works with the Zeolite Crystal Growth (ZCG) experiment in the Destiny laboratory on the International Space Station (ISS).

  16. In-Line Measurement of Water Contents in Ethanol Using a Zeolite-Coated Quartz Crystal Microbalance

    PubMed Central

    Kim, Byoung Chul; Yamamoto, Takuji; Kim, Young Han

    2015-01-01

    A quartz crystal microbalance (QCM) was utilized to measure the water content in ethanol. For the improvement of measurement sensitivity, the QCM was modified by applying zeolite particles on the surface with poly(methyl methacrylate) (PMMA) binder. The measurement performance was examined with ethanol of 1% to 5% water content in circulation. The experimental results showed that the frequency drop of the QCM was related with the water content though there was some deviation. The sensitivity of the zeolite-coated QCM was sufficient to be implemented in water content determination, and a higher ratio of silicon to aluminum in the molecular structure of the zeolite gave better performance. The coated surface was inspected by microscopy to show the distribution of zeolite particles and PMMA spread. PMID:26516859

  17. One-pot pseudomorphic crystallization of mesoporous porous silica to hierarchical porous zeolites

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

    Xing, Jun-Ling; Jiang, Shu-Hua; Pang, Jun-Ling

    2015-09-15

    Hierarchically porous silica with mesopore and zeolitic micropore was synthesized via pseudomorphic crystallization under high-temperature hydrothermal treatment in the presence of cetyltrimethylammonium tosylate and tetrapropylammonium ions. A combined characterization using small-angle X-ray diffraction (XRD), nitrogen adsorption, high-resolution transmission electron microscopy (TEM), thermogravimetric analysis (TG), and elemental analysis showed that dual templates, CTA{sup +} and TPA{sup +} molecules, can work in a cooperative manner to synthesize mesoporous zeolite in a one-pot system by precisely tuning the reaction conditions, such as reaction time and temperature, and type and amount of heterometal atoms. It is found that the presence of Ti precursor ismore » critical to the successful synthesis of such nanostructure. It not only retards the nucleation and growth of crystalline MFI domains, but also acts as nano-binder or nano-glue to favor the assembly of zeolite nanoblocks. - Graphical abstract: Display Omitted - Highlights: • A facile method to synthesize mesoporous zeolites with hierarchical porosity was presented. • It gives a new insight into keeping the balance between mesoscopic and molecular ordering in hierarchical porous materials. • A new understanding on the solid–solid transformation mechanism for the synthesis of titanosilicate zeolites was proposed.« less

  18. A bioscaffolding strategy for hierarchical zeolites with a nanotube-trimodal network.

    PubMed

    Li, Guannan; Huang, Haibo; Yu, Bowen; Wang, Yun; Tao, Jiawei; Wei, Yingxu; Li, Shougui; Liu, Zhongmin; Xu, Yan; Xu, Ruren

    2016-02-01

    Hierarchical zeolite monoliths with multimodal porosity are of paramount importance as they open up new horizons for advanced applications. So far, hierarchical zeolites based on nanotube scaffolds have never been reported. Inspired by the organization of biominerals, we have developed a novel precursor scaffolding-solid phase crystallization strategy for hierarchical zeolites with a unique nanotube scaffolding architecture and nanotube-trimodal network, where biomolecular self-assembly (BSA) provides a scaffolding blueprint. By vapor-treating Sil-1 seeded precursor scaffolds, zeolite MFI nanotube scaffolds are self-generated, during which evolution phenomena such as segmented voids and solid bridges are observed, in agreement with the Kirkendall effect in a solid-phase crystallization system. The nanotube walls are made of intergrown single crystals rendering good mechanical stability. The inner diameter of the nanotube is tunable between 30 and 90 nm by varying the thickness of the precursor layers. Macropores enclosed by cross-linked nanotubes can be modulated by the choice of BSA. Narrow mesopores are formed by intergrown nanocrystals. Hierarchical ZSM-5 monoliths with nanotube (90 nm), micropore (0.55 nm), mesopore (2 nm) and macropore (700 nm) exhibit superior catalytic performance in the methanol-to-hydrocarbon (MTH) conversion compared to conventional ZSM-5. BSA remains intact after crystallization, allowing a higher level of organization and functionalization of the zeolite nanotube scaffolds. The current work may afford a versatile strategy for hierarchical zeolite monoliths with nanotube scaffolding architectures and a nanotube-multimodal network leading to self-supporting and active zeolite catalysts, and for applications beyond.

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

    NASA Technical Reports Server (NTRS)

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

    2003-01-01

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

  20. Zeolite-like liquid crystals

    NASA Astrophysics Data System (ADS)

    Poppe, Silvio; Lehmann, Anne; Scholte, Alexander; Prehm, Marko; Zeng, Xiangbing; Ungar, Goran; Tschierske, Carsten

    2015-10-01

    Zeolites represent inorganic solid-state materials with porous structures of fascinating complexity. Recently, significant progress was made by reticular synthesis of related organic solid-state materials, such as metal-organic or covalent organic frameworks. Herein we go a step further and report the first example of a fluid honeycomb mimicking a zeolitic framework. In this unique self-assembled liquid crystalline structure, transverse-lying π-conjugated rod-like molecules form pentagonal channels, encircling larger octagonal channels, a structural motif also found in some zeolites. Additional bundles of coaxial molecules penetrate the centres of the larger channels, unreachable by chains attached to the honeycomb framework. This creates a unique fluid hybrid structure combining positive and negative anisotropies, providing the potential for tuning the directionality of anisotropic optical, electrical and magnetic properties. This work also demonstrates a new approach to complex soft-matter self-assembly, by using frustration between space filling and the entropic penalty of chain extension.

  1. Crystallization process of zeolite rho prepared by hydrothermal synthesis using 18-crown-6 ether as organic template.

    PubMed

    Araki, Sadao; Kiyohara, Yasato; Tanaka, Shunsuke; Miyake, Yoshikazu

    2012-06-15

    There are many viewpoints on the formation mechanisms for zeolites, but the details are not clear. An understanding of the elementary steps for their formation is important for the development of large-scale membranes and efficient manufacturing processes. In this study, the effects of silicon, aluminum, and the incorporation of 18-crown-6 (18C6) ether, on the formation of zeolite rho, using 18C6 as the structure directing agent (SDA) have been investigated by using field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray fluorescence spectrometry (EDX), nuclear magnetic resonance spectroscopy (NMR), thermo gravimetric analysis (TGA), and the pH measurement. These results suggested that a zeolite rho has four synthesis steps; (1) 0-3 h, the dehydration and condensation reaction between the silica and alumina to form amorphous aluminosilicates; (2) 3-20 h, the particle growth and aggregation process for the amorphous aluminosilicates; (3) 20-48 h, the crystallization and crystal growth of zeolite rho, with the incorporation of 18C6; and (4) 48-96 h, gentle growth with an increase in Na/Si ratio and a change in rate for the bounding state between the silica- and the alumina-based species. We consider the above to reflect the four steps for the formation of zeolite rho. Copyright © 2012 Elsevier Inc. All rights reserved.

  2. A systematic typology for negative Poisson's ratio materials and the prediction of complete auxeticity in pure silica zeolite JST.

    PubMed

    Siddorn, M; Coudert, F-X; Evans, K E; Marmier, A

    2015-07-21

    Single crystals can commonly have negative Poisson's ratio in a few directions; however more generalised auxeticity is rarer. We propose a typology to distinguish auxetic materials. We characterise numerous single crystals and demonstrate that partial auxeticity occurs for around 37%. We find average auxeticity to be limited to α-cristobalite and no example of complete auxeticity. We simulate two hundreds pure silica zeolites with empirical potentials and quantum chemistry methods, and for the first time identify complete auxeticity in a zeolite network, JST.

  3. Early stages of zeolite growth

    NASA Astrophysics Data System (ADS)

    Kumar, Sandeep

    Zeolites are crystalline nonporous aluminosilicates with important applications in separation, purification, and adsorption of liquid and gaseous molecules. However, an ability to tailor the zeolite microstructure, such as particle size/shape and pore-size, to make it benign for specific application requires control over nucleation and particle growth processes. But, the nucleation and crystallization mechanisms of zeolites are not fully understood. In this context, the synthesis of an all-silica zeolite with MFI-type framework has been studied extensively as a model system. Throughout chapters 2, 4 and 5, MFI growth process has been investigated by small-angle x-ray scattering (SAXS) and transmission electron microscopy (TEM). Of fundamental importance is the role of nanoparticles (~5 nm), which are present in the precursor sol, in MFI nucleation and crystallization. Formation of amorphous aggregates and their internal restructuring are concluded as essential steps in MFI nucleation. Early stage zeolite particles have disordered and less crystalline regions within, which indicates the role of structurally distributed population of nanoparticles in growth. Faceting occurs after the depletion of nanoparticles. The chapter 6 presents growth studies in silica sols prepared by using a dimer of tertaprpylammonium (TPA) and reports that MFI nucleation and crystallization are delayed with a more pronounced delay in crystal growth.

  4. Rapid synthesis of beta zeolites

    DOEpatents

    Fan, Wei; Chang, Chun -Chih; Dornath, Paul; Wang, Zhuopeng

    2015-08-18

    The invention provides methods for rapidly synthesizing heteroatom containing zeolites including Sn-Beta, Si-Beta, Ti-Beta, Zr-Beta and Fe-Beta. The methods for synthesizing heteroatom zeolites include using well-crystalline zeolite crystals as seeds and using a fluoride-free, caustic medium in a seeded dry-gel conversion method. The Beta zeolite catalysts made by the methods of the invention catalyze both isomerization and dehydration reactions.

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

    NASA Technical Reports Server (NTRS)

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

    1999-01-01

    Crystals grown from liquid solutions have important industrial applications. Zeolites, for instance, a class of crystalline aluminosilicate materials, form the backbone of the chemical process industry worldwide, as they are used as adsorbents and catalysts. Many of the phenomena associated with crystal growth processes are not well understood due to complex microscopic and macroscopic interactions. Microgravity could help elucidate these phenomena and allow the control of defect locations, concentration, as well as size of crystals. Microgravity in an orbiting spacecraft could help isolate the possible effects of natural convection (which affects defect formation) and minimize sedimentation. In addition, crystals will stay essentially suspended in the nutrient pool under a diffusion-limited growth condition. This is expected to promote larger crystals by allowing a longer residence time in a high-concentration nutrient field. Among other factors, the crystal size distribution depends on the nucleation rate and crystallization. These two are also related to the "gel" polymerization/depolymerization rate. Macroscopic bulk mass and flow transport and especially gravity, force the crystals down to the bottom of the reactor, thus forming a sedimentation layer. In this layer, the growth rate of the crystals slows down as crystals compete for a limited amount of nutrients. The macroscopic transport phenomena under certain conditions can, however, enhance the nutrient supply and therefore, accelerate crystal growth. Several zeolite experiments have been performed in space with mixed results. The results from our laboratory have indicated an enhancement in size of 30 to 70 percent compared to the best ground based controls, and a reduction of lattice defects in many of the space grown crystals. Such experiments are difficult to interpret, and cannot be easily used to derive empirical or other laws since many physical parameters are simultaneously involved in the process

  6. Coke formation in a zeolite crystal during the methanol-to-hydrocarbons reaction as studied with atom probe tomography

    DOE PAGES

    Schmidt, Joel E.; Poplawsky, Jonathan D.; Mazumder, Baishakhi; ...

    2016-08-03

    Understanding the formation of carbon deposits in zeolites is vital to developing new, superior materials for various applications, including oil and gas conversion processes. Herein, atom probe tomography (APT) has been used to spatially resolve the 3D compositional changes at the sub-nm length scale in a single zeolite ZSM-5 crystal, which has been partially deactivated by the methanol-to-hydrocarbons reaction using 13C-labeled methanol. The results reveal the formation of coke in agglomerates that span length scales from tens of nanometers to atomic clusters with a median size of 30–60 13C atoms. These clusters correlate with local increases in Brønsted acid sitemore » density, demonstrating that the formation of the first deactivating coke precursor molecules occurs in nanoscopic regions enriched in aluminum. Here, this nanoscale correlation underscores the importance of carefully engineering materials to suppress detrimental coke formation.« less

  7. Synthesis of zeolite NaA membrane from fused fly ash extract.

    PubMed

    Ameh, Alechine E; Musyoka, Nicholas M; Fatoba, Ojo O; Syrtsova, Daria A; Teplyakov, Vladimir V; Petrik, Leslie F

    2016-01-01

    Zeolite-NaA membranes were synthesized from an extract of fused South African fly ash on a porous titanium support by a secondary growth method. The influence of the synthesis molar regime on the formation of zeolite NaA membrane layer was investigated. Two synthesis mixtures were generated by adding either aluminium hydroxide or sodium aluminate to the fused fly ash extract. The feedstock material and the synthesized membranes were characterized by X-diffraction (XRD), scanning electron microscopy (SEM) and X-ray fluorescence spectroscopy (XRF). It was found by XRD and SEM that the cubic crystals of a typical zeolite NaA with a dense intergrown layer was formed on the porous Ti support. The study shows that the source of Al used had an effect on the membrane integrity as sodium aluminate provided the appropriate amount of Na(+) to form a coherent membrane of zeolite NaA, whereas aluminium hydroxide did not. Morphological, the single hydrothermal stage seeded support formed an interlocked array of zeolite NaA particles with neighbouring crystals. Also, a robust, continuous and well-intergrown zeolite NaA membrane was formed with neighbouring crystals of zeolite fused to each other after the multiple stage synthesis. The synthesized membrane was permeable to He (6.0 × 10(6) L m(-2)h(-1) atm(-1)) and CO2 (5.6 × 10(6) L m(-2)h(-1) atm(-1)), which indicate that the layer of the membrane was firmly attached to the porous Ti support. Membrane selectivity was maintained showing membrane integrity with permselectivity of 1.1, showing that a waste feedstock, fly ash, could be utilized for preparing robust zeolite NaA membranes on Ti support.

  8. Rapid screening of the antimicrobial efficacy of Ag zeolites.

    PubMed

    Tosheva, L; Belkhair, S; Gackowski, M; Malic, S; Al-Shanti, N; Verran, J

    2017-09-01

    A semi-quantitative screening method was used to compare the killing efficacy of Ag zeolites against bacteria and yeast as a function of the zeolite type, crystal size and concentration. The method, which substantially reduced labor, consumables and waste and provided an excellent preliminary screen, was further validated by quantitative plate count experiments. Two pairs of zeolite X and zeolite beta with different sizes (ca. 200nm and 2μm for zeolite X and ca. 250 and 500nm for zeolite beta) were tested against Escherichia coli (E. coli) and Candida albicans (C. albicans) at concentrations in the range 0.05-0.5mgml -1 . Reduction of the zeolite crystal size resulted in a decrease in the killing efficacy against both microorganisms. The semi-quantitative tests allowed convenient optimization of the zeolite concentrations to achieve targeted killing times. Zeolite beta samples showed higher activity compared to zeolite X despite their lower Ag content, which was attributed to the higher concentration of silver released from zeolite beta samples. Cytotoxicity measurements using peripheral blood mononuclear cells (PBMCs) indicated that Ag zeolite X was more toxic than Ag zeolite beta. However, the trends for the dependence of cytotoxicity on zeolite crystal size at different zeolite concentrations were different for the two zeolites and no general conclusions about zeolite cytotoxicity could be drawn from these experiments. This result indicates a complex relationship, requiring the necessity for individual cytotoxicity measurements for all antimicrobial applications based on the use of zeolites. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Design and fabrication of zeolite macro- and micromembranes

    NASA Astrophysics Data System (ADS)

    Chau, Lik Hang Joseph

    2001-07-01

    The chemical nature of the support surface influences zeolite nucleation, crystal growth and elm adhesion. It had been demonstrated that chemical modification of support surface can significantly alter the zeolite film and has a good potential for large-scale applications for zeolite membrane production. The incorporation of titanium and vanadium metal ions into the structural framework of MFI zeolite imparts the material with catalytic properties. The effects of silica and metal (i.e., Ti and V) content, template concentration and temperature on the zeolite membrane growth and morphology were investigated. Single-gas permeation experiments were conducted for noble gases (He and Ar), inorganic gases (H2, N2, SF6) and hydrocarbons (methane, n-C4, i-C4) to determine the separation performance of these membranes. Using a new fabrication method based on microelectronic fabrication and zeolite thin film technologies, complex microchannel geometry and network (<5 mum), as well as zeolite arrays (<10 mum) were successfully fabricated onto highly orientated supported zeolite films. The zeolite micropatterns were stable even after repeated thermal cycling between 303 K and 873 K for prolonged periods of time. This work also demonstrates that zeolites (i.e., Sil-1, ZSM-5 and TS-1) can be employed as catalyst, membrane or structural materials in miniature chemical devices. Traditional semiconductor fabrication technology was employed in micromachining the device architecture. Four strategies for the manufacture of zeolite catalytic microreactors were discussed: zeolite powder coating, uniform zeolite film growth, localized zeolite growth, and etching of zeolite-silicon composite film growth inhibitors. Silicalite-1 was also prepared as free-standing membrane for zeolite membrane microseparators.

  10. Bubble formed as a result of a Zeolite Crystal Growth experiment in the U.S. Laboratory

    NASA Image and Video Library

    2002-12-14

    ISS006-E-08835 (14 December 2002) --- View of a bubble formed as a result of a Zeolite Crystal Growth (ZCG) experiment in the Destiny laboratory on the International Space Station (ISS). Expedition Six Commander Kenneth D. Bowersox used a Space Station drill to mix 12 Zeolite samples in clear tubes. Scientists on the ground watching on TV noticed bubbles in the samples. Bowersox used a modified mixing procedure to process autoclaves to isolate bubbles. He re-inserted the samples in the ZCG furnace in Express Rack 2 in the U.S. laboratory/Destiny. This experiment has shown that the bubbles could cause larger number of smaller deformed crystals to grow. Bowersox rotated the samples so that the heavier fluid was thrown to the outside while the lighter bubbles stayed on the inside.

  11. Bubble formed as a result of a Zeolite Crystal Growth experiment in the U.S. Laboratory

    NASA Image and Video Library

    2002-12-14

    ISS006-E-08778 (14 December 2002) --- View of a bubble formed as a result of a Zeolite Crystal Growth (ZCG) experiment in the Destiny laboratory on the International Space Station (ISS). Expedition Six Commander Kenneth D. Bowersox used a Space Station drill to mix 12 Zeolite samples in clear tubes. Scientists on the ground watching on TV noticed bubbles in the samples. Bowersox used a modified mixing procedure to process autoclaves to isolate bubbles. He re-inserted the samples in the ZCG furnace in Express Rack 2 in the U.S. laboratory/Destiny. This experiment has shown that the bubbles could cause larger number of smaller deformed crystals to grow. Bowersox rotated the samples so that the heavier fluid was thrown to the outside while the lighter bubbles stayed on the inside.

  12. Bubble formed as a result of a Zeolite Crystal Growth experiment in the U.S. Laboratory

    NASA Image and Video Library

    2002-12-14

    ISS006-E-08775 (14 December 2002) --- View of a bubble formed as a result of a Zeolite Crystal Growth (ZCG) experiment in the Destiny laboratory on the International Space Station (ISS). Expedition Six Commander Kenneth D. Bowersox used a Space Station drill to mix 12 Zeolite samples in clear tubes. Scientists on the ground watching on TV noticed bubbles in the samples. Bowersox used a modified mixing procedure to process autoclaves to isolate bubbles. He re-inserted the samples in the ZCG furnace in Express Rack 2 in the U.S. laboratory/Destiny. This experiment has shown that the bubbles could cause larger number of smaller deformed crystals to grow. Bowersox rotated the samples so that the heavier fluid was thrown to the outside while the lighter bubbles stayed on the inside.

  13. Bubble formed as a result of a Zeolite Crystal Growth experiment in the U.S. Laboratory

    NASA Image and Video Library

    2002-12-14

    ISS006-E-08773 (14 December 2002) --- View of a bubble formed as a result of a Zeolite Crystal Growth (ZCG) experiment in the Destiny laboratory on the International Space Station (ISS). Expedition Six Commander Kenneth D. Bowersox used a Space Station drill to mix 12 Zeolite samples in clear tubes. Scientists on the ground watching on TV noticed bubbles in the samples. Bowersox used a modified mixing procedure to process autoclaves to isolate bubbles. He re-inserted the samples in the ZCG furnace in Express Rack 2 in the U.S. laboratory/Destiny. This experiment has shown that the bubbles could cause larger number of smaller deformed crystals to grow. Bowersox rotated the samples so that the heavier fluid was thrown to the outside while the lighter bubbles stayed on the inside.

  14. Bubble formed as a result of a Zeolite Crystal Growth experiment in the U.S. Laboratory

    NASA Image and Video Library

    2002-12-14

    ISS006-E-08822 (14 December 2002) --- View of a bubble formed as a result of a Zeolite Crystal Growth (ZCG) experiment in the Destiny laboratory on the International Space Station (ISS). Expedition Six Commander Kenneth D. Bowersox used a Space Station drill to mix 12 Zeolite samples in clear tubes. Scientists on the ground watching on TV noticed bubbles in the samples. Bowersox used a modified mixing procedure to process autoclaves to isolate bubbles. He re-inserted the samples in the ZCG furnace in Express Rack 2 in the U.S. laboratory/Destiny. This experiment has shown that the bubbles could cause larger number of smaller deformed crystals to grow. Bowersox rotated the samples so that the heavier fluid was thrown to the outside while the lighter bubbles stayed on the inside.

  15. Bubble formed as a result of a Zeolite Crystal Growth experiment in the U.S. Laboratory

    NASA Image and Video Library

    2002-12-14

    ISS006-E-08831 (14 December 2002) --- View of a bubble formed as a result of a Zeolite Crystal Growth (ZCG) experiment in the Destiny laboratory on the International Space Station (ISS). Expedition Six Commander Kenneth D. Bowersox used a Space Station drill to mix 12 Zeolite samples in clear tubes. Scientists on the ground watching on TV noticed bubbles in the samples. Bowersox used a modified mixing procedure to process autoclaves to isolate bubbles. He re-inserted the samples in the ZCG furnace in Express Rack 2 in the U.S. laboratory/Destiny. This experiment has shown that the bubbles could cause larger number of smaller deformed crystals to grow. Bowersox rotated the samples so that the heavier fluid was thrown to the outside while the lighter bubbles stayed on the inside.

  16. Bubble formed as a result of a Zeolite Crystal Growth experiment in the U.S. Laboratory

    NASA Image and Video Library

    2002-12-14

    ISS006-E-08805 (14 December 2002) --- View of a bubble formed as a result of a Zeolite Crystal Growth (ZCG) experiment in the Destiny laboratory on the International Space Station (ISS). Expedition Six Commander Kenneth D. Bowersox used a Space Station drill to mix 12 Zeolite samples in clear tubes. Scientists on the ground watching on TV noticed bubbles in the samples. Bowersox used a modified mixing procedure to process autoclaves to isolate bubbles. He re-inserted the samples in the ZCG furnace in Express Rack 2 in the U.S. laboratory/Destiny. This experiment has shown that the bubbles could cause larger number of smaller deformed crystals to grow. Bowersox rotated the samples so that the heavier fluid was thrown to the outside while the lighter bubbles stayed on the inside.

  17. Bubble formed as a result of a Zeolite Crystal Growth experiment in the U.S. Laboratory

    NASA Image and Video Library

    2002-12-14

    ISS006-E-08784 (14 December 2002) --- View of a bubble formed as a result of a Zeolite Crystal Growth (ZCG) experiment in the Destiny laboratory on the International Space Station (ISS). Expedition Six Commander Kenneth D. Bowersox used a Space Station drill to mix 12 Zeolite samples in clear tubes. Scientists on the ground watching on TV noticed bubbles in the samples. Bowersox used a modified mixing procedure to process autoclaves to isolate bubbles. He re-inserted the samples in the ZCG furnace in Express Rack 2 in the U.S. laboratory/Destiny. This experiment has shown that the bubbles could cause larger number of smaller deformed crystals to grow. Bowersox rotated the samples so that the heavier fluid was thrown to the outside while the lighter bubbles stayed on the inside.

  18. Bubble formed as a result of a Zeolite Crystal Growth experiment in the U.S. Laboratory

    NASA Image and Video Library

    2002-12-14

    ISS006-E-08836 (14 December 2002) --- View of a bubble formed as a result of a Zeolite Crystal Growth (ZCG) experiment in the Destiny laboratory on the International Space Station (ISS). Expedition Six Commander Kenneth D. Bowersox used a Space Station drill to mix 12 Zeolite samples in clear tubes. Scientists on the ground watching on TV noticed bubbles in the samples. Bowersox used a modified mixing procedure to process autoclaves to isolate bubbles. He re-inserted the samples in the ZCG furnace in Express Rack 2 in the U.S. laboratory/Destiny. This experiment has shown that the bubbles could cause larger number of smaller deformed crystals to grow. Bowersox rotated the samples so that the heavier fluid was thrown to the outside while the lighter bubbles stayed on the inside.

  19. Bubble formed as a result of a Zeolite Crystal Growth experiment in the U.S. Laboratory

    NASA Image and Video Library

    2002-12-14

    ISS006-E-08799 (14 December 2002) --- View of a bubble formed as a result of a Zeolite Crystal Growth (ZCG) experiment in the Destiny laboratory on the International Space Station (ISS). Expedition Six Commander Kenneth D. Bowersox used a Space Station drill to mix 12 Zeolite samples in clear tubes. Scientists on the ground watching on TV noticed bubbles in the samples. Bowersox used a modified mixing procedure to process autoclaves to isolate bubbles. He re-inserted the samples in the ZCG furnace in Express Rack 2 in the U.S. laboratory/Destiny. This experiment has shown that the bubbles could cause larger number of smaller deformed crystals to grow. Bowersox rotated the samples so that the heavier fluid was thrown to the outside while the lighter bubbles stayed on the inside.

  20. Adsorption Device Based on a Langatate Crystal Microbalance for High Temperature High Pressure Gas Adsorption in Zeolite H-ZSM-5.

    PubMed

    Ding, Wenjin; Baracchini, Giulia; Klumpp, Michael; Schwieger, Wilhelm; Dittmeyer, Roland

    2016-08-25

    We present a high-temperature and high-pressure gas adsorption measurement device based on a high-frequency oscillating microbalance (5 MHz langatate crystal microbalance, LCM) and its use for gas adsorption measurements in zeolite H-ZSM-5. Prior to the adsorption measurements, zeolite H-ZSM-5 crystals were synthesized on the gold electrode in the center of the LCM, without covering the connection points of the gold electrodes to the oscillator, by the steam-assisted crystallization (SAC) method, so that the zeolite crystals remain attached to the oscillating microbalance while keeping good electroconductivity of the LCM during the adsorption measurements. Compared to a conventional quartz crystal microbalance (QCM) which is limited to temperatures below 80 °C, the LCM can realize the adsorption measurements in principle at temperatures as high as 200-300 °C (i.e., at or close to the reaction temperature of the target application of one-stage DME synthesis from the synthesis gas), owing to the absence of crystalline-phase transitions up to its melting point (1,470 °C). The system was applied to investigate the adsorption of CO2, H2O, methanol and dimethyl ether (DME), each in the gas phase, on zeolite H-ZSM-5 in the temperature and pressure range of 50-150 °C and 0-18 bar, respectively. The results showed that the adsorption isotherms of these gases in H-ZSM-5 can be well fitted by Langmuir-type adsorption isotherms. Furthermore, the determined adsorption parameters, i.e., adsorption capacities, adsorption enthalpies, and adsorption entropies, compare well to literature data. In this work, the results for CO2 are shown as an example.

  1. Adsorption Device Based on a Langatate Crystal Microbalance for High Temperature High Pressure Gas Adsorption in Zeolite H-ZSM-5

    PubMed Central

    Ding, Wenjin; Baracchini, Giulia; Klumpp, Michael; Schwieger, Wilhelm; Dittmeyer, Roland

    2016-01-01

    We present a high-temperature and high-pressure gas adsorption measurement device based on a high-frequency oscillating microbalance (5 MHz langatate crystal microbalance, LCM) and its use for gas adsorption measurements in zeolite H-ZSM-5. Prior to the adsorption measurements, zeolite H-ZSM-5 crystals were synthesized on the gold electrode in the center of the LCM, without covering the connection points of the gold electrodes to the oscillator, by the steam-assisted crystallization (SAC) method, so that the zeolite crystals remain attached to the oscillating microbalance while keeping good electroconductivity of the LCM during the adsorption measurements. Compared to a conventional quartz crystal microbalance (QCM) which is limited to temperatures below 80 °C, the LCM can realize the adsorption measurements in principle at temperatures as high as 200-300 °C (i.e., at or close to the reaction temperature of the target application of one-stage DME synthesis from the synthesis gas), owing to the absence of crystalline-phase transitions up to its melting point (1,470 °C). The system was applied to investigate the adsorption of CO2, H2O, methanol and dimethyl ether (DME), each in the gas phase, on zeolite H-ZSM-5 in the temperature and pressure range of 50-150 °C and 0-18 bar, respectively. The results showed that the adsorption isotherms of these gases in H-ZSM-5 can be well fitted by Langmuir-type adsorption isotherms. Furthermore, the determined adsorption parameters, i.e., adsorption capacities, adsorption enthalpies, and adsorption entropies, compare well to literature data. In this work, the results for CO2 are shown as an example. PMID:27585356

  2. Hydrothermal synthesis of free-template zeolite T from kaolin

    NASA Astrophysics Data System (ADS)

    Arshad, Sazmal E.; Yusslee, Eddy F.; Rahman, Md. Lutfor; Sarkar, Shaheen M.; Patuwan, Siti Z.

    2017-12-01

    Free-template zeolite T crystals were synthesized via hydrothermal synthesis by utilizing the activated kaolin as silica and alumina source, with the molar composition of 1 SiO2: 0.04 Al2O3: 0.26 Na2O: 0.09 K2O: 14 H2O. Observation of the formation of free-template zeolite crystals were done at temperature 90°C, 100 °C and 110 °C respectively. It was therefore determined that during the 120 h of the synthesis at 90 °C, zeolite T nucleated and formed a first competitive phase with zeolite L. As temperature increases to 100 °C, zeolite T presented itself as a major phase in the system at time 168 h. Subsequently, development of Zeolite T with second competitive phase of zeolite W was observed at temperature 110 °C. In this study, XRD and SEM instruments were used to monitor the behavior of zeolite T crystals with respect of temperature and time. By using natural resource of kaolin clay as a starting material, this paper hence aims to provide new findings in synthesis of zeolite T using low energy consumption and low production cost.

  3. Controllable cyanation of carbon-hydrogen bonds by zeolite crystals over manganese oxide catalyst

    PubMed Central

    Wang, Liang; Wang, Guoxiong; Zhang, Jian; Bian, Chaoqun; Meng, Xiangju; Xiao, Feng-Shou

    2017-01-01

    The synthesis of organic nitriles without using toxic cyanides is in great demand but challenging to make. Here we report an environmentally benign and cost-efficient synthesis of nitriles from the direct oxidative cyanation of primary carbon-hydrogen bonds with easily available molecular oxygen and urea. The key to this success is to design and synthesize manganese oxide catalysts fixed inside zeolite crystals, forming a manganese oxide catalyst with zeolite sheath (MnOx@S-1), which exhibits high selectivity for producing nitriles by efficiently facilitating the oxidative cyanation reaction and hindering the side hydration reaction. The work delineates a sustainable strategy for synthesizing nitriles while avoiding conventional toxic cyanide, which might open a new avenue for selective transformation of carbon-hydrogen bonds. PMID:28504259

  4. Solvent-Free Synthesis of Zeolites: Mechanism and Utility.

    PubMed

    Wu, Qinming; Meng, Xiangju; Gao, Xionghou; Xiao, Feng-Shou

    2018-05-08

    Zeolites have been extensively studied for years in different areas of chemical industry, such as shape selective catalysis, ion-exchange, and gas adsorption and separation. Generally, zeolites are prepared from solvothermal synthesis in the presence of a large amounts of solvents such as water and alcohols in sealed autoclaves under autogenous pressure. Water has been regarded as essential to synthesize zeolites for fast mass transfer of reactants, but it occupies a large space in autoclaves, which greatly reduces the yield of zeolite products. Furthermore, polluted wastes and relatively high pressure due to the presence of water solvent in the synthesis also leads to environmental and safety issues. Recently, inspired by great benefits of solvent-free synthesis, including the environmental concerns, energy consumption, safety, and economic cost, researchers continually challenge the rationale of the solvent and reconsider the age-old question "Do we actually need solvents at all in zeolite synthesis?" In this Account, we briefly summarize our efforts to rationally synthesize zeolites via a solvent-free route. Our research demonstrates that a series of silica, aluminosilicate, and aluminophosphate-based zeolites can be successfully prepared by mixing, grinding, and heating starting solid materials under solvent-free conditions. Combining an organotemplate-free synthesis with a solvent-free approach maximizes the advantages resulting in a more sustainable synthetic route, which avoids using toxic and costly organic templates and the formation of harmful gases by calcination of organic templates at high temperature. Furthermore, new insights into the solvent-free crystallization process of zeolites have been provided by modern techniques such as NMR and UV-Raman spectroscopy, which should be helpful in designing new zeolite structures and developing novel routes for synthesis of zeolites. The role of water and the vital intermediates during the crystallization of

  5. Ultra-selective high-flux membranes from directly synthesized zeolite nanosheets

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

    Jeon, Mi Young; Kim, Donghun; Kumar, Prashant

    A zeolite with structure type MFI is an aluminosilicate or silicate material that has a three-dimensionally connected pore network, which enables molecular recognition in the size range 0.5-0.6 nm. These micropore dimensions are relevant for many valuable chemical intermediates, and therefore MFI-type zeolites are widely used in the chemical industry as selective catalysts or adsorbents. As with all zeolites, strategies to tailor them for specific applications include controlling their crystal size and shape. Nanometre-thick MFI crystals (nanosheets) have been introduced in pillared and self-pillared (intergrown) architectures, offering improved mass-transfer characteristics for certain adsorption and catalysis applications. Moreover, single (non-intergrown andmore » nonlayered) nanosheets have been used to prepare thin membranes that could be used to improve the energy efficiency of separation processes. However, until now, single MFI nanosheets have been prepared using a multi-step approach based on the exfoliation of layered MFI9,15, followed by centrifugation to remove non-exfoliated particles. This top-down method is time-consuming, costly and low-yield and it produces fragmented nanosheets with submicrometre lateral dimensions. Alternatively, direct (bottom-up) synthesis could produce high-aspect-ratio zeolite nanosheets, with improved yield and at lower cost. Here we use a nanocrystal-seeded growth method triggered by a single rotational intergrowth to synthesize high-aspect-ratio MFI nanosheets with a thickness of 5 nanometres (2.5 unit cells). These high-aspect-ratio nanosheets allow the fabrication of thin and defect-free coatings that effectively cover porous substrates. Finally, these coatings can be intergrown to produce high-flux and ultra-selective MFI membranes that compare favourably with other MFI membranes prepared from existing MFI materials (such as exfoliated nanosheets or nanocrystals).« less

  6. Ultra-selective high-flux membranes from directly synthesized zeolite nanosheets

    DOE PAGES

    Jeon, Mi Young; Kim, Donghun; Kumar, Prashant; ...

    2017-03-15

    A zeolite with structure type MFI is an aluminosilicate or silicate material that has a three-dimensionally connected pore network, which enables molecular recognition in the size range 0.5-0.6 nm. These micropore dimensions are relevant for many valuable chemical intermediates, and therefore MFI-type zeolites are widely used in the chemical industry as selective catalysts or adsorbents. As with all zeolites, strategies to tailor them for specific applications include controlling their crystal size and shape. Nanometre-thick MFI crystals (nanosheets) have been introduced in pillared and self-pillared (intergrown) architectures, offering improved mass-transfer characteristics for certain adsorption and catalysis applications. Moreover, single (non-intergrown andmore » nonlayered) nanosheets have been used to prepare thin membranes that could be used to improve the energy efficiency of separation processes. However, until now, single MFI nanosheets have been prepared using a multi-step approach based on the exfoliation of layered MFI9,15, followed by centrifugation to remove non-exfoliated particles. This top-down method is time-consuming, costly and low-yield and it produces fragmented nanosheets with submicrometre lateral dimensions. Alternatively, direct (bottom-up) synthesis could produce high-aspect-ratio zeolite nanosheets, with improved yield and at lower cost. Here we use a nanocrystal-seeded growth method triggered by a single rotational intergrowth to synthesize high-aspect-ratio MFI nanosheets with a thickness of 5 nanometres (2.5 unit cells). These high-aspect-ratio nanosheets allow the fabrication of thin and defect-free coatings that effectively cover porous substrates. Finally, these coatings can be intergrown to produce high-flux and ultra-selective MFI membranes that compare favourably with other MFI membranes prepared from existing MFI materials (such as exfoliated nanosheets or nanocrystals).« less

  7. Large zeolites - Why and how to grow in space

    NASA Technical Reports Server (NTRS)

    Sacco, Albert, Jr.

    1991-01-01

    The growth of zeolite crystals which are considered to be the most valuable catalytic and adsorbent materials of the chemical processing industry are discussed. It is proposed to use triethanolamine as a nucleation control agent to control the time release of Al in a zeolite A solution and to increase the average and maximum crystal size by 25-50 times. Large zeolites could be utilized to make membranes for reactors/separators which will substantially increase their efficiency.

  8. A multistep single-crystal-to-single-crystal bromodiacetylene dimerization

    NASA Astrophysics Data System (ADS)

    Hoheisel, Tobias N.; Schrettl, Stephen; Marty, Roman; Todorova, Tanya K.; Corminboeuf, Clémence; Sienkiewicz, Andrzej; Scopelliti, Rosario; Schweizer, W. Bernd; Frauenrath, Holger

    2013-04-01

    Packing constraints and precise placement of functional groups are the reason that organic molecules in the crystalline state often display unusual physical or chemical properties not observed in solution. Here we report a single-crystal-to-single-crystal dimerization of a bromodiacetylene that involves unusually large atom displacements as well as the cleavage and formation of several bonds. Density functional theory computations support a mechanism in which the dimerization is initiated by a [2 + 1] photocycloaddition favoured by the nature of carbon-carbon short contacts in the crystal structure. The reaction proceeded up to the theoretical degree of conversion without loss of crystallinity, and it was also performed on a preparative scale with good yield. Moreover, it represents the first synthetic pathway to (E)-1,2-dibromo-1,2-diethynylethenes, which could serve as synthetic intermediates for the preparation of molecular carbon scaffolds. Our findings both extend the scope of single-crystal-to-single-crystal reactions and highlight their potential as a synthetic tool for complex transformations.

  9. Nanoscale Chemical Imaging of Zeolites Using Atom Probe Tomography.

    PubMed

    Weckhuysen, Bert Marc; Schmidt, Joel; Peng, Linqing; Poplawsky, Jonathan

    2018-05-02

    Understanding structure-composition-property relationships in zeolite-based materials is critical to engineering improved solid catalysts. However, this can be difficult to realize as even single zeolite crystals can exhibit heterogeneities spanning several orders of magnitude, with consequences for e.g. reactivity, diffusion as well as stability. Great progress has been made in characterizing these porous solids using tomographic techniques, though each method has an ultimate spatial resolution limitation. Atom Probe Tomography (APT) is the only technique so far capable of producing 3-D compositional reconstructions with sub-nm-scale resolution, and has only recently been applied to zeolite-based catalysts. Herein, we discuss the use of APT to study zeolites, including the critical aspects of sample preparation, data collection, assignment of mass spectral peaks including the predominant CO peak, the limitations of spatial resolution for the recovery of crystallographic information, and proper data analysis. All sections are illustrated with examples from recent literature, as well as previously unpublished data and analyses to demonstrate practical strategies to overcome potential pitfalls in applying APT to zeolites, thereby highlighting new insights gained from the APT method. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. High-resolution single-molecule fluorescence imaging of zeolite aggregates within real-life fluid catalytic cracking particles.

    PubMed

    Ristanović, Zoran; Kerssens, Marleen M; Kubarev, Alexey V; Hendriks, Frank C; Dedecker, Peter; Hofkens, Johan; Roeffaers, Maarten B J; Weckhuysen, Bert M

    2015-02-02

    Fluid catalytic cracking (FCC) is a major process in oil refineries to produce gasoline and base chemicals from crude oil fractions. The spatial distribution and acidity of zeolite aggregates embedded within the 50-150 μm-sized FCC spheres heavily influence their catalytic performance. Single-molecule fluorescence-based imaging methods, namely nanometer accuracy by stochastic chemical reactions (NASCA) and super-resolution optical fluctuation imaging (SOFI) were used to study the catalytic activity of sub-micrometer zeolite ZSM-5 domains within real-life FCC catalyst particles. The formation of fluorescent product molecules taking place at Brønsted acid sites was monitored with single turnover sensitivity and high spatiotemporal resolution, providing detailed insight in dispersion and catalytic activity of zeolite ZSM-5 aggregates. The results point towards substantial differences in turnover frequencies between the zeolite aggregates, revealing significant intraparticle heterogeneities in Brønsted reactivity. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Advances in nanosized zeolites

    NASA Astrophysics Data System (ADS)

    Mintova, Svetlana; Gilson, Jean-Pierre; Valtchev, Valentin

    2013-07-01

    This review highlights recent developments in the synthesis of nanosized zeolites. The strategies available for their preparation (organic-template assisted, organic-template free, and alternative procedures) are discussed. Major breakthroughs achieved by the so-called zeolite crystal engineering and encompass items such as mastering and using the physicochemical properties of the precursor synthesis gel/suspension, optimizing the use of silicon and aluminium precursor sources, the rational use of organic templates and structure-directing inorganic cations, and careful adjustment of synthesis conditions (temperature, pressure, time, heating processes from conventional to microwave and sonication) are addressed. An on-going broad and deep fundamental understanding of the crystallization process, explaining the influence of all variables of this complex set of reactions, underpins an even more rational design of nanosized zeolites with exceptional properties. Finally, the advantages and limitations of these methods are addressed with particular attention to their industrial prospects and utilization in existing and advanced applications.

  12. Effects of Coke Deposits on the Catalytic Performance of Large Zeolite H-ZSM-5 Crystals during Alcohol-to-Hydrocarbon Reactions as Investigated by a Combination of Optical Spectroscopy and Microscopy

    PubMed Central

    Nordvang, Emily C; Borodina, Elena; Ruiz-Martínez, Javier; Fehrmann, Rasmus; Weckhuysen, Bert M

    2015-01-01

    The catalytic activity of large zeolite H-ZSM-5 crystals in methanol (MTO) and ethanol-to-olefins (ETO) conversions was investigated and, using operando UV/Vis measurements, the catalytic activity and deactivation was correlated with the formation of coke. These findings were related to in situ single crystal UV/Vis and confocal fluorescence micro-spectroscopy, allowing the observation of the spatiotemporal formation of intermediates and coke species during the MTO and ETO conversions. It was observed that rapid deactivation at elevated temperatures was due to the fast formation of aromatics at the periphery of the H-ZSM-5 crystals, which are transformed into more poly-aromatic coke species at the external surface, preventing the diffusion of reactants and products into and out of the H-ZSM-5 crystal. Furthermore, we were able to correlate the operando UV/Vis spectroscopy results observed during catalytic testing with the single crystal in situ results. PMID:26463581

  13. Recent advances in secondary ion mass spectrometry of solid acid catalysts: large zeolite crystals under bombardment.

    PubMed

    Hofmann, Jan P; Rohnke, Marcus; Weckhuysen, Bert M

    2014-03-28

    This Perspective aims to inform the heterogeneous catalysis and materials science community about the recent advances in Time-of-Flight-Secondary Ion Mass Spectrometry (ToF-SIMS) to characterize catalytic solids by taking large model H-ZSM-5 zeolite crystals as a showcase system. SIMS-based techniques have been explored in the 1980-1990's to study porous catalyst materials but, due to their limited spectral and spatiotemporal resolution, there was no real major breakthrough at that time. The technical advancements in SIMS instruments, namely improved ion gun design and new mass analyser concepts, nowadays allow for a much more detailed analysis of surface species relevant to catalytic action. Imaging with high mass and lateral resolution, determination of fragment ion patterns, novel sputter ion concepts as well as new mass analysers (e.g. ToF, FTICR) are just a few novelties, which will lead to new fundamental insight from SIMS analysis of heterogeneous catalysts. The Perspective article ends with an outlook on instrumental innovations and their potential use for catalytic systems other than zeolite crystals.

  14. Selective synthesis of FAU-type zeolites

    NASA Astrophysics Data System (ADS)

    Garcia, Gustavo; Cabrera, Saúl; Hedlund, Jonas; Mouzon, Johanne

    2018-05-01

    In the present work, parameters influencing the selectivity of the synthesis of FAU-zeolites from diatomite were studied. The final products after varying synthesis time were characterized by scanning electron microscopy, energy dispersive spectroscopy, X-ray diffraction and gas adsorption. It was found that high concentrations of NaCl could completely inhibit the formation of zeolite P, which otherwise usually forms as soon as maximum FAU crystallinity is reached. In the presence of NaCl, the FAU crystals were stable for extended time after completed crystallization of FAU before formation of sodalite. It was also found that addition of NaCl barely changed the crystallization kinetics of FAU zeolite and only reduced the final FAU particle size and SiO2/Al2O3 ratio slightly. Other salts containing either Na or Cl were also investigated. Our results suggest that there is a synergistic effect between Na+ and Cl-. This is attributed to the formation of (Na4Cl)3+ clusters that stabilize the sodalite cages. This new finding may be used to increase the selectivity of syntheses leading to FAU-zeolites and avoid the formation of undesirable by-products, especially if impure natural sources of aluminosilica are used.

  15. Synthesis and Characterization of Zeolite Na-Y and Its Conversion to the Solid Acid Zeolite H-Y

    ERIC Educational Resources Information Center

    Warner, Terence E.; Klokker, Mads Galsgaard; Nielsen, Ulla Gro

    2017-01-01

    Zeolite Y has an iconic crystal structure, but more importantly, the hydrogen modification zeolite H-Y is the classic example of a solid acid which is used extensively as a catalyst in the oil industry. This metastable compound cannot be synthesized directly, which creates an opportunity to discuss various preparative strategies with the students,…

  16. 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.

  17. Thermally programmable gas storage and release in single crystals of an organic van der Waals host.

    PubMed

    Enright, Gary D; Udachin, Konstantin A; Moudrakovski, Igor L; Ripmeester, John A

    2003-08-20

    A single crystal of a low density form of guest-free p-tert-butylcalix[4]arene can take up and release small guest molecules by controlling the temperature and pressure without changing the structure. Using NMR spectroscopy with flowing hyperpolarized xenon, we have shown that at room temperature access of xenon to the pore system is difficult, whereas it is relatively easy at 100 degrees C. There are good prospects for simple van der Waals materials such as the title material to be used as programmable zeolite mimics.

  18. Zeolite A imidazolate frameworks

    NASA Astrophysics Data System (ADS)

    Hayashi, Hideki; Côté, Adrien P.; Furukawa, Hiroyasu; O'Keeffe, Michael; Yaghi, Omar M.

    2007-07-01

    Faujasite (FAU) and zeolite A (LTA) are technologically important porous zeolites (aluminosilicates) because of their extensive use in petroleum cracking and water softening. Introducing organic units and transition metals into the backbone of these types of zeolite allows us to expand their pore structures, enhance their functionality and access new applications. The invention of metal-organic frameworks and zeolitic imidazolate frameworks (ZIFs) has provided materials based on simple zeolite structures where only one type of cage is present. However, so far, no metal-organic analogues based on FAU or LTA topologies exist owing to the difficulty imposed by the presence of two types of large cage (super- and β-cages for FAU, α- and β-cages for LTA). Here, we have identified a strategy to produce an LTA imidazolate framework in which both the link geometry and link-link interactions play a decisive structure-directing role. We describe the synthesis and crystal structures of three porous ZIFs that are expanded analogues of zeolite A; their cage walls are functionalized, and their metal ions can be changed without changing the underlying LTA topology. Hydrogen, methane, carbon dioxide and argon gas adsorption isotherms are reported and the selectivity of this material for carbon dioxide over methane is demonstrated.

  19. Zeolite A imidazolate frameworks.

    PubMed

    Hayashi, Hideki; Côté, Adrien P; Furukawa, Hiroyasu; O'Keeffe, Michael; Yaghi, Omar M

    2007-07-01

    Faujasite (FAU) and zeolite A (LTA) are technologically important porous zeolites (aluminosilicates) because of their extensive use in petroleum cracking and water softening. Introducing organic units and transition metals into the backbone of these types of zeolite allows us to expand their pore structures, enhance their functionality and access new applications. The invention of metal-organic frameworks and zeolitic imidazolate frameworks (ZIFs) has provided materials based on simple zeolite structures where only one type of cage is present. However, so far, no metal-organic analogues based on FAU or LTA topologies exist owing to the difficulty imposed by the presence of two types of large cage (super- and beta-cages for FAU, alpha- and beta-cages for LTA). Here, we have identified a strategy to produce an LTA imidazolate framework in which both the link geometry and link-link interactions play a decisive structure-directing role. We describe the synthesis and crystal structures of three porous ZIFs that are expanded analogues of zeolite A; their cage walls are functionalized, and their metal ions can be changed without changing the underlying LTA topology. Hydrogen, methane, carbon dioxide and argon gas adsorption isotherms are reported and the selectivity of this material for carbon dioxide over methane is demonstrated.

  20. Hydrogen Separation by Natural Zeolite Composite Membranes: Single and Multicomponent Gas Transport.

    PubMed

    Farjoo, Afrooz; Kuznicki, Steve M; Sadrzadeh, Mohtada

    2017-10-06

    Single and multicomponent gas permeation tests were used to evaluate the performance of metal-supported clinoptilolite membranes. The efficiency of hydrogen separation from lower hydrocarbons (methane, ethane, and ethylene) was studied within the temperature and pressure ranges of 25-600 °C and 110-160 kPa, respectively. The hydrogen separation factor was found to reduce noticeably in the gas mixture compared with single gas experiments at 25 °C. The difference between the single and multicomponent gas results decreased as the temperature increased to higher than 300 °C, which is when the competitive adsorption-diffusion mechanism was replaced by Knudsen diffusion or activated diffusion mechanisms. To evaluate the effect of gas adsorption, the zeolite surface isotherms of each gas in the mixture were obtained from 25 °C to 600 °C. The results indicated negligible adsorption of individual gases at temperatures higher than 300 °C. Increasing the feed pressure resulted in a higher separation efficiency for the individual gases compared with the multicomponent mixture, due to the governing effect of the adsorptive mechanism. This study provides valuable insight into the application of natural zeolites for the separation of hydrogen from a mixture of hydrocarbons.

  1. Standard Reference Material (SRM 1990) for Single Crystal Diffractometer Alignment

    USGS Publications Warehouse

    Wong-Ng, W.; Siegrist, T.; DeTitta, G.T.; Finger, L.W.; Evans, H.T.; Gabe, E.J.; Enright, G.D.; Armstrong, J.T.; Levenson, M.; Cook, L.P.; Hubbard, C.R.

    2001-01-01

    An international project was successfully completed which involved two major undertakings: (1) a round-robin to demonstrate the viability of the selected standard and (2) the certification of the lattice parameters of the SRM 1990, a Standard Reference Material?? for single crystal diffractometer alignment. This SRM is a set of ???3500 units of Cr-doped Al2O3, or ruby spheres [(0 420.011 mole fraction % Cr (expanded uncertainty)]. The round-robin consisted of determination of lattice parameters of a pair of crystals' the ruby sphere as a standard, and a zeolite reference to serve as an unknown. Fifty pairs of crystals were dispatched from Hauptman-Woodward Medical Research Institute to volunteers in x-ray laboratories world-wide. A total of 45 sets of data was received from 32 laboratories. The mean unit cell parameters of the ruby spheres was found to be a=4.7608 A?? ?? 0.0062 A??, and c=12.9979 A?? ?? 0.020 A?? (95 % intervals of the laboratory means). The source of errors of outlier data was identified. The SRM project involved the certification of lattice parameters using four well-aligned single crystal diffractometers at (Bell Laboratories) Lucent Technologies and at NRC of Canada (39 ruby spheres), the quantification of the Cr content using a combined microprobe and SEM/EDS technique, and the evaluation of the mosaicity of the ruby spheres using a double-crystal spectrometry method. A confirmation of the lattice parameters was also conducted using a Guinier-Ha??gg camera. Systematic corrections of thermal expansion and refraction corrections were applied. These rubies_ are rhombohedral, with space group R3c. The certified mean unit cell parameters are a=4.76080 ?? 0.00029 A??, and c=12 99568 A?? ?? 0.00087 A?? (expanded uncertainty). These certified lattice parameters fall well within the results of those obtained from the international round-robin study. The Guinier-Ha??gg transmission measurements on five samples of powdered rubies (a=4.7610 A?? ?? 0

  2. Standard Reference Material (SRM 1990) For Single Crystal Diffractometer Alignment

    PubMed Central

    Wong-Ng, W.; Siegrist, T.; DeTitta, G. T.; Finger, L. W.; Evans, H. T.; Gabe, E. J.; Enright, G. D.; Armstrong, J. T.; Levenson, M.; Cook, L. P.; Hubbard, C. R.

    2001-01-01

    An international project was successfully completed which involved two major undertakings: (1) a round-robin to demonstrate the viability of the selected standard and (2) the certification of the lattice parameters of the SRM 1990, a Standard Reference Material® for single crystal diffractometer alignment. This SRM is a set of ≈3500 units of Cr-doped Al2O3, or ruby spheres [(0.420.011 mole fraction % Cr (expanded uncertainty)]. The round-robin consisted of determination of lattice parameters of a pair of crystals: the ruby sphere as a standard, and a zeolite reference to serve as an unknown. Fifty pairs of crystals were dispatched from Hauptman-Woodward Medical Research Institute to volunteers in x-ray laboratories world-wide. A total of 45 sets of data was received from 32 laboratories. The mean unit cell parameters of the ruby spheres was found to be a=4.7608 ű0.0062 Å, and c=12.9979 ű0.020 Å (95 % intervals of the laboratory means). The source of errors of outlier data was identified. The SRM project involved the certification of lattice parameters using four well-aligned single crystal diffractometers at (Bell Laboratories) Lucent Technologies and at NRC of Canada (39 ruby spheres), the quantification of the Cr content using a combined microprobe and SEM/EDS technique, and the evaluation of the mosaicity of the ruby spheres using a double-crystal spectrometry method. A confirmation of the lattice parameters was also conducted using a Guinier-Hägg camera. Systematic corrections of thermal expansion and refraction corrections were applied. These rubies– are rhombohedral, with space group R3¯c. The certified mean unit cell parameters are a=4.76080±0.00029 Å, and c=12.99568 ű0.00087 Å (expanded uncertainty). These certified lattice parameters fall well within the results of those obtained from the international round-robin study. The Guinier-Hägg transmission measurements on five samples of powdered rubies (a=4.7610 ű0.0013 Å, and c = 12

  3. Continuous flow synthesis of ZSM-5 zeolite on the order of seconds

    PubMed Central

    Liu, Zhendong; Okabe, Kotatsu; Anand, Chokkalingam; Yonezawa, Yasuo; Zhu, Jie; Yamada, Hiroki; Endo, Akira; Yanaba, Yutaka; Yoshikawa, Takeshi; Ohara, Koji; Okubo, Tatsuya; Wakihara, Toru

    2016-01-01

    The hydrothermal synthesis of zeolites carried out in batch reactors takes a time so long (typically, on the order of days) that the crystallization of zeolites has long been believed to be very slow in nature. We herein present a synthetic process for ZSM-5, an industrially important zeolite, on the order of seconds in a continuous flow reactor using pressurized hot water as a heating medium. Direct mixing of a well-tuned precursor (90 °C) with the pressurized water preheated to extremely high temperature (370 °C) in the millimeter-sized continuous flow reactor resulted in immediate heating to high temperatures (240–300 °C); consequently, the crystallization of ZSM-5 in a seed-free system proceeded to completion within tens of or even several seconds. These results indicate that the crystallization of zeolites can complete in a period on the order of seconds. The subtle design combining a continuous flow reactor with pressurized hot water can greatly facilitate the mass production of zeolites in the future. PMID:27911823

  4. Enhanced water transport and salt rejection through hydrophobic zeolite pores.

    PubMed

    Humplik, Thomas; Lee, Jongho; O'Hern, Sean; Laoui, Tahar; Karnik, Rohit; Wang, Evelyn N

    2017-12-15

    The potential of improvements to reverse osmosis (RO) desalination by incorporating porous nanostructured materials such as zeolites into the selective layer in the membrane has spurred substantial research efforts over the past decade. However, because of the lack of methods to probe transport across these materials, it is still unclear which pore size or internal surface chemistry is optimal for maximizing permeability and salt rejection. We developed a platform to measure the transport of water and salt across a single layer of zeolite crystals, elucidating the effects of internal wettability on water and salt transport through the ≈5.5 Å pores of MFI zeolites. MFI zeolites with a more hydrophobic (i.e., less attractive) internal surface chemistry facilitated an approximately order of magnitude increase in water permeability compared to more hydrophilic MFI zeolites, while simultaneously fully rejecting both potassium and chlorine ions. However, our results also demonstrated approximately two orders of magnitude lower permeability compared to molecular simulations. This decreased performance suggests that additional transport resistances (such as surface barriers, pore collapse or blockages due to contamination) may be limiting the performance of experimental nanostructured membranes. Nevertheless, the inclusion of hydrophobic sub-nanometer pores into the active layer of RO membranes should improve both the water permeability and salt rejection of future RO membranes (Fasano et al 2016 Nat. Commun. 7 12762).

  5. Enhanced water transport and salt rejection through hydrophobic zeolite pores

    NASA Astrophysics Data System (ADS)

    Humplik, Thomas; Lee, Jongho; O'Hern, Sean; Laoui, Tahar; Karnik, Rohit; Wang, Evelyn N.

    2017-12-01

    The potential of improvements to reverse osmosis (RO) desalination by incorporating porous nanostructured materials such as zeolites into the selective layer in the membrane has spurred substantial research efforts over the past decade. However, because of the lack of methods to probe transport across these materials, it is still unclear which pore size or internal surface chemistry is optimal for maximizing permeability and salt rejection. We developed a platform to measure the transport of water and salt across a single layer of zeolite crystals, elucidating the effects of internal wettability on water and salt transport through the ≈5.5 Å pores of MFI zeolites. MFI zeolites with a more hydrophobic (i.e., less attractive) internal surface chemistry facilitated an approximately order of magnitude increase in water permeability compared to more hydrophilic MFI zeolites, while simultaneously fully rejecting both potassium and chlorine ions. However, our results also demonstrated approximately two orders of magnitude lower permeability compared to molecular simulations. This decreased performance suggests that additional transport resistances (such as surface barriers, pore collapse or blockages due to contamination) may be limiting the performance of experimental nanostructured membranes. Nevertheless, the inclusion of hydrophobic sub-nanometer pores into the active layer of RO membranes should improve both the water permeability and salt rejection of future RO membranes (Fasano et al 2016 Nat. Commun. 7 12762).

  6. Hydrogen Separation by Natural Zeolite Composite Membranes: Single and Multicomponent Gas Transport

    PubMed Central

    Farjoo, Afrooz; Kuznicki, Steve M.

    2017-01-01

    Single and multicomponent gas permeation tests were used to evaluate the performance of metal-supported clinoptilolite membranes. The efficiency of hydrogen separation from lower hydrocarbons (methane, ethane, and ethylene) was studied within the temperature and pressure ranges of 25–600 °C and 110–160 kPa, respectively. The hydrogen separation factor was found to reduce noticeably in the gas mixture compared with single gas experiments at 25 °C. The difference between the single and multicomponent gas results decreased as the temperature increased to higher than 300 °C, which is when the competitive adsorption–diffusion mechanism was replaced by Knudsen diffusion or activated diffusion mechanisms. To evaluate the effect of gas adsorption, the zeolite surface isotherms of each gas in the mixture were obtained from 25 °C to 600 °C. The results indicated negligible adsorption of individual gases at temperatures higher than 300 °C. Increasing the feed pressure resulted in a higher separation efficiency for the individual gases compared with the multicomponent mixture, due to the governing effect of the adsorptive mechanism. This study provides valuable insight into the application of natural zeolites for the separation of hydrogen from a mixture of hydrocarbons. PMID:28984833

  7. 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

  8. History and utility of zeolite framework-type discovery from a data-science perspective

    DOE PAGES

    Zimmermann, Nils E. R.; Haranczyk, Maciej

    2016-05-02

    Mature applications such as fluid catalytic cracking and hydrocracking rely critically on early zeolite structures. With a data-driven approach, we find that the discovery of exceptional zeolite framework types around the new millennium was spurred by exciting new utilization routes. The promising processes have yet not been successfully implemented (“valley of death” effect), mainly because of the lack of thermal stability of the crystals. As a result, this foreshadows limited deployability of recent zeolite discoveries that were achieved by novel crystal synthesis routes.

  9. Hierarchical zeolites from class F coal fly ash

    NASA Astrophysics Data System (ADS)

    Chitta, Pallavi

    Fly ash, a coal combustion byproduct is classified as types class C and class F. Class C fly ash is traditionally recycled for concrete applications and Class F fly ash often disposed in landfills. Class F poses an environmental hazard due to disposal and leaching of heavy metals into ground water and is important to be recycled in order to mitigate the environmental challenges. A major recycling option is to reuse the fly ash as a low-cost raw material for the production of crystalline zeolites, which serve as catalysts, detergents and adsorbents in the chemical industry. Most of the prior literature of fly ash conversion to zeolites does not focus on creating high zeolite surface area zeolites specifically with hierarchical pore structure, which are very important properties in developing a heterogeneous catalyst for catalysis applications. This research work aids in the development of an economical process for the synthesis of high surface area hierarchical zeolites from class F coal fly ash. In this work, synthesis of zeolites from fly ash using classic hydrothermal treatment approach and fusion pretreatment approach were examined. The fusion pretreatment method led to higher extent of dissolution of silica from quartz and mullite phases, which in turn led to higher surface area and pore size of the zeolite. A qualitative kinetic model developed here attributes the difference in silica content to Si/Al ratio of the beginning fraction of fly ash. At near ambient crystallization temperatures and longer crystallization times, the zeolite formed is a hierarchical faujasite with high surface area of at least 360 m2/g. This work enables the large scale recycling of class F coal fly ash to produce zeolites and mitigate environmental concerns. Design of experiments was used to predict surface area and pore sizes of zeolites - thus obviating the need for intense experimentation. The hierarchical zeolite catalyst supports tested for CO2 conversion, yielded hydrocarbons

  10. Feasible conversion of solid waste bauxite tailings into highly crystalline 4A zeolite with valuable application.

    PubMed

    Ma, Dongyang; Wang, Zhendong; Guo, Min; Zhang, Mei; Liu, Jingbo

    2014-11-01

    Bauxite tailings are a major type of solid wastes generated in the flotation process. The waste by-products caused significant environmental impact. To lessen this hazardous effect from poisonous mine tailings, a feasible and cost-effective solution was conceived and implemented. Our approach focused on reutilization of the bauxite tailings by converting it to 4A zeolite for reuse in diverse applications. Three steps were involved in the bauxite conversion: wet-chemistry, alkali fusion, and crystallization to remove impurities and to prepare porous 4A zeolite. It was found that the cubic 4A zeolite was single phase, in high purity, with high crystallinity and well-defined structure. Importantly, the 4A zeolite displayed maximum calcium ion exchange capacity averaged at 296 mg CaCO3/g, comparable to commercially-available zeolite (310 mg CaCO3/g) exchange capacity. Base on the optimal synthesis condition, the reaction yield of zeolite 4A from bauxite tailings achieved to about 38.43%, hence, this study will provide a new paradigm for remediation of bauxite tailings, further mitigating the environmental and health care concerns, particularly in the mainland of PR China. Copyright © 2014 Elsevier Ltd. All rights reserved.

  11. Vapor Responsive One-Dimensional Photonic Crystals from Zeolite Nanoparticles and Metal Oxide Films for Optical Sensing

    PubMed Central

    Lazarova, Katerina; Awala, Hussein; Thomas, Sebastien; Vasileva, Marina; Mintova, Svetlana; Babeva, Tsvetanka

    2014-01-01

    The preparation of responsive multilayered structures with quarter-wave design based on layer-by-layer deposition of sol-gel derived Nb2O5 films and spin-coated MEL type zeolite is demonstrated. The refractive indices (n) and thicknesses (d) of the layers are determined using non-linear curve fitting of the measured reflectance spectra. Besides, the surface and cross-sectional features of the multilayered structures are characterized by scanning electron microscopy (SEM). The quasi-omnidirectional photonic band for the multilayered structures is predicted theoretically, and confirmed experimentally by reflectance measurements at oblique incidence with polarized light. The sensing properties of the multilayered structures toward acetone are studied by measuring transmittance spectra prior and after vapor exposure. Furthermore, the potential of the one-dimensional photonic crystals based on the multilayered structure consisting of Nb2O5 and MEL type zeolite as a chemical sensor with optical read-out is discussed. PMID:25010695

  12. Synthesis, characterization, and ion-exchange properties of colloidal zeolite nanocrystals

    NASA Astrophysics Data System (ADS)

    Jawor, Anna; Jeong, Byeong-Heon; Hoek, Eric M. V.

    2009-10-01

    Here, we present physical-chemical properties of Linde type A (LTA) zeolite crystals synthesized via conventional hydrothermal and microwave heating methods. Both heating methods produced LTA crystals that were sub-micron in size, highly negatively charged, super-hydrophilic, and stable when dispersed in water. However, microwave heating produced relatively narrow crystal size distributions, required much shorter heating times, and did not significantly change composition, crystallinity, or surface chemistry. Moreover, microwave heating allowed systematic variation of crystal size by varying heating temperature and time during the crystallization reaction, thus producing a continuous gradient of crystal sizes ranging from about 90 to 300 nm. In ion-exchange studies, colloidal zeolites exhibited excellent sorption kinetics and capacity for divalent metal ions, suggesting their potential for use in water softening, scale inhibition, and scavenging of toxic metal ions from water.

  13. Atmospheric Pressure Plasma Jet-Assisted Synthesis of Zeolite-Based Low-k Thin Films.

    PubMed

    Huang, Kai-Yu; Chi, Heng-Yu; Kao, Peng-Kai; Huang, Fei-Hung; Jian, Qi-Ming; Cheng, I-Chun; Lee, Wen-Ya; Hsu, Cheng-Che; Kang, Dun-Yen

    2018-01-10

    Zeolites are ideal low-dielectric constant (low-k) materials. This paper reports on a novel plasma-assisted approach to the synthesis of low-k thin films comprising pure-silica zeolite MFI. The proposed method involves treating the aged solution using an atmospheric pressure plasma jet (APPJ). The high reactivity of the resulting nitrogen plasma helps to produce zeolite crystals with high crystallinity and uniform crystal size distribution. The APPJ treatment also remarkably reduces the time for hydrothermal reaction. The zeolite MFI suspensions synthesized with the APPJ treatment are used for the wet deposition to form thin films. The deposited zeolite thin films possessed dense morphology and high crystallinity, which overcome the trade-off between crystallinity and film quality. Zeolite thin films synthesized using the proposed APPJ treatment achieve low leakage current (on the order of 10 -8 A/cm 2 ) and high Young's modulus (12 GPa), outperforming the control sample synthesized without plasma treatment. The dielectric constant of our zeolite thin films was as low as 1.41. The overall performance of the low-k thin films synthesized with the APPJ treatment far exceed existing low-k films comprising pure-silica MFI.

  14. Sponge-like nanoporous single crystals of gold

    PubMed Central

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

    2015-01-01

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

  15. A database of new zeolite-like materials.

    PubMed

    Pophale, Ramdas; Cheeseman, Phillip A; Deem, Michael W

    2011-07-21

    We here describe a database of computationally predicted zeolite-like materials. These crystals were discovered by a Monte Carlo search for zeolite-like materials. Positions of Si atoms as well as unit cell, space group, density, and number of crystallographically unique atoms were explored in the construction of this database. The database contains over 2.6 M unique structures. Roughly 15% of these are within +30 kJ mol(-1) Si of α-quartz, the band in which most of the known zeolites lie. These structures have topological, geometrical, and diffraction characteristics that are similar to those of known zeolites. The database is the result of refinement by two interatomic potentials that both satisfy the Pauli exclusion principle. The database has been deposited in the publicly available PCOD database and in www.hypotheticalzeolites.net/database/deem/. This journal is © the Owner Societies 2011

  16. 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.

  17. Zeolites replacing plant fossils in the Denver formation, Lakewood, Colorado.

    USGS Publications Warehouse

    Modreski, P.J.; Verbeek, E.R.; Grout, M.A.

    1984-01-01

    Well-developed crystals of heulandite and stilbite, within fossil wood, occur in sedimentary rocks in Lakewood, Jefferson County. The rocks belong to the Denver formation, a locally fossiliferous deposit of fluvial claystone, siltstone, sandstone and conglomerate, containing some volcanic mudflows (andesitic) of late Cretaceous to Palaeocene age. Altered volcanic glass released Na and Ca into the ground-water and subsequently zeolites were crystallized in the open spaces between grains and within fossil plant structures. Minor pyrite, quartz (jasper), calcite and apatite also occur as replacements of fossil wood. Similar zeolite occurrences in other areas are reviewed.-R.S.M.

  18. Method of making single crystal fibers

    NASA Technical Reports Server (NTRS)

    Westfall, Leonard J. (Inventor)

    1990-01-01

    Single crystal fibers are made from miniature extruded ceramic feed rods. A decomposable binder is mixed with powders to inform a slurry which is extruded into a small rod which may be sintered, either in air or in vacuum, or it may be used in the extruded and dried condition. A pair of laser beams focuses onto the tip of the rod to melt it thereby forming a liquid portion. A single crystal seed fiber of the same material as the feed rod contacts this liquid portion to establish a zone of liquid material between the feed rod and the single crystal seed fiber. The feed rod and the single crystal feed fiber are moved at a predetermined speed to solidify the molten zone onto the seed fiber while simultaneously melting additional feed rod. In this manner a single crystal fiber is formed from the liquid portion.

  19. Enhanced chromium adsorption capacity via plasma modification of natural zeolites

    NASA Astrophysics Data System (ADS)

    Cagomoc, Charisse Marie D.; Vasquez, Magdaleno R., Jr.

    2017-01-01

    Natural zeolites such as mordenite are excellent adsorbents for heavy metals. To enhance the adsorption capacity of zeolite, sodium-exchanged samples were irradiated with 13.56 MHz capacitively coupled radio frequency (RF) argon gas discharge. Hexavalent chromium [Cr(VI)] was used as the test heavy metal. Pristine and plasma-treated zeolite samples were soaked in 50 mg/L Cr solution and the amount of adsorbed Cr(VI) on the zeolites was calculated at predetermined time intervals. Compared with untreated zeolite samples, initial Cr(VI) uptake was 70% higher for plasma-treated zeolite granules (50 W 30 min) after 1 h of soaking. After 24 h, all plasma-treated zeolites showed increased Cr(VI) uptake. For a 2- to 4-month period, Cr(VI) uptake increased about 130% compared with untreated zeolite granules. X-ray diffraction analyses between untreated and treated zeolite samples revealed no major difference in terms of its crystal structure. However, for plasma-treated samples, an increase in the number of surface defects was observed from scanning electron microscopy images. This increase in the number of surface defects induced by plasma exposure played a crucial role in increasing the number of active sorption sites on the zeolite surface.

  20. Mechanochemical Synthesis of Carbon Nanothread Single Crystals.

    PubMed

    Li, Xiang; Baldini, Maria; Wang, Tao; Chen, Bo; Xu, En-Shi; Vermilyea, Brian; Crespi, Vincent H; Hoffmann, Roald; Molaison, Jamie J; Tulk, Christopher A; Guthrie, Malcolm; Sinogeikin, Stanislav; Badding, John V

    2017-11-15

    Synthesis of well-ordered reduced dimensional carbon solids with extended bonding remains a challenge. For example, few single-crystal organic monomers react under topochemical control to produce single-crystal extended solids. We report a mechanochemical synthesis in which slow compression at room temperature under uniaxial stress can convert polycrystalline or single-crystal benzene monomer into single-crystalline packings of carbon nanothreads, a one-dimensional sp 3 carbon nanomaterial. The long-range order over hundreds of microns of these crystals allows them to readily exfoliate into fibers. The mechanochemical reaction produces macroscopic single crystals despite large dimensional changes caused by the formation of multiple strong, covalent C-C bonds to each monomer and a lack of reactant single-crystal order. Therefore, it appears not to follow a topochemical pathway, but rather one guided by uniaxial stress, to which the nanothreads consistently align. Slow-compression room-temperature synthesis may allow diverse molecular monomers to form single-crystalline packings of polymers, threads, and higher dimensional carbon networks.

  1. Single crystal diamond membranes for nanoelectronics.

    PubMed

    Bray, Kerem; Kato, Hiromitsu; Previdi, Rodolfo; Sandstrom, Russell; Ganesan, Kumaravelu; Ogura, Masahiko; Makino, Toshiharu; Yamasaki, Satoshi; Magyar, Andrew P; Toth, Milos; Aharonovich, Igor

    2018-02-22

    Single crystal, nanoscale diamond membranes are highly sought after for a variety of applications including nanophotonics, nanoelectronics and quantum information science. However, so far, the availability of conductive diamond membranes has remained an unreachable goal. In this work we present a complete nanofabrication methodology for engineering high aspect ratio, electrically active single crystal diamond membranes. The membranes have large lateral directions, exceeding ∼500 × 500 μm 2 and are only several hundreds of nanometers thick. We further realize vertical single crystal p-n junctions made from the diamond membranes that exhibit onset voltages of ∼10 V and a current of several mA. Moreover, we deterministically introduce optically active color centers into the membranes, and demonstrate for the first time a single crystal nanoscale diamond LED. The robust and scalable approach to engineer the electrically active single crystal diamond membranes offers new pathways for advanced nanophotonic, nanoelectronic and optomechanical devices employing diamond.

  2. Nanoassembled dynamic optical waveguides and sensors based on zeolite L nanocontainers

    NASA Astrophysics Data System (ADS)

    Barroso, Álvaro; Dieckmann, Katrin; Alpmann, Christina; Buscher, Tim; Studer, Armido; Denz, Cornelia

    2015-03-01

    Although optical functional devices as waveguides and sensors are of utmost importance for metrology on the nano scale, the micro-and nano-assembly by optical means of functional materials to create such optical elements has yet not been considered. In the last years, an elegant strategy based on holographic optical tweezers (HOT) has been developed to design and fabricate permanent and dynamic three-dimensional micro- and nanostructures based on functional nanocontainers as building blocks. Nanocontainers that exhibit stable and ordered voids to hierarchically organize guest materials are especially attractive. Zeolite L are a type of porous micro-sized crystals which features a high number of strictly one-dimensional, parallel aligned nanochannels. They are highly interesting as building blocks of functional nano-and microsystems due to their potential as nanocontainers to accommodate various different guest molecules and to assemble them in specific configurations. For instance, based on zeolite L crystals, microscopic polarization sensors and chains of several microcrystals for hierarchical supramolecular organization have been realized. Here, we demonstrate the ability of nanocontainers in general, and zeolite L crystals in particular to represent the basic constituent of optical functional microsystems. We show that the capability of HOT to manipulate multitude of non-spherical microparticles in three dimensions can be exploited for the investigation of zeolite L nanocontainers as dynamic optical waveguides. Moreover, we implement as additional elements dye-loaded zeolite L to sense the guiding features of these novel waveguides with high spatial precision and microspheres to enhance the light coupling into the zeolite L waveguides. With this elaborated approach of using nanocontainers as tailored building blocks for functional optical systems a new era of bricking optical components in a lego-like style becomes feasible.

  3. Feasible conversion of solid waste bauxite tailings into highly crystalline 4A zeolite with valuable application

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

    Ma, Dongyang; Wang, Zhendong; Guo, Min

    2014-11-15

    Highlights: • Concept to convert waste to valuable product is carried out in this study. • An industrially feasible and cost-effective approach was developed and optimized. • Highly crystalline and well-defined zeolite was produced under moderate conditions. • The zeolite derived from the bauxite tailings displayed high ion exchange capacity. • Bauxite tailings have potential application in heavy metal ions adsorbent. - Abstract: Bauxite tailings are a major type of solid wastes generated in the flotation process. The waste by-products caused significant environmental impact. To lessen this hazardous effect from poisonous mine tailings, a feasible and cost-effective solution was conceivedmore » and implemented. Our approach focused on reutilization of the bauxite tailings by converting it to 4A zeolite for reuse in diverse applications. Three steps were involved in the bauxite conversion: wet-chemistry, alkali fusion, and crystallization to remove impurities and to prepare porous 4A zeolite. It was found that the cubic 4A zeolite was single phase, in high purity, with high crystallinity and well-defined structure. Importantly, the 4A zeolite displayed maximum calcium ion exchange capacity averaged at 296 mg CaCO{sub 3}/g, comparable to commercially-available zeolite (310 mg CaCO{sub 3}/g) exchange capacity. Base on the optimal synthesis condition, the reaction yield of zeolite 4A from bauxite tailings achieved to about 38.43%, hence, this study will provide a new paradigm for remediation of bauxite tailings, further mitigating the environmental and health care concerns, particularly in the mainland of PR China.« less

  4. Atomic sites and stability of Cs+ captured within zeolitic nanocavities

    PubMed Central

    Yoshida, Kaname; Toyoura, Kazuaki; Matsunaga, Katsuyuki; Nakahira, Atsushi; Kurata, Hiroki; Ikuhara, Yumi H.; Sasaki, Yukichi

    2013-01-01

    Zeolites have potential application as ion-exchangers, catalysts and molecular sieves. Zeolites are once again drawing attention in Japan as stable adsorbents and solidification materials of fission products, such as 137Cs+ from damaged nuclear-power plants. Although there is a long history of scientific studies on the crystal structures and ion-exchange properties of zeolites for practical application, there are still open questions, at the atomic-level, on the physical and chemical origins of selective ion-exchange abilities of different cations and detailed atomic structures of exchanged cations inside the nanoscale cavities of zeolites. Here, the precise locations of Cs+ ions captured within A-type zeolite were analyzed using high-resolution electron microscopy. Together with theoretical calculations, the stable positions of absorbed Cs+ ions in the nanocavities are identified, and the bonding environment within the zeolitic framework is revealed to be a key factor that influences the locations of absorbed cations. PMID:23949184

  5. 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.

  6. Effects of ultrasonic treatment on zeolite NaA synthesized from by-product silica.

    PubMed

    Vaičiukynienė, Danutė; Kantautas, Aras; Vaitkevičius, Vitoldas; Jakevičius, Leonas; Rudžionis, Žymantas; Paškevičius, Mantas

    2015-11-01

    The synthesis of zeolite NaA from silica by-product was carried out in the presence of 20 kHz ultrasound at room temperature. Zeolites obtained in this type of synthesis were compared to zeolites obtained by performing conventional static syntheses under similar conditions. The sonication effects on zeolite NaA synthesis were characterized by phase identification, crystallinity etc. The effects of different parameters such as crystallization time and initial materials preparation methods on the crystallinity and morphology of the synthesized zeolites were investigated. The final products were characterized by XRD and FT-IR. It was possible to obtain crystalline zeolite NaA from by-product silica in the presence of ultrasound. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Na, K, Rb, and Cs Exchange in Heulandite Single-Crystals: X-Ray Structure Refinements at 100 K

    NASA Astrophysics Data System (ADS)

    Yang, Ping; Armbruster, Thomas

    1996-04-01

    The crystal structures of Na-, K-, Rb-, and Cs-exchanged varieties of the zeolite heulandite with the simplified compositionM+9Al9Si27O72·nH2O were studied by single-crystal X-ray diffraction at 100 K. The structure refinements of Na-, K-, and Rb-exchanged heulandite were performed in space groupC2/mwith resultantRvalues of 3.8, 3.0, and 4.9%, respectively. Cs-exchanged heulandite was refined in space groupC[formula], yielding anRvalue of 3.4%. X-ray single-crystal data of the Cs-exchanged variety indicated that many reflections of typeh k lwere not equivalent toh -k las expected for monoclinic symmetry. With increasing radius of the incorporated channel cations, thebaxis increases from 17.93 to 18.09 Å leading to a slight widening of the channels. The number of H2O molecules also decreases with increasing cation radius due to space limitations. Three general cation positions (II-1,C3, andB4) were found in the four exchanged heulandite samples. For Rb- and Cs-exchanged crystals, the additional cation siteA2 occurs. In Cs-exchanged heulandite symmetry lowering is due to partial Si, Al ordering in the framework accompanied with a more asymmetric arrangement of channel Cs. Only if heavy elements in the channels are present the symmetry information of the framework is enforced, thus partial Si, Al ordering can be resolved.

  8. Formation of curved micrometer-sized single crystals.

    PubMed

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

    2014-05-27

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

  9. One-Step Hydrothermal Synthesis of Zeolite X Powder from Natural Low-Grade Diatomite.

    PubMed

    Yao, Guangyuan; Lei, Jingjing; Zhang, Xiaoyu; Sun, Zhiming; Zheng, Shuilin

    2018-05-28

    Zeolite X powder was synthesized using natural low-grade diatomite as the main source of Si but only as a partial source of Al via a simple and green hydrothermal method. The microstructure and surface properties of the obtained samples were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), wavelength dispersive X-ray fluorescence (XRF), calcium ion exchange capacity (CEC), thermogravimetric-differential thermal (TG-DTA) analysis, and N₂ adsorption-desorption technique. The influence of various synthesis factors, including aging time and temperature, crystallization time and temperature, Na₂O/SiO₂ and H₂O/Na₂O ratio on the CEC of zeolite, were systematically investigated. The as-synthesized zeolite X with binary meso-microporous structure possessed remarkable thermal stability, high calcium ion exchange capacity of 248 mg/g and large surface area of 453 m²/g. In addition, the calcium ion exchange capacity of zeolite X was found to be mainly determined by the crystallization degree. In conclusion, the synthesized zeolite X using diatomite as a cost-effective raw material in this study has great potential for industrial application such as catalyst support and adsorbent.

  10. Development of n- and p-type Doped Perovskite Single Crystals Using Solid-State Single Crystal Growth (SSCG) Technique

    DTIC Science & Technology

    2017-10-09

    doped BaTiO3 single crystal) could be also fabricated by using a BaTiO3 ceramics with the same compositional gradient (Fig. 8). This result has...piezoelectric applications. Compositionally PZT ceramics lie near the MPB between the tetragonal and rhombohedral phases and MPB compositions ...single crystal growth) technique are suitable to grow a variety of “n- and p-type doped” perovskite single crystals of complicated compositions . The

  11. The growth of zeolites A, X and mordenite in space

    NASA Technical Reports Server (NTRS)

    Sacco, Albert, Jr.; Bac, N.; Coker, E. N.; Dixon, A. G.; Warzywoda, J.; Thompson, R. W.

    1994-01-01

    supersaturation, and this gel undergoes a continuous 'polymerization' type reaction during nucleation and growth. Generally, for structure characterization and diffusion studies, which are useful in evaluating zeolites for improving yield in petroleum refining as well as for many of the proposed new applications (e.g., catalytic membranes, molecular electronics, chemical sensors) large zeolites (greater than 100 to 1000 times normal size) with minimum lattice defects are desired. Presently, the lack of understanding of zeolite nucleation and growth precludes the custom design of zeolites for these or other uses. It was hypothesized that the microgravity levels achieved in an orbiting spacecraft could help to isolate the possible effects of natural convection (which affects defect formation) and minimize sedimentation, which occurs since zeolites are twice as dense as the solution from which they are formed. This was expected to promote larger crystals by allowing growing crystals a longer residence time in a high-concentration nutrient field. Thus it was hypothesized that the microgravity environment of Earth orbit would allow the growth of large, more defect-free zeolite crystals in high yield.

  12. 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.

  13. Co-remediation of the lead-polluted garden soil by exogenous natural zeolite and humic acids.

    PubMed

    Shi, Wei-yu; Shao, Hong-bo; Li, Hua; Shao, Ming-an; Du, Sheng

    2009-08-15

    The current study reported the co-remediation effect on the lead-polluted garden soil by zeolite and humic acids (HA), which was from comparing with the remediation of single zeolite in term of the lead fraction of sequential extraction in the soil and the distribution of lead in different parts of rape. Mixed treatment (zeolite and HA) and single treatment (zeolite) were, respectively, applied to the artificially polluted garden soil to examine the difference of their remediation effects in pot experiment. Results indicated that the co-remediation led to significantly greater (p<0.01) reduction in the lead concentration in plants than by singly adding to zeolite. The co-application of zeolite and HA reduced the available fraction of lead compounds, but slightly increased (p<0.01) the water-soluble fraction of lead compounds in the garden soil, compared with the application of single zeolite, especially in the severe lead-polluted soil (> or =1000 mg kg(-1)). This method might be an efficient way to remediate the lead-polluted soils on a large scale, although zeolite is a kind of hazardous material.

  14. Scaling Relations for Acidity and Reactivity of Zeolites

    PubMed Central

    2017-01-01

    Zeolites are widely applied as solid acid catalysts in various technological processes. In this work we have computationally investigated how catalytic reactivity scales with acidity for a range of zeolites with different topologies and chemical compositions. We found that straightforward correlations are limited to zeolites with the same topology. The adsorption energies of bases such as carbon monoxide (CO), acetonitrile (CH3CN), ammonia (NH3), trimethylamine (N(CH3)3), and pyridine (C5H5N) give the same trend of acid strength for FAU zeolites with varying composition. Crystal orbital Hamilton populations (COHP) analysis provides a detailed molecular orbital picture of adsorbed base molecules on the Brønsted acid sites (BAS). Bonding is dominated by strong σ donation from guest molecules to the BAS for the adsorbed CO and CH3CN complexes. An electronic descriptor of acid strength is constructed based on the bond order calculations, which is an intrinsic parameter rather than adsorption energy that contains additional contributions due to secondary effects such as van der Waals interactions with the zeolite walls. The bond order parameter derived for the CH3CN adsorption complex represents a useful descriptor for the intrinsic acid strength of FAU zeolites. For FAU zeolites the activation energy for the conversion of π-adsorbed isobutene into alkoxy species correlates well with the acid strength determined by the NH3 adsorption energies. Other zeolites such as MFI and CHA do not follow the scaling relations obtained for FAU; we ascribe this to the different van der Waals interactions and steric effects induced by zeolite framework topology. PMID:29142616

  15. Ames Lab 101: Single Crystal Growth

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

    Schlagel, Deborah

    2013-09-27

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

  16. Ames Lab 101: Single Crystal Growth

    ScienceCinema

    Schlagel, Deborah

    2018-01-16

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

  17. Exploitation of Unique Properties of Zeolites in the Development of Gas Sensors

    PubMed Central

    Zheng, Yangong; Li, Xiaogan; Dutta, Prabir K.

    2012-01-01

    The unique properties of microporous zeolites, including ion-exchange properties, adsorption, molecular sieving, catalysis, conductivity have been exploited in improving the performance of gas sensors. Zeolites have been employed as physical and chemical filters to improve the sensitivity and selectivity of gas sensors. In addition, direct interaction of gas molecules with the extraframework cations in the nanoconfined space of zeolites has been explored as a basis for developing new impedance-type gas/vapor sensors. In this review, we summarize how these properties of zeolites have been used to develop new sensing paradigms. There is a considerable breadth of transduction processes that have been used for zeolite incorporated sensors, including frequency measurements, optical and the entire gamut of electrochemical measurements. It is clear from the published literature that zeolites provide a route to enhance sensor performance, and it is expected that commercial manifestation of some of the approaches discussed here will take place. The future of zeolite-based sensors will continue to exploit its unique properties and use of other microporous frameworks, including metal organic frameworks. Zeolite composites with electronic materials, including metals will lead to new paradigms in sensing. Use of nano-sized zeolite crystals and zeolite membranes will enhance sensor properties and make possible new routes of miniaturized sensors. PMID:22666081

  18. Nanoparticles Incorporated inside Single-Crystals: Enhanced Fluorescent Properties

    DOE PAGES

    Liu, Yujing; Zang, Huidong; Wang, Ling; ...

    2016-09-25

    Incorporation of guest materials inside single-crystalline hosts leads to single-crystal composites that have become more and more frequently seen in both biogenic and synthetic crystals. The unique composite structure together with long-range ordering promises special properties that are, however, less often demonstrated. In this study, we examine the fluorescent properties of quantum dots (QDs) and polymer dots (Pdots) encapsulated inside the hosts of calcite single-crystals. Two CdTe QDs and two Pdots are incorporated into growing calcite crystals, as the QDs and Pdots are dispersed in the crystallization media of agarose gels. As a result, enhanced fluorescent properties are obtained frommore » the QDs and Pdots inside calcite single-crystals with greatly improved photostability and significantly prolonged fluorescence lifetime, compared to those in solutions and gels. Particularly, the fluorescence lifetime increases by 0.5-1.6 times after the QDs or Pdots are incorporated. The enhanced fluorescent properties indicate the advantages of encapsulation by single-crystal hosts that provide dense shells to isolate the fluorescent nanoparticles from atmosphere. As such, this work has implications for advancing the research of single-crystal composites toward their functional design.« less

  19. GROWTH AND CHARACTERIZATION OF SINGLE CRYSTALS OF RARE EARTH COMPOUNDS.

    DTIC Science & Technology

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

  20. 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.

  1. Single crystals of selected titanates and tungstates

    NASA Technical Reports Server (NTRS)

    Loiacono, G. M.

    1972-01-01

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

  2. Growth of single crystals of BaFe12O19 by solid state crystal growth

    NASA Astrophysics Data System (ADS)

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

    2016-10-01

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

  3. La roca magica: Uses of natural zeolites in agriculture and industry

    PubMed Central

    Mumpton, Frederick A.

    1999-01-01

    For nearly 200 years since their discovery in 1756, geologists considered the zeolite minerals to occur as fairly large crystals in the vugs and cavities of basalts and other traprock formations. Here, they were prized by mineral collectors, but their small abundance and polymineralic nature defied commercial exploitation. As the synthetic zeolite (molecular sieve) business began to take hold in the late 1950s, huge beds of zeolite-rich sediments, formed by the alteration of volcanic ash (glass) in lake and marine waters, were discovered in the western United States and elsewhere in the world. These beds were found to contain as much as 95% of a single zeolite; they were generally flat-lying and easily mined by surface methods. The properties of these low-cost natural materials mimicked those of many of their synthetic counterparts, and considerable effort has made since that time to develop applications for them based on their unique adsorption, cation-exchange, dehydration–rehydration, and catalytic properties. Natural zeolites (i.e., those found in volcanogenic sedimentary rocks) have been and are being used as building stone, as lightweight aggregate and pozzolans in cements and concretes, as filler in paper, in the take-up of Cs and Sr from nuclear waste and fallout, as soil amendments in agronomy and horticulture, in the removal of ammonia from municipal, industrial, and agricultural waste and drinking waters, as energy exchangers in solar refrigerators, as dietary supplements in animal diets, as consumer deodorizers, in pet litters, in taking up ammonia from animal manures, and as ammonia filters in kidney-dialysis units. From their use in construction during Roman times, to their role as hydroponic (zeoponic) substrate for growing plants on space missions, to their recent success in the healing of cuts and wounds, natural zeolites are now considered to be full-fledged mineral commodities, the use of which promise to expand even more in the future. PMID

  4. La roca magica: uses of natural zeolites in agriculture and industry.

    PubMed

    Mumpton, F A

    1999-03-30

    For nearly 200 years since their discovery in 1756, geologists considered the zeolite minerals to occur as fairly large crystals in the vugs and cavities of basalts and other traprock formations. Here, they were prized by mineral collectors, but their small abundance and polymineralic nature defied commercial exploitation. As the synthetic zeolite (molecular sieve) business began to take hold in the late 1950s, huge beds of zeolite-rich sediments, formed by the alteration of volcanic ash (glass) in lake and marine waters, were discovered in the western United States and elsewhere in the world. These beds were found to contain as much as 95% of a single zeolite; they were generally flat-lying and easily mined by surface methods. The properties of these low-cost natural materials mimicked those of many of their synthetic counterparts, and considerable effort has made since that time to develop applications for them based on their unique adsorption, cation-exchange, dehydration-rehydration, and catalytic properties. Natural zeolites (i.e., those found in volcanogenic sedimentary rocks) have been and are being used as building stone, as lightweight aggregate and pozzolans in cements and concretes, as filler in paper, in the take-up of Cs and Sr from nuclear waste and fallout, as soil amendments in agronomy and horticulture, in the removal of ammonia from municipal, industrial, and agricultural waste and drinking waters, as energy exchangers in solar refrigerators, as dietary supplements in animal diets, as consumer deodorizers, in pet litters, in taking up ammonia from animal manures, and as ammonia filters in kidney-dialysis units. From their use in construction during Roman times, to their role as hydroponic (zeoponic) substrate for growing plants on space missions, to their recent success in the healing of cuts and wounds, natural zeolites are now considered to be full-fledged mineral commodities, the use of which promise to expand even more in the future.

  5. Porosity Evolution in a Creeping Single Crystal (Preprint)

    DTIC Science & Technology

    2012-08-01

    1] indicated that the growth of initially present processing induced voids in a nickel based single crystal superalloy played a significant role in...processing induced voids in a nickel based single crystal superalloy played a significant role in limiting creep life. Also, creep tests on single...experimental observations of creep deformation and failure of a nickel based single crystal superalloy, [1, 2]. Metallographic observations have shown that Ni

  6. Ultratough single crystal boron-doped diamond

    DOEpatents

    Hemley, Russell J [Carnegie Inst. for Science, Washington, DC ; Mao, Ho-Kwang [Carnegie Inst. for Science, Washington, DC ; Yan, Chih-Shiue [Carnegie Inst. for Science, Washington, DC ; Liang, Qi [Carnegie Inst. for Science, Washington, DC

    2015-05-05

    The invention relates to a single crystal boron doped CVD diamond that has a toughness of at least about 22 MPa m.sup.1/2. The invention further relates to a method of manufacturing single crystal boron doped CVD diamond. The growth rate of the diamond can be from about 20-100 .mu.m/h.

  7. GIS-NaP1 zeolite microspheres as potential water adsorption material: Influence of initial silica concentration on adsorptive and physical/topological properties

    PubMed Central

    Sharma, Pankaj; Song, Ju-Sub; Han, Moon Hee; Cho, Churl-Hee

    2016-01-01

    GIS-NaP1 zeolite samples were synthesized using seven different Si/Al ratios (5–11) of the hydrothermal reaction mixtures having chemical composition Al2O3:xSiO2:14Na2O:840H2O to study the impact of Si/Al molar ratio on the water vapour adsorption potential, phase purity, morphology and crystal size of as-synthesized GIS-NaP1 zeolite crystals. The X-ray diffraction (XRD) observations reveal that Si/Al ratio does not affect the phase purity of GIS-NaP1 zeolite samples as high purity GIS-NaP1 zeolite crystals were obtained from all Si/Al ratios. Contrary, Si/Al ratios have remarkable effect on the morphology, crystal size and porosity of GIS-NaP1 zeolite microspheres. Transmission electron microscopy (TEM) evaluations of individual GIS-NaP1 zeolite microsphere demonstrate the characteristic changes in the packaging/arrangement, shape and size of primary nano crystallites. Textural characterisation using water vapour adsorption/desorption, and nitrogen adsorption/desorption data of as-synthesized GIS-NaP1 zeolite predicts the existence of mix-pores i.e., microporous as well as mesoporous character. High water storage capacity 1727.5 cm3 g−1 (138.9 wt.%) has been found for as-synthesized GIS-NaP1 zeolite microsphere samples during water vapour adsorption studies. Further, the total water adsorption capacity values for P6 (1299.4 mg g−1) and P7 (1388.8 mg g−1) samples reveal that these two particular samples can absorb even more water than their own weights. PMID:26964638

  8. GIS-NaP1 zeolite microspheres as potential water adsorption material: Influence of initial silica concentration on adsorptive and physical/topological properties.

    PubMed

    Sharma, Pankaj; Song, Ju-Sub; Han, Moon Hee; Cho, Churl-Hee

    2016-03-11

    GIS-NaP1 zeolite samples were synthesized using seven different Si/Al ratios (5-11) of the hydrothermal reaction mixtures having chemical composition Al2O3:xSiO2:14Na2O:840H2O to study the impact of Si/Al molar ratio on the water vapour adsorption potential, phase purity, morphology and crystal size of as-synthesized GIS-NaP1 zeolite crystals. The X-ray diffraction (XRD) observations reveal that Si/Al ratio does not affect the phase purity of GIS-NaP1 zeolite samples as high purity GIS-NaP1 zeolite crystals were obtained from all Si/Al ratios. Contrary, Si/Al ratios have remarkable effect on the morphology, crystal size and porosity of GIS-NaP1 zeolite microspheres. Transmission electron microscopy (TEM) evaluations of individual GIS-NaP1 zeolite microsphere demonstrate the characteristic changes in the packaging/arrangement, shape and size of primary nano crystallites. Textural characterisation using water vapour adsorption/desorption, and nitrogen adsorption/desorption data of as-synthesized GIS-NaP1 zeolite predicts the existence of mix-pores i.e., microporous as well as mesoporous character. High water storage capacity 1727.5 cm(3) g(-1) (138.9 wt.%) has been found for as-synthesized GIS-NaP1 zeolite microsphere samples during water vapour adsorption studies. Further, the total water adsorption capacity values for P6 (1299.4 mg g(-1)) and P7 (1388.8 mg g(-1)) samples reveal that these two particular samples can absorb even more water than their own weights.

  9. Single crystal, liquid crystal, and hybrid organic semiconductors

    NASA Astrophysics Data System (ADS)

    Twieg, Robert J.; Getmanenko, Y.; Lu, Z.; Semyonov, A. N.; Huang, S.; He, P.; Seed, A.; Kiryanov, A.; Ellman, B.; Nene, S.

    2003-07-01

    The synthesis and characterization of organic semiconductors is being pursued in three primary structure formats: single crystal, liquid crystal and organic-inorganic hybrid. The strategy here is to share common structures, synthesis methods and fabrication techniques across these formats and to utilize common characterization tools such as the time of flight technique. The single crystal efforts concentrate on aromatic and heteroaromatic compounds including simple benzene derivatives and derivatives of the acenes. The structure-property relationships due to incorporation of small substituents and heteroatoms are being examined. Crystals are grown by solution, melt or vapor transport techniques. The liquid crystal studies exploit their self-organizing properties and relative ease of sample preparation. Though calamitic systems tha deliver the largest mobilities are higher order smectics, even some unusual twist grain boundary phases are being studied. We are attempting to synthesize discotic acene derivatives with appropriate substitution patterns to render them mesogenic. The last format being examined is the hybrid organic-inorganic class. Here, layered materials of alternating organic and inorganic composition are designed and synthesized. Typical materials are conjugated aromatic compounds, usually functinalized with an amine or a pyridine and reacted with appropriate reactive metal derivatives to incorporate them into metal oxide or sulfide layers.

  10. Piezoelectric single crystals for ultrasonic transducers in biomedical applications

    PubMed Central

    Zhou, Qifa; Lam, Kwok Ho; Zheng, Hairong; Qiu, Weibao; Shung, K. Kirk

    2014-01-01

    Piezoelectric single crystals, which have excellent piezoelectric properties, have extensively been employed for various sensors and actuators applications. In this paper, the state–of–art in piezoelectric single crystals for ultrasonic transducer applications is reviewed. Firstly, the basic principles and design considerations of piezoelectric ultrasonic transducers will be addressed. Then, the popular piezoelectric single crystals used for ultrasonic transducer applications, including LiNbO3 (LN), PMN–PT and PIN–PMN–PT, will be introduced. After describing the preparation and performance of the single crystals, the recent development of both the single–element and array transducers fabricated using the single crystals will be presented. Finally, various biomedical applications including eye imaging, intravascular imaging, blood flow measurement, photoacoustic imaging, and microbeam applications of the single crystal transducers will be discussed. PMID:25386032

  11. Synthesis and Properties of Nanoparticle Forms Saponite Clay, Cancrinite Zeolite and Phase Mixtures Thereof.

    PubMed

    Shao, Hua; Pinnavaia, Thomas J

    2010-09-01

    The low-temperature synthesis (90°C) of nanoparticle forms of a pure phase smectic clay (saponite) and zeolite (cancrinite) is reported, along with phase mixtures thereof. A synthesis gel corresponding to the Si:Al:Mg unit cell composition of saponite (3.6:0.40:3.0) and a NaOH/Si ratio of 1.39 affords the pure phase clay with disordered nanolayer stacking. Progressive increases in the NaOH/Si ratio up to a value of 8.33 results in the co-crystallization of first garronite and then cancrinite zeolites with nanolath morphology. The resulting phase mixtures exhibit a compound particulate structure of intertwined saponite nanolayers and cancrinite nanolaths that cannot be formed through physical mixing of the pure phase end members. Under magnesium-free conditions, pure phase cancrinite nanocrystals are formed. The Si/Al ratio of the reaction mixture affects the particle morphology as well as the chemical composition of the cancrinite zeolite. Ordinarily, cancrinite crystallizes with a Si/Al ratio of 1.0, but a silicon-rich form of the zeolite (Si/Al=1.25) is crystallized at low temperature from a silica rich synthesis gel, as evidenced by (29)Si NMR spectroscopy and XEDS-TEM. Owing to the exceptionally high external surface areas of the pure phase clay (875 m(2)/g) and zeolite end members (8.9 - 40 m(2)/g), as well as their unique mixed phase composites (124 - 329 m(2)/g), these synthetic derivatives are promising model nanoparticles for studies of the bioavailability of poly-aromatic hydrocarbons immobilized in silicate bearing sediments and soils.

  12. Inkjet printing of single-crystal films.

    PubMed

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

    2011-07-13

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

  13. Structural analysis of zeolite NaA synthesized by a cost-effective hydrothermal method using kaolin and its use as water softener.

    PubMed

    Loiola, A R; Andrade, J C R A; Sasaki, J M; da Silva, L R D

    2012-02-01

    Zeolite 4A (LTA) has been successfully synthesized by a hydrothermal method, where kaolin was used as silica and alumina source. The synthesized zeolite was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), laser granulometry, and FTIR spectroscopy. XRD data from the Rietveld refinement method confirmed only one crystallographic phase. Zeolite A morphology was observed by SEM analysis, and it showed well-defined crystals with slightly different sizes but with the same cubic shape. Particle size distribution of the crystals was confirmed by laser granulometry, whereas FTIR spectroscopy revealed significant structural differences between the starting material and the final zeolite product used as water softener. Copyright © 2010 Elsevier Inc. All rights reserved.

  14. Halloysite nanotube-based electrospun ceramic nanofibre mat: a novel support for zeolite membranes

    PubMed Central

    Chen, Zhuwen; Zeng, Jiaying; Lv, Dong; Gao, Jinqiang; Zhang, Jian; Bai, Shan; Li, Ruili; Wu, Jingshen

    2016-01-01

    Some key parameters of supports such as porosity, pore shape and size are of great importance for fabrication and performance of zeolite membranes. In this study, we fabricated millimetre-thick, self-standing electrospun ceramic nanofibre mats and employed them as a novel support for zeolite membranes. The nanofibre mats were prepared by electrospinning a halloysite nanotubes/polyvinyl pyrrolidone composite followed by a programmed sintering process. The interwoven nanofibre mats possess up to 80% porosity, narrow pore size distribution, low pore tortuosity and highly interconnected pore structure. Compared with the commercial α-Al2O3 supports prepared by powder compaction and sintering, the halloysite nanotube-based mats (HNMs) show higher flux, better adsorption of zeolite seeds, adhesion of zeolite membranes and lower Al leaching. Four types of zeolite membranes supported on HNMs have been successfully synthesized with either in situ crystallization or a secondary growth method, demonstrating good universality of HNMs for supporting zeolite membranes. PMID:28083098

  15. Halloysite nanotube-based electrospun ceramic nanofibre mat: a novel support for zeolite membranes

    NASA Astrophysics Data System (ADS)

    Chen, Zhuwen; Zeng, Jiaying; Lv, Dong; Gao, Jinqiang; Zhang, Jian; Bai, Shan; Li, Ruili; Hong, Mei; Wu, Jingshen

    2016-12-01

    Some key parameters of supports such as porosity, pore shape and size are of great importance for fabrication and performance of zeolite membranes. In this study, we fabricated millimetre-thick, self-standing electrospun ceramic nanofibre mats and employed them as a novel support for zeolite membranes. The nanofibre mats were prepared by electrospinning a halloysite nanotubes/polyvinyl pyrrolidone composite followed by a programmed sintering process. The interwoven nanofibre mats possess up to 80% porosity, narrow pore size distribution, low pore tortuosity and highly interconnected pore structure. Compared with the commercial α-Al2O3 supports prepared by powder compaction and sintering, the halloysite nanotube-based mats (HNMs) show higher flux, better adsorption of zeolite seeds, adhesion of zeolite membranes and lower Al leaching. Four types of zeolite membranes supported on HNMs have been successfully synthesized with either in situ crystallization or a secondary growth method, demonstrating good universality of HNMs for supporting zeolite membranes.

  16. Methods of using structures including catalytic materials disposed within porous zeolite materials to synthesize hydrocarbons

    DOEpatents

    Rollins, Harry W [Idaho Falls, ID; Petkovic, Lucia M [Idaho Falls, ID; Ginosar, Daniel M [Idaho Falls, ID

    2011-02-01

    Catalytic structures include a catalytic material disposed within a zeolite material. The catalytic material may be capable of catalyzing a formation of methanol from carbon monoxide and/or carbon dioxide, and the zeolite material may be capable of catalyzing a formation of hydrocarbon molecules from methanol. The catalytic material may include copper and zinc oxide. The zeolite material may include a first plurality of pores substantially defined by a crystal structure of the zeolite material and a second plurality of pores dispersed throughout the zeolite material. Systems for synthesizing hydrocarbon molecules also include catalytic structures. Methods for synthesizing hydrocarbon molecules include contacting hydrogen and at least one of carbon monoxide and carbon dioxide with such catalytic structures. Catalytic structures are fabricated by forming a zeolite material at least partially around a template structure, removing the template structure, and introducing a catalytic material into the zeolite material.

  17. Systems including catalysts in porous zeolite materials within a reactor for use in synthesizing hydrocarbons

    DOEpatents

    Rolllins, Harry W [Idaho Falls, ID; Petkovic, Lucia M [Idaho Falls, ID; Ginosar, Daniel M [Idaho Falls, ID

    2012-07-24

    Catalytic structures include a catalytic material disposed within a zeolite material. The catalytic material may be capable of catalyzing a formation of methanol from carbon monoxide and/or carbon dioxide, and the zeolite material may be capable of catalyzing a formation of hydrocarbon molecules from methanol. The catalytic material may include copper and zinc oxide. The zeolite material may include a first plurality of pores substantially defined by a crystal structure of the zeolite material and a second plurality of pores dispersed throughout the zeolite material. Systems for synthesizing hydrocarbon molecules also include catalytic structures. Methods for synthesizing hydrocarbon molecules include contacting hydrogen and at least one of carbon monoxide and carbon dioxide with such catalytic structures. Catalytic structures are fabricated by forming a zeolite material at least partially around a template structure, removing the template structure, and introducing a catalytic material into the zeolite material.

  18. Solution-processed, Self-organized Organic Single Crystal Arrays with Controlled Crystal Orientation

    PubMed Central

    Kumatani, Akichika; Liu, Chuan; Li, Yun; Darmawan, Peter; Takimiya, Kazuo; Minari, Takeo; Tsukagoshi, Kazuhito

    2012-01-01

    A facile solution process for the fabrication of organic single crystal semiconductor devices which meets the demand for low-cost and large-area fabrication of high performance electronic devices is demonstrated. In this paper, we develop a bottom-up method which enables direct formation of organic semiconductor single crystals at selected locations with desired orientations. Here oriented growth of one-dimensional organic crystals is achieved by using self-assembly of organic molecules as the driving force to align these crystals in patterned regions. Based upon the self-organized organic single crystals, we fabricate organic field effect transistor arrays which exhibit an average field-effect mobility of 1.1 cm2V−1s−1. This method can be carried out under ambient atmosphere at room temperature, thus particularly promising for production of future plastic electronics. PMID:22563523

  19. Microwave-assisted regeneration of synthetic zeolite used in tritium removal systems

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

    Tanaka, M.; Takayama, S.; Sano, S.

    The regeneration process using synthetic honeycomb type 5A zeolite under microwave irradiation was experimentally investigated using a single-mode cavity at 2.46 GHz. In order to investigate the effect of electromagnetic fields, inductive heating by a magnetic field was applied to synthetic zeolite containing water. Because the microwave energy absorbed in the sample was less than 15 W, the zeolite sample was only heated to a temperature of 71 C. degrees. Water desorption was observed based on the increased temperature of the zeolite sample and the thermogravimetric curve that indicated a single step phenomenon. As a result, the regeneration process ofmore » zeolite was not complete over a period of 6000 s. A comparison of dielectric heating by an electric field with inductive heating by a magnetic field showed that the regeneration process by microwave irradiation was particularly beneficial in dielectric heating. (authors)« less

  20. Single Crystal Faceplate Evaluation

    DTIC Science & Technology

    1993-10-25

    conventional powder phosphor. The utility of garnets is amplified by the high state of the art of liquid phase epitaxy ( LPE ). Liquid phase epitaxy of...7]. Much the research at Allied-Signal, Inc. in garnet layer growth has been involved with the kinetics of crystallization of garnet from LPE melts...acceptable resolution and light output characteristics. Single crystal faceplates being evaluated are composed of yttrium aluminum garnet (YAG) with an

  1. Studies on the formation of hierarchical zeolite T aggregates with well-defined morphology in different template systems

    NASA Astrophysics Data System (ADS)

    Yin, Xiaoyan; Chu, Naibo; Lu, Xuewei; Li, Zhongfang; Guo, Hong

    2016-01-01

    In this paper, the disk-like and pumpkin-like hierarchical zeolite T aggregates consisted of primary nano-grains have been hydrothermally synthesized with and without the aid of the second template. The first template is used with tetramethylammonium hydroxide (TMAOH) and the second template is used with triethanolamine (TEA) or polyving akohol (PVA). A combination of characterization techniques, including XRD, SEM, TEM and N2 adsorption-desorption to examine the crystal crystallinity, morphology and surface properties of hierarchical zeolite T aggregates. In the single-template preparation process, the two-step varying-temperature treatment has been used to improve the meso-porosity of zeolite T aggregates. In the double-template preparation process, the amounts of PVA or TEA on the crystallinity, morphology and meso-porosity of zeolite T aggregates have been studied. It has been proved that the interstitial voids between the primary grains of aggregates are the origin of additional mesopores of samples. The micro- and meso-porosities of samples prepared with and without the second template have been contrasted in detail at last. In particular, the sample synthesized with the addition of PVA presents a hierarchical pore structure with the highest Sext value of 122 m2/g and Vmeso value of 0.255 cm3/g.

  2. Anisotropy of nickel-base superalloy single crystals

    NASA Technical Reports Server (NTRS)

    Mackay, R. A.; Dreshfield, R. L.; Maier, R. D.

    1980-01-01

    The influence of orientation on the tensile and stress rupture behavior of 52 Mar-M247 single crystals was studied. Tensile tests were performed at temperatures between 23 and 1093 C; stress rupture behavior was examined between 760 and 1038 C. The mechanical behavior of the single crystals was rationalized on the basis of the Schmid factor contours for the operative slip systems and the lattice rotations which the crystals underwent during deformation. The tensile properties correlated well with the appropriate Schmid factor contours. The stress rupture lives at lower testing temperatures were greatly influenced by the lattice rotations required to produce cross slip. A unified analysis was attained for the stress rupture life data generated for the Mar-M247 single crystals at 760 and 774 C under a stress of 724 MPa and the data reported for Mar-M200 single crystals tested at 760 C under a stress of 689 MPa. Based on this analysis, the stereographic triangle was divided into several regions which were rank ordered according to stress rupture life for this temperature regime.

  3. Moderate-temperature zeolitic alteration in a cooling pyroclastic deposit

    USGS Publications Warehouse

    Levy, S.S.; O'Neil, J.R.

    1989-01-01

    The locally zeolitized Topopah Spring Member of the Paintbrush Tuff (13 Myr.), Yucca Mountain, Nevada, U.S.A., is part of a thick sequence of zeolitized pyroclastic units. Most of the zeolitized units are nonwelded tuffs that were altered during low-temperature diagenesis, but the distribution and textural setting of zeolite (heulandite-clinoptilolite) and smectite in the densely welded Topopah Spring tuff suggest that these hydrous minerals formed while the tuff was still cooling after pyroclastic emplacement and welding. The hydrous minerals are concentrated within a transition zone between devitrified tuff in the central part of the unit and underlying vitrophyre. Movement of liquid and convected heat along fractures from the devitrified tuff to the ritrophyre caused local devitrification and hydrous mineral crystallization. Oxygen isotope geothermometry of cogenetic quartz confirms the nondiagenetic moderate temperature origin of the hydrous minerals at temperatures of ??? 40-100??C, assuming a meteoric water source. The Topopah Spring tuff is under consideration for emplacement of a high-level nuclear waste repository. The natural rock alteration of the cooling pyroclastic deposit may be a good natural analog for repository-induced hydrothermal alteration. As a result of repository thermal loading, temperatures in the Topopah Spring vitrophyre may rise sufficiently to duplicate the inferred temperatures of natural zeolitic alteration. Heated water moving downward from the repository into the vitrophyre may contribute to new zeolitic alteration. ?? 1989.

  4. 3D Study of the Morphology and Dynamics of Zeolite Nucleation.

    PubMed

    Melinte, Georgian; Georgieva, Veselina; Springuel-Huet, Marie-Anne; Nossov, Andreï; Ersen, Ovidiu; Guenneau, Flavien; Gedeon, Antoine; Palčić, Ana; Bozhilov, Krassimir N; Pham-Huu, Cuong; Qiu, Shilun; Mintova, Svetlana; Valtchev, Valentin

    2015-12-07

    The principle aspects and constraints of the dynamics and kinetics of zeolite nucleation in hydrogel systems are analyzed on the basis of a model Na-rich aluminosilicate system. A detailed time-series EMT-type zeolite crystallization study in the model hydrogel system was performed to elucidate the topological and temporal aspects of zeolite nucleation. A comprehensive set of analytical tools and methods was employed to analyze the gel evolution and complement the primary methods of transmission electron microscopy (TEM) and nuclear magnetic resonance (NMR) spectroscopy. TEM tomography reveals that the initial gel particles exhibit a core-shell structure. Zeolite nucleation is topologically limited to this shell structure and the kinetics of nucleation is controlled by the shell integrity. The induction period extends to the moment when the shell is consumed and the bulk solution can react with the core of the gel particles. These new findings, in particular the importance of the gel particle shell in zeolite nucleation, can be used to control the growth process and properties of zeolites formed in hydrogels. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Synthesis Strategies for Ultrastable Zeolite GIS Polymorphs as Sorbents for Selective Separations

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

    Oleksiak, Matthew D.; Ghorbanpour, Arian; Conato, Marlon T.

    Designing nanoporous zeolites with tunable physicochemical properties can substantially impact their performance in commercial applications spanning diverse areas such as adsorption, separations, catalysis, and drug delivery. Zeolite synthesis typically requires the use of an organic structure-directing agent to facilitate the formation of crystals with specific pore size and topology. Attempts to remove organics from syntheses to achieve commercially-viable methods of preparing zeolites often lead to the formation of unwanted crystal polymorphs (i.e., impurities). Here, we present an organic-free synthesis of the small-pore zeolite P (GIS framework topology) that can be selectively tailored to produce two pure polymorphs: P1 and P2.more » To this end, we developed kinetic phase diagrams that identify synthesis compositions leading to the formation of GIS (P1 and P2), as well as their structural analogues MER and PHI. Using a combination of adsorption measurements and density functional theory (DFT) calculations, we also show that both GIS polymorphs are highly selective adsorbents for H2O relative to other light gases (e.g,, H2, N2, CO2). These studies highlight the potential application of GIS materials for dehydration processes, while our findings also refute prior theoretical studies postulating that GIS-type zeolites are excellent materials for CO2 separation/sequestration. Moreover, there is an impetus for discovering novel small-pore zeolites that are shape-selective catalysts for the production of value-added chemicals (e.g., light olefins); thus, our discovery of more thermally-stable P2 opens new avenues for exploring the potential role of this material as a high-performance catalyst.« less

  6. Distributed Feedback Laser Based on Single Crystal Perovskite

    NASA Astrophysics Data System (ADS)

    Sun, Shang; Xiao, Shumin; Song, Qinghai

    2017-06-01

    We demonstrate a single crystal perovskite based, with grating-structured photoresist on top, highly polarized distributed feedback laser. A lower laser threshold than the Fabry-Perot mode lasers from the same single crystal CH3NH3PbBr3 microplate was obtained. Single crystal CH3NH3PbBr3 microplates was synthesized with one-step solution processed precipitation method. Once the photoresist on top of the microplate was patterned with electron beam, the device was realized. This one-step fabrication process utilized the advantage of single crystal to the greatest extend. The ultra-low defect density in single crystalline microplate offer an opportunity for lower threshold lasing action compare with poly-crystal perovskite films. In the experiment, the lasing action based on the distributed feedback grating design was found with lower threshold and higher intensity than the Fabry-Perot mode lasers supported by the flat facets of the same microplate.

  7. Single crystal fibers for high power lasers

    NASA Astrophysics Data System (ADS)

    Kim, W.; Florea, C.; Baker, C.; Gibson, D.; Shaw, L. B.; Bowman, S.; O'Connor, S.; Villalobos, G.; Bayya, S.; Aggarwal, I. D.; Sanghera, J. S.

    2012-11-01

    In this paper, we present our recent results in developing cladded-single crystal fibers for high power single frequency fiber lasers significantly exceeding the capabilities of existing silica fiber based lasers. This fiber laser would not only exploit the advantages of crystals, namely their high temperature stability, high thermal conductivity, superior environmental ruggedness, high propensity for rare earth ion doping and low nonlinearity, but will also provide the benefits from an optical fiber geometry to enable better thermal management thereby enabling the potential for high laser power output in short lengths. Single crystal fiber cores with diameters as small as 35μm have been drawn using high purity rare earth doped ceramic or single crystal feed rods by Laser Heated Pedestal Growth (LHPG) process. The mechanical, optical and morphological properties of these fibers have been characterized. The fibers are very flexible and show good overall uniformity. We also measured the optical loss as well as the non-radiative loss of the doped crystal fibers and the results show that the fibers have excellent optical and morphological quality. The gain coefficient of the crystal fiber matches the low quantum defect laser model and it is a good indication of the high quality of the fibers.

  8. Surface modification of a natural zeolite by treatment with cold oxygen plasma: Characterization and application in water treatment

    NASA Astrophysics Data System (ADS)

    De Velasco-Maldonado, Paola S.; Hernández-Montoya, Virginia; Montes-Morán, Miguel A.; Vázquez, Norma Aurea-Rangel; Pérez-Cruz, Ma. Ana

    2018-03-01

    In the present work the possible surface modification of natural zeolite using cold oxygen plasma was studied. The sample with and without treatment was characterized using nitrogen adsorption isotherms at -196 °C, FT-IR spectroscopy, SEM/EDX analysis and X-Ray Diffraction. Additionally, the two samples were used for the removal of lead and acid, basic, reactive and food dyes in batch systems. The natural zeolite was found to be a mesoporous material with a low specific surface area (23 m2/g). X-ray patterns confirmed that clinoptilolite was the main crystal structure present in the natural zeolite. The molecular properties of dyes and the zeolitic structure were studied using molecular simulation, with the purpose to understand the adsorption mechanism. The results pointed out that only the roughness of the clinoptilolite was affected by the plasma treatment, whereas the specific surface area, chemical functionality and crystal structure remained constant. Finally, adsorption results confirmed that the plasma treatment had no significant effects on the dyes and lead retention capacities of the natural zeolite.

  9. Synthesis and characterization of nanocrystalline mordenite, high silica zeolite RHO, and copper faujasite

    NASA Astrophysics Data System (ADS)

    Hincapie Palacio, Beatriz Omaira

    Mordenite is a zeolite that has been used as a selective adsorbent and as a catalyst. In reactions where the diffusion of reagents into the pore system is the rate-determining step, nanoparticles of the catalyst improve the reaction rate. Mordenite with a crystal diameter smaller than 100 nm has been prepared by the modification of different synthetic parameters such as the source of aluminum, the presence of seeds, the use of low temperatures (150°C vs. 170°C), longer crystallization times (24 h vs. 96 h), and different silica to alumina ratios (10--30). The decrease in the crystal diameter of the prepared mordenite was monitored by the application of the Scherrer equation that relates the broadness of the X-ray diffraction peaks to crystal sizes. Zeolite RHO with an initial silica to alumina ratio (SAR) higher than 20 has been prepared. EDTA, citric acid, and tartaric acid have been used as complexing agents in the synthesis of zeolite RHO. Crystallization time increases (from 48 h to 900 h) with increasing the silica to alumina ratios (SAR) of the initial gel (SAR: 10.8 to 30) and by adding complexing agents. Complexing agents favor the formation of small crystals (0.8 mum) with increased silica to alumina ratio (final SAR: 4.5 vs. 4.0 without complexing agents). The products were characterized by XRD, FESEM, EDX, FTIR, and in-situ XRD. Copper containing faujasite has been successfully prepared for the first time using a direct synthesis method. Ammonium hydroxide was used to form a copper complex that was later mixed with the reacting gel. Crystallization took place at 85°C for 11 days. The copper containing faujasite obtained was characterized by XRD, FESEM, EDX, EPR, FTIR, TPR, and BET. According to the XRD pattern only FAU type zeolite was obtained. According to TPR experiments, the reduction temperature for Cu2+ ions present in Cu-FAU prepared by direct synthesis was 70 K higher than for Cu-FAU prepared by ion-exchange. This difference can be due to the

  10. Removal of ammonium and heavy metals by cost-effective zeolite synthesized from waste quartz sand and calcium fluoride sludge.

    PubMed

    Zhang, Qian; Lin, Bing; Hong, Junming; Chang, Chang-Tang

    2017-02-01

    This study focuses on the effectiveness of zeolite (10% CF-Z [0.5]) hydrothermally synthesized from waste quartz sand and calcium fluoride (CF) for ammonium ion and heavy metal removal. Zeolite was characterized through powder X-ray diffraction, Fourier-transform infrared spectroscopy, micromeritics N 2 adsorption/desorption analysis, and field emission scanning electron microscopy. The effects of CF addition, Si/Al ratio, initial ammonium concentration, solution pH, and temperature on the adsorption of ammonium on 10% CF-Z (0.5) were further examined. Results showed that 10% CF-Z (0.5) was a single-phase zeolite A with cubic-shaped crystals and 10% CF-Z (0.5) efficiently adsorbs ammonium and heavy metals. For instance, 91% ammonium (10 mg L -1 ) and 93% lead (10 mg L -1 ) are removed. The adsorption isotherm, kinetics, and thermodynamics of ammonium adsorption on 10% CF-Z (0.5) were also theoretically analyzed. The adsorption isotherm of ammonium and lead on 10% CF-Z (0.5) in single systems indicated that Freundlich model provides the best fit for the equilibrium data, whereas pseudo-second-order model best describes the adsorption kinetics. The adsorption degree of ions on 10% CF-Z (0.5) in mixed systems exhibits the following pattern: lead > ammonium > cadmium > chromium.

  11. 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).

  12. Crystal structure, spectral, thermal and dielectric studies of a new zinc benzoate single crystal

    NASA Astrophysics Data System (ADS)

    Bijini, B. R.; Prasanna, S.; Deepa, M.; Nair, C. M. K.; Rajendra Babu, K.

    2012-11-01

    Single crystals of zinc benzoate with a novel structure were grown in gel media. Sodium metasilicate of gel density 1.04 g/cc at pH 6 was employed to yield transparent single crystals. The crystal structure of the compound was ascertained by single crystal X-ray diffractometry. It was noted that the crystal belongs to monoclinic system with space group P21/c with unit cell parameters a = 10.669(1) Å, b = 12.995(5) Å, c = 19.119(3) Å, and β = 94.926(3)°. The crystal was seen to possess a linear polymeric structure along b-axis; with no presence of coordinated or lattice water. CHN analysis established the stoichiometric composition of the crystal. The existence of functional groups present in the single crystal system was confirmed by FT-IR studies. The thermal characteristic of the sample was analysed by TGA-DTA techniques, and the sample was found to be thermally stable up to 280 °C. The kinetic and thermodynamic parameters were also determined. UV-Vis spectroscopy corroborated the transparency of the crystal and revealed the optical band gap to be 4 eV. Dielectric studies showed decrease in the dielectric constant of the sample with increase in frequency.

  13. Effect of Crystal Orientation on Fatigue Failure of Single Crystal Nickel Base Turbine Blade Superalloys

    NASA Technical Reports Server (NTRS)

    Arakere, N. K.; Swanson, G.

    2002-01-01

    High cycle fatigue (HCF) induced failures in aircraft gas turbine and rocket engine turbopump blades is a pervasive problem. Single crystal nickel turbine blades are being utilized in rocket engine turbopumps and jet engines throughout industry because of their superior creep, stress rupture, melt resistance, and thermomechanical fatigue capabilities over polycrystalline alloys. Currently the most widely used single crystal turbine blade superalloys are PWA 1480/1493, PWA 1484, RENE' N-5 and CMSX-4. These alloys play an important role in commercial, military and space propulsion systems. Single crystal materials have highly orthotropic properties making the position of the crystal lattice relative to the part geometry a significant factor in the overall analysis. The failure modes of single crystal turbine blades are complicated to predict due to the material orthotropy and variations in crystal orientations. Fatigue life estimation of single crystal turbine blades represents an important aspect of durability assessment. It is therefore of practical interest to develop effective fatigue failure criteria for single crystal nickel alloys and to investigate the effects of variation of primary and secondary crystal orientation on fatigue life. A fatigue failure criterion based on the maximum shear stress amplitude /Delta(sub tau)(sub max))] on the 24 octahedral and 6 cube slip systems, is presented for single crystal nickel superalloys (FCC crystal). This criterion reduces the scatter in uniaxial LCF test data considerably for PWA 1493 at 1200 F in air. Additionally, single crystal turbine blades used in the alternate advanced high-pressure fuel turbopump (AHPFTP/AT) are modeled using a large-scale three-dimensional finite element model. This finite element model is capable of accounting for material orthotrophy and variation in primary and secondary crystal orientation. Effects of variation in crystal orientation on blade stress response are studied based on 297

  14. Synthetic zeolites and other microporous oxide molecular sieves

    PubMed Central

    Sherman, John D.

    1999-01-01

    Use of synthetic zeolites and other microporous oxides since 1950 has improved insulated windows, automobile air-conditioning, refrigerators, air brakes on trucks, laundry detergents, etc. Their large internal pore volumes, molecular-size pores, regularity of crystal structures, and the diverse framework chemical compositions allow “tailoring” of structure and properties. Thus, highly active and selective catalysts as well as adsorbents and ion exchangers with high capacities and selectivities were developed. In the petroleum refining and petrochemical industries, zeolites have made possible cheaper and lead-free gasoline, higher performance and lower-cost synthetic fibers and plastics, and many improvements in process efficiency and quality and in performance. Zeolites also help protect the environment by improving energy efficiency, reducing automobile exhaust and other emissions, cleaning up hazardous wastes (including the Three Mile Island nuclear power plant and other radioactive wastes), and, as specially tailored desiccants, facilitating the substitution of new refrigerants for the ozone-depleting chlorofluorocarbons banned by the Montreal Protocol. PMID:10097059

  15. Synthetic Zeolites and Other Microporous Oxide Molecular Sieves

    NASA Astrophysics Data System (ADS)

    Sherman, John D.

    1999-03-01

    Use of synthetic zeolites and other microporous oxides since 1950 has improved insulated windows, automobile air-conditioning, refrigerators, air brakes on trucks, laundry detergents, etc. Their large internal pore volumes, molecular-size pores, regularity of crystal structures, and the diverse framework chemical compositions allow "tailoring" of structure and properties. Thus, highly active and selective catalysts as well as adsorbents and ion exchangers with high capacities and selectivities were developed. In the petroleum refining and petrochemical industries, zeolites have made possible cheaper and lead-free gasoline, higher performance and lower-cost synthetic fibers and plastics, and many improvements in process efficiency and quality and in performance. Zeolites also help protect the environment by improving energy efficiency, reducing automobile exhaust and other emissions, cleaning up hazardous wastes (including the Three Mile Island nuclear power plant and other radioactive wastes), and, as specially tailored desiccants, facilitating the substitution of new refrigerants for the ozone-depleting chlorofluorocarbons banned by the Montreal Protocol.

  16. 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

  17. Synthesis Strategies for Ultrastable Zeolite GIS Polymorphs as Sorbents for Selective Separations.

    PubMed

    Oleksiak, Matthew D; Ghorbanpour, Arian; Conato, Marlon T; McGrail, B Peter; Grabow, Lars C; Motkuri, Radha Kishan; Rimer, Jeffrey D

    2016-11-02

    Designing zeolites with tunable physicochemical properties can substantially impact their performance in commercial applications, such as adsorption, separations, catalysis, and drug delivery. Zeolite synthesis typically requires an organic structure-directing agent to produce crystals with specific pore topology. Attempts to remove organics from syntheses to achieve commercially viable methods of preparing zeolites often lead to the formation of impurities. Herein, we present organic-free syntheses of two polymorphs of the small-pore zeolite P (GIS), P1 and P2. Using a combination of adsorption measurements and density functional theory calculations, we show that GIS polymorphs are selective adsorbents for H 2 O relative to other light gases (e.g., H 2 , N 2 , CO 2 ). Our findings refute prior theoretical studies postulating that GIS-type zeolites are excellent materials for CO 2 separation/sequestration. We also show that P2 is significantly more thermally stable than P1, which broadens the operating conditions for GIS-type zeolites in commercial applications and opens new avenues for exploring their potential use in processes such as catalysis. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Chiral photonic crystal fibers with single mode and single polarization

    NASA Astrophysics Data System (ADS)

    Li, She; Li, Junqing

    2015-12-01

    Chiral photonic crystal fiber (PCF) with a solid core is numerically investigated by a modified chiral plane-wave expansion method. The effects of structural parameters and chirality strength are analyzed on single-polarization single-mode range and polarization states of guided modes. The simulation demonstrates that the chiral photonic crystal fiber compared to its achiral counterpart possesses another single-circular-polarization operation range, which is located in the short-wavelength region. The original single-polarization operation range in the long-wavelength region extends to the short wavelength caused by introducing chirality. Then this range becomes a broadened one with elliptical polarization from linear polarization. With increase of chirality, the two single-polarization single-mode ranges may fuse together. By optimizing the structure, an ultra-wide single-circular-polarization operation range from 0.5 μm to 1.67 μm for chiral PCF can be realized with moderate chirality strength.

  19. 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.

  20. Magnetic zeolite NaA: synthesis, characterization based on metakaolin and its application for the removal of Cu2+, Pb2+.

    PubMed

    Liu, Haibo; Peng, Shuchuan; Shu, Lin; Chen, Tianhu; Bao, Teng; Frost, Ray L

    2013-06-01

    The optimum parameters for synthesis of zeolite NaA based on metakaolin were investigated according to results of cation exchange capacity and static water adsorption of all synthesis products and selected X-ray diffraction (XRD). Magnetic zeolite NaA was synthesized by adding Fe3O4 in the precursor of zeolite. Zeolite NaA and magnetic zeolite NaA were characterized with scanning electron microscopy (SEM) and XRD. Magnetic zeolite NaA with different Fe3O4 loadings was prepared and used for removal of heavy metals (Cu(2+), Pb(2+)). The results show the optimum parameters for synthesis zeolite NaA are SiO2/Al2O3=2.3, Na2O/SiO2=1.4, H2O/Na2O=50, crystallization time 8h, crystallization temperature 95 °C. The addition of Fe3O4 makes the NaA zeolite with good magnetic susceptibility and good magnetic stability regardless of the Fe3O4 loading, confirming the considerable separation efficiency. Additionally, Fe3O4 loading had a little effect on removal of heavy metal by magnetic zeolite, however, the adsorption capacity still reaches 2.3 mmol g(-1) for Cu(2+), Pb(2+) with a removal efficiency of over 95% in spite of 4.7% Fe3O4 loading. This indicates magnetic zeolite can be used to remove metal heavy at least Cu(2+), Pb(2+) from water with metallic contaminants and can be separated easily after a magnetic process. Copyright © 2013 Elsevier Ltd. All rights reserved.

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

    PubMed Central

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

    2017-01-01

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

  2. Organic field-effect transistors using single crystals.

    PubMed

    Hasegawa, Tatsuo; Takeya, Jun

    2009-04-01

    Organic field-effect transistors using small-molecule organic single crystals are developed to investigate fundamental aspects of organic thin-film transistors that have been widely studied for possible future markets for 'plastic electronics'. In reviewing the physics and chemistry of single-crystal organic field-effect transistors (SC-OFETs), the nature of intrinsic charge dynamics is elucidated for the carriers induced at the single crystal surfaces of molecular semiconductors. Materials for SC-OFETs are first reviewed with descriptions of the fabrication methods and the field-effect characteristics. In particular, a benchmark carrier mobility of 20-40 cm 2 Vs -1 , achieved with thin platelets of rubrene single crystals, demonstrates the significance of the SC-OFETs and clarifies material limitations for organic devices. In the latter part of this review, we discuss the physics of microscopic charge transport by using SC-OFETs at metal/semiconductor contacts and along semiconductor/insulator interfaces. Most importantly, Hall effect and electron spin resonance (ESR) measurements reveal that interface charge transport in molecular semiconductors is properly described in terms of band transport and localization by charge traps.

  3. Effect of Crystal Orientation on Analysis of Single-Crystal, Nickel-Based Turbine Blade Superalloys

    NASA Technical Reports Server (NTRS)

    Swanson, G. R.; Arakere, N. K.

    2000-01-01

    High-cycle fatigue-induced failures in turbine and turbopump blades is a pervasive problem. Single-crystal nickel turbine blades are used because of their superior creep, stress rupture, melt resistance, and thermomechanical fatigue capabilities. Single-crystal materials have highly orthotropic properties making the position of the crystal lattice relative to the part geometry a significant and complicating factor. A fatigue failure criterion based on the maximum shear stress amplitude on the 24 octahedral and 6 cube slip systems is presented for single-crystal nickel superalloys (FCC crystal). This criterion greatly reduces the scatter in uniaxial fatigue data for PWA 1493 at 1,200 F in air. Additionally, single-crystal turbine blades used in the Space Shuttle main engine high pressure fuel turbopump/alternate turbopump are modeled using a three-dimensional finite element (FE) model. This model accounts for material orthotrophy and crystal orientation. Fatigue life of the blade tip is computed using FE stress results and the failure criterion that was developed. Stress analysis results in the blade attachment region are also presented. Results demonstrate that control of crystallographic orientation has the potential to significantly increase a component's resistance to fatigue crack growth without adding additional weight or cost.

  4. Zeolite inorganic scaffolds for novel biomedical application: Effect of physicochemical characteristic of zeolite membranes on cell adhesion and viability

    NASA Astrophysics Data System (ADS)

    Tavolaro, Palmira; Catalano, Silvia; Martino, Guglielmo; Tavolaro, Adalgisa

    2016-09-01

    The design, preparation and selection of inorganic materials useful as functional scaffolds for cell adhesion is a complex question based both on the understanding of the chemical behavior of the materials and individual cells, and on their interactions. Pure zeolite membranes formed from synthetic crystals offer chemically-capable being modulated silanolic surfaces that are amenable to adhesion and growth of fibroblasts. We report the facile preparation of reusable, very longlasting, biocompatible, easily sterilized synthetic scaffolds in a zeolite membrane configuration, which are very stable in aqueous media (apart from ionic strength and pH values), able to adsorb pollutant species and to confine undesired toxic ions (present in culture media). This may ultimately lead to the development of cell supports for economic antibiotic-free culture media.

  5. Single-crystal gallium nitride nanotubes.

    PubMed

    Goldberger, Joshua; He, Rongrui; Zhang, Yanfeng; Lee, Sangkwon; Yan, Haoquan; Choi, Heon-Jin; Yang, Peidong

    2003-04-10

    Since the discovery of carbon nanotubes in 1991 (ref. 1), there have been significant research efforts to synthesize nanometre-scale tubular forms of various solids. The formation of tubular nanostructure generally requires a layered or anisotropic crystal structure. There are reports of nanotubes made from silica, alumina, silicon and metals that do not have a layered crystal structure; they are synthesized by using carbon nanotubes and porous membranes as templates, or by thin-film rolling. These nanotubes, however, are either amorphous, polycrystalline or exist only in ultrahigh vacuum. The growth of single-crystal semiconductor hollow nanotubes would be advantageous in potential nanoscale electronics, optoelectronics and biochemical-sensing applications. Here we report an 'epitaxial casting' approach for the synthesis of single-crystal GaN nanotubes with inner diameters of 30-200 nm and wall thicknesses of 5-50 nm. Hexagonal ZnO nanowires were used as templates for the epitaxial overgrowth of thin GaN layers in a chemical vapour deposition system. The ZnO nanowire templates were subsequently removed by thermal reduction and evaporation, resulting in ordered arrays of GaN nanotubes on the substrates. This templating process should be applicable to many other semiconductor systems.

  6. Ultratough CVD single crystal diamond and three dimensional growth thereof

    DOEpatents

    Hemley, Russell J [Washington, DC; Mao, Ho-kwang [Washington, DC; Yan, Chih-shiue [Washington, DC

    2009-09-29

    The invention relates to a single-crystal diamond grown by microwave plasma chemical vapor deposition that has a toughness of at least about 30 MPa m.sup.1/2. The invention also relates to a method of producing a single-crystal diamond with a toughness of at least about 30 MPa m.sup.1/2. The invention further relates to a process for producing a single crystal CVD diamond in three dimensions on a single crystal diamond substrate.

  7. 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

  8. High-quality bulk hybrid perovskite single crystals within minutes by inverse temperature crystallization

    NASA Astrophysics Data System (ADS)

    Saidaminov, Makhsud I.; Abdelhady, Ahmed L.; Murali, Banavoth; Alarousu, Erkki; Burlakov, Victor M.; Peng, Wei; Dursun, Ibrahim; Wang, Lingfei; He, Yao; Maculan, Giacomo; Goriely, Alain; Wu, Tom; Mohammed, Omar F.; Bakr, Osman M.

    2015-07-01

    Single crystals of methylammonium lead trihalide perovskites (MAPbX3; MA=CH3NH3+, X=Br- or I-) have shown remarkably low trap density and charge transport properties; however, growth of such high-quality semiconductors is a time-consuming process. Here we present a rapid crystal growth process to obtain MAPbX3 single crystals, an order of magnitude faster than previous reports. The process is based on our observation of the substantial decrease of MAPbX3 solubility, in certain solvents, at elevated temperatures. The crystals can be both size- and shape-controlled by manipulating the different crystallization parameters. Despite the rapidity of the method, the grown crystals exhibit transport properties and trap densities comparable to the highest quality MAPbX3 reported to date. The phenomenon of inverse or retrograde solubility and its correlated inverse temperature crystallization strategy present a major step forward for advancing the field on perovskite crystallization.

  9. Attenuation of thermal neutrons by an imperfect single crystal

    NASA Astrophysics Data System (ADS)

    Naguib, K.; Adib, M.

    1996-06-01

    A semi-empirical formula is given which allows one to calculate the total thermal cross section of an imperfect single crystal as a function of crystal constants, temperature and neutron energy E, in the energy range between 3 meV and 10 eV. The formula also includes the contribution of the parasitic Bragg scattering to the total cross section that takes into account the crystal mosaic spread value and its orientation with respect to the neutron beam direction. A computer program (ISCANF) was developed to calculate the total attenuation of neutrons using the proposed formula. The ISCANF program was applied to investigate the neutron attenuation through a copper single crystal. The calculated values of the neutron transmission through the imperfect copper single crystal were fitted to the measured ones in the energy range 3 - 40 meV at different crystal orientations. The result of fitting shows that use of the computer program ISCANF allows one to predict the behaviour of the total cross section of an imperfect copper single crystal for the whole energy range.

  10. How far could energy transport within a single crystal

    NASA Astrophysics Data System (ADS)

    Zhang, Yifan; Che, Yanke; Zhao, Jincai; Steve, Granick

    Efficient transport of excitation energy over long distance is a vital process in light-harvesting systems and molecular electronics. The energy transfer distance is largely restricted by the probability decay of the exciton when hopping within a single crystal. Here, we fabricated an organic single crystal within which the energy could transfer more than 100 μm, a distance only limited by its crystal size. Our system could be regarded as a ``Sprint relay game'' performing on different surface of tracks. Photoinduced ``athletes'' (excitons) triggered intermolecular ``domino'' reaction to propagate energy for a long distance. In addition, athletes with the same ability runs much farther on smooth ideal track (single crystal assembled from merely van der Waals interaction) than bumpy mud track (crystal assembled from combination of pi-stacking, hydrogen bond and van der Waals interactions). Our finding presents new physics on enhancing energy transfer length within a single crystal. Current Affiliation: Institute for Basic Science, South Korea.

  11. Synthesis of novel perfluoroalkylglucosides on zeolite and non-zeolite catalysts.

    PubMed

    Nowicki, Janusz; Mokrzycki, Łukasz; Sulikowski, Bogdan

    2015-04-08

    Perfluoroalkylglucosides comprise a very important class of fluorine-containing surfactants. These compounds can be synthesized by using the Fisher reaction, starting directly from glucose and the required perfluoroalcohols. We wish to report on the use of zeolite catalysts of different structure and composition for the synthesis of perfluoroalkylglucosides when using glucose and 1-octafluoropentanol as substrates. Zeolites of different pore architecture have been chosen (ZSM-5, ZSM-12, MCM-22 and Beta). Zeolites were characterized by XRD, nitrogen sorption, scanning electron microscopy (SEM) and solid-state 27Al MAS NMR spectroscopy. The activity of the zeolite catalysts in the glycosidation reaction was studied in a batch reactor at 100 °C below atmospheric pressure. The performance of zeolites was compared to other catalysts, an ion-exchange resin (Purolite) and a montmorillonite-type layered aluminosilicate. The catalytic performance of zeolite Beta was the highest among the zeolites studied and the results were comparable to those obtained over Purolite and montmorillonite type catalysts.

  12. Application of natural zeolite for phosphorus and ammonium removal from aqueous solutions.

    PubMed

    Karapinar, Nuray

    2009-10-30

    Removal of both nutrients ammonium and phosphorus by natural zeolite has been studied in lab scale by using a mechanically stirred batch system (1000 ml). Zeolite, a mean particle size of 13 microm, was used as an adsorbent for the removal of ammonium and then as a seed material for the precipitation of calcium phosphate. A relationship was established between the uptake of ammonium by zeolite and the ratio of initial ammonium concentration to zeolite dosage. Ammonium uptake of zeolite was almost completed within initial 5 min of adsorption period. There is no pronounced effect of zeolite and ammonium, neither positive nor negative on the amount of calcium phosphate precipitation. The extent of the precipitation of phosphate increased with rising pH. It was also observed that when the system was allowed to relax at constant pH (i.e. under relatively low super saturations), a certain lag time was noted to elapse at the onset of the precipitation. At the pH 7.2, the amount of initial fast precipitation within 5 min and total precipitation within 120 min were around 34% and 93%, respectively. Precipitation of calcium phosphate on to ammonium-loaded zeolite was achieved at low super saturations (< pH 7.5) through secondary nucleation and crystal growth, leading to an increase in particle size.

  13. Development of a Single-Crystal Fifth-Generation Nickel Superalloy

    NASA Astrophysics Data System (ADS)

    Petrushin, N. V.; Elyutin, E. S.; Visik, E. M.; Golynets, S. A.

    2017-11-01

    The chemical and phase compositions of a rhenium-ruthenium-containing fifth-generation VZhM8 nickel superalloy, which is intended for single-crystal turbine blades of an aviation engine, are calculated using computer simulation. VZhM8 alloy <001>, <011>, and <111> single crystals are fabricated. The microstructure, the γ/γ' misfit, the segregation coefficients of alloying elements, the dissolution temperature of the γ' phase, and the solidus and liquidus temperatures of the VZhM8 alloy single crystals in the as-cast state and after heat treatment are studied. The temperature-time dependences of the static elastic modulus, the short-term mechanical properties, and the long-term strength of the alloy single crystals are determined

  14. Organic field-effect transistors using single crystals

    PubMed Central

    Hasegawa, Tatsuo; Takeya, Jun

    2009-01-01

    Organic field-effect transistors using small-molecule organic single crystals are developed to investigate fundamental aspects of organic thin-film transistors that have been widely studied for possible future markets for ‘plastic electronics’. In reviewing the physics and chemistry of single-crystal organic field-effect transistors (SC-OFETs), the nature of intrinsic charge dynamics is elucidated for the carriers induced at the single crystal surfaces of molecular semiconductors. Materials for SC-OFETs are first reviewed with descriptions of the fabrication methods and the field-effect characteristics. In particular, a benchmark carrier mobility of 20–40 cm2 Vs−1, achieved with thin platelets of rubrene single crystals, demonstrates the significance of the SC-OFETs and clarifies material limitations for organic devices. In the latter part of this review, we discuss the physics of microscopic charge transport by using SC-OFETs at metal/semiconductor contacts and along semiconductor/insulator interfaces. Most importantly, Hall effect and electron spin resonance (ESR) measurements reveal that interface charge transport in molecular semiconductors is properly described in terms of band transport and localization by charge traps. PMID:27877287

  15. Refinement of the crystal structures of biomimetic weddellites produced by microscopic fungus Aspergillus niger

    NASA Astrophysics Data System (ADS)

    Rusakov, A. V.; Frank-Kamenetskaya, O. V.; Gurzhiy, V. V.; Zelenskaya, M. S.; Izatulina, A. R.; Sazanova, K. V.

    2014-05-01

    The single-crystal structures of four biomimetic weddellites CaC2O4 · (2 + x)H2O with different contents of zeolitic water ( x = 0.10-0.24 formula units) produced by the microscopic fungus Aspergillus niger were refined from X-ray diffraction data ( R = 0.029-0.038). The effect of zeolitic water content on the structural stability of weddellite was analyzed. The parameter a was shown to increase with increasing x due to the increase in the distance between water molecules along this direction. The water content and structural parameters of the synthesized weddellites are similar to those of weddellites from biofilms and kidney stones.

  16. Low-cost single-crystal turbine blades, volume 2

    NASA Technical Reports Server (NTRS)

    Strangman, T. E.; Dennis, R. E.; Heath, B. R.

    1984-01-01

    The overall objectives of Project 3 were to develop the exothermic casting process to produce uncooled single-crystal (SC) HP turbine blades in MAR-M 247 and higher strength derivative alloys and to validate the materials process and components through extensive mechanical property testing, rig testing, and 200 hours of endurance engine testing. These Program objectives were achieved. The exothermic casting process was successfully developed into a low-cost nonproperietary method for producing single-crystal castings. Single-crystal MAR-M 247 and two derivatives DS alloys developed during this project, NASAIR 100 and SC Alloy 3, were fully characterized through mechanical property testing. SC MAR-M 247 shows no significant improvement in strength over directionally solidified (DS) MAR-M 247, but the derivative alloys, NASAIR 100 and Alloy 3, show significant tensile and fatigue improvements. Firtree testing, holography, and strain-gauge rig testing were used to determine the effects of the anisotropic characteristics of single-crystal materials. No undesirable characteristics were found. In general, the single-crystal material behaved similarly to DS MAR-M 247. Two complete engine sets of SC HP turbine blades were cast using the exothermic casting process and fully machined. These blades were successfully engine-tested.

  17. The energetics of mesopore formation in zeolites with surfactants.

    PubMed

    Linares, Noemi; Jardim, Erika de Oliveira; Sachse, Alexander; Serrano, Elena; Garcia-Martinez, Javier

    2018-05-02

    Mesoporosity can be conveniently introduced in zeolites by treating them in basic surfactant solutions. The apparent activation energy involved in the formation of mesopores in USY via surfactant-templating was obtained through the combination of in situ synchrotron XRD and ex situ gas adsorption. Additionally, techniques such as pH measurements and TG/DTA were employed to determine the OH- evolution and the CTA+ uptake during the development of mesoporosity, providing information about the different steps involved. By combining both in situ and ex situ techniques, we have been able, for the first time, to determine the apparent activation energies of the different processes involved in the mesostructuring of USY zeolites, which are in the same order of magnitude (30 - 65 kJ mol-1) of those involved in the crystallization of zeolites. Hence, important mechanistic insights on the surfactant-templating method were obtained. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Electrical characteristics of organic perylene single-crystal-based field-effect transistors

    NASA Astrophysics Data System (ADS)

    Lee, Jin-Woo; Kang, Han-Saem; Kim, Min-Ki; Kim, Kihyun; Cho, Mi-Yeon; Kwon, Young-Wan; Joo, Jinsoo; Kim, Jae-Il; Hong, Chang-Seop

    2007-12-01

    We report on the fabrication of organic field-effect transistors (OFETs) using perylene single crystal as the active material and their electrical characteristics. Perylene single crystals were directly grown from perylene powder in a furnace using a relatively short growth time of 1-3 h. The crystalline structure of the perylene single crystals was characterized by means of a single-crystal x-ray diffractometer. In order to place the perylene single crystal onto the Au electrodes of the field-effect transistor, a polymethlymethacrylate thin layer was spin-coated on top of the crystal surface. The OFETs fabricated using the perylene single crystal showed a typical p-type operating mode. The field-effect mobility of the perylene crystal based OFETs was measured to be ˜9.62×10-4 cm2/V s at room temperature. The anisotropy of the mobility implying the existence of different mobilities when applying currents in different directions was observed for the OFETs, and the existence of traps in the perylene crystal was found through the measurements of the temperature-dependent mobility at various operating drain voltages.

  19. Growth and nonlinear optical characterization of organic single crystal films

    NASA Astrophysics Data System (ADS)

    Zhou, Ligui

    1997-12-01

    Organic single crystal films are important for various future applications in photonics and integrated optics. The conventional method for inorganic crystal growth is not suitable for organic materials, and the high temperature melting method is not good for most organic materials due to decomposition problems. We developed a new method-modified shear method-to grow large area organic single crystal thin films which have exceptional nonlinear optical properties and high quality surfaces. Several organic materials (NPP, PNP and DAST) were synthesized and purified before the thin film crystal growth. Organic single crystal thin films were grown from saturated organic solutions using modified shear method. The area of single crystal films were about 1.5 cm2 for PNP, 1 cm2 for NPP and 5 mm2 for DAST. The thickness of the thin films which could be controlled by the applied pressure ranged from 1μm to 10 μm. The single crystal thin films of organic materials were characterized by polarized microscopy, x-ray diffraction, polarized UV-Visible and polarized micro-FTIR spectroscopy. Polarized microscopy showed uniform birefringence and complete extinction with the rotation of the single crystal thin films under crossed- polarization, which indicated high quality single crystals with no scattering. The surface orientation of single crystal thin films was characterized by x-ray diffraction. The molecular orientation within the crystal was further studied by the polarized UV-Visible and Polarized micro-FTIR techniques combined with the x-ray and polarized microscopy results. A Nd:YAG laser with 35 picosecond pulses at 1064nm wavelength was employed to perform the nonlinear optical characterization of the organic single crystal thin films. Two measurement techniques were used to study the crystal films: second harmonic generation (SHG) and electro-optic (EO) effect. SHG results showed that the nonlinear optical coefficient of NPP was 18 times that of LiNbO3, a standard

  20. 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.

  1. Solar cell structure incorporating a novel single crystal silicon material

    DOEpatents

    Pankove, Jacques I.; Wu, Chung P.

    1983-01-01

    A novel hydrogen rich single crystal silicon material having a band gap energy greater than 1.1 eV can be fabricated by forming an amorphous region of graded crystallinity in a body of single crystalline silicon and thereafter contacting the region with atomic hydrogen followed by pulsed laser annealing at a sufficient power and for a sufficient duration to recrystallize the region into single crystal silicon without out-gassing the hydrogen. The new material can be used to fabricate semiconductor devices such as single crystal silicon solar cells with surface window regions having a greater band gap energy than that of single crystal silicon without hydrogen.

  2. Numerical study of slip system activity and crystal lattice rotation under wedge nanoindents in tungsten single crystals

    NASA Astrophysics Data System (ADS)

    Volz, T.; Schwaiger, R.; Wang, J.; Weygand, S. M.

    2018-05-01

    Tungsten is a promising material for plasma facing components in future nuclear fusion reactors. In the present work, we numerically investigate the deformation behavior of unirradiated tungsten (a body-centered cubic (bcc) single crystal) underneath nanoindents. A finite element (FE) model is presented to simulate wedge indentation. Crystal plasticity finite element (CPFE) simulations were performed for face-centered and body-centered single crystals accounting for the slip system family {110} <111> in the bcc crystal system and the {111} <110> slip family in the fcc system. The 90° wedge indenter was aligned parallel to the [1 ¯01 ]-direction and indented the crystal in the [0 1 ¯0 ]-direction up to a maximum indentation depth of 2 µm. In both, the fcc and bcc single crystals, the activity of slip systems was investigated and compared. Good agreement with the results from former investigations on fcc single crystals was observed. Furthermore, the in-plane lattice rotation in the material underneath an indent was determined and compared for the fcc and bcc single crystals.

  3. 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.

  4. Three-Dimensional Conformation of Folded Polymers in Single Crystals

    NASA Astrophysics Data System (ADS)

    Hong, You-lee; Yuan, Shichen; Li, Zhen; Ke, Yutian; Nozaki, Koji; Miyoshi, Toshikazu

    2015-10-01

    The chain-folding mechanism and structure of semicrystalline polymers have long been controversial. Solid-state NMR was applied to determine the chain trajectory of 13C CH3 -labeled isotactic poly(1-butene) (i PB 1 ) in form III chiral single crystals blended with nonlabeled i PB 1 crystallized in dilute solutions under low supercooling. An advanced 13C - 13C double-quantum NMR technique probing the spatial proximity pattern of labeled 13C nuclei revealed that the chains adopt a three-dimensional (3D) conformation in single crystals. The determined results indicate a two-step crystallization process of (i) cluster formation via self-folding in the precrystallization stage and (ii) deposition of the nanoclusters as a building block at the growth front in single crystals.

  5. Selective Metal Cation Capture by Soft Anionic Metal-Organic Frameworks via Drastic Single-Crystal-to-Single-Crystal Transformations

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

    Tian, Jian; Saraf, Laxmikant V.; Schwenzer, Birgit

    2012-05-25

    Flexible anionic metal-organic frameworks transform to neutral heterobimetallic systems via single-crystal-to-single-crystal processes invoked by cation insertion. These transformations are directed by cooperative bond breakage and formation, resulting in expansion or contraction of the 3D framework by up to 33% due to the flexible nature of the organic linker. These MOFs displays highly selective uptake of divalent transition metal cations (Co2+ and Ni2+ for example) over alkali metal cations (Li+ and Na+).

  6. Selective Ring Opening of 1-Methylnaphthalene Over NiW-Supported Catalyst Using Dealuminated Beta Zeolite.

    PubMed

    Kim, Eun-Sang; Lee, You-Jin; Kim, Jeong-Rang; Kim, Joo-Wan; Kim, Tae-Wan; Chae, Ho-Jeong; Kim, Chul-Ung; Lee, Chang-Ha; Jeong, Soon-Yong

    2016-02-01

    Nanoporous Beta zeolite was dealuminated by weak acid treatment for reducing the acidity. Bi-functional catalysts were prepared using commercial Beta zeolites and the dealuminated zeolites for acidic function, NiW for metallic function. 1-Methylnaphthalene was selected as a model compound for multi-ring aromatics in heavy oil, and its selective ring opening reaction has been investigated using the prepared bi-functional catalysts with different acidity in fixed bed reaction system. The dealuminated Beta zeolites, which crystal structure and nanoporosity were maintained, showed the higher SiO2/Al2O3 ratio and smaller acidity than their original zeolite. NiW-supported catalyst using the dealuminated Beta zeolite with SiO2/Al203 mole ratio of 55 showed the highest performance for the selective ring opening. The acidity of catalyst seemed to play an important role as active sites for the selective ring opening of 1-methylnaphthalene but there should be some optimum catalyst acidity for the reaction. The acidity of Beta zeolite could be controlled by the acid treatment and the catalyst with the optimum acidity for the selective ring opening could be prepared.

  7. High quality factor single-crystal diamond mechanical resonators

    NASA Astrophysics Data System (ADS)

    Ovartchaiyapong, P.; Pascal, L. M. A.; Myers, B. A.; Lauria, P.; Bleszynski Jayich, A. C.

    2012-10-01

    Single-crystal diamond is a promising material for microelectromechanical systems (MEMs) because of its low mechanical loss, compatibility with extreme environments, and built-in interface to high-quality spin centers. But its use has been limited by challenges in processing and growth. We demonstrate a wafer bonding-based technique to form diamond on insulator, from which we make single-crystal diamond micromechanical resonators with mechanical quality factors as high as 338 000 at room temperature. Variable temperature measurements down to 10 K reveal a nonmonotonic dependence of quality factor on temperature. These resonators enable integration of single-crystal diamond into MEMs technology for classical and quantum applications.

  8. 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.

  9. Gallium arsenide single crystal solar cell structure and method of making

    NASA Technical Reports Server (NTRS)

    Stirn, Richard J. (Inventor)

    1983-01-01

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

  10. Modified floating-zone growth of organic single crystals

    NASA Astrophysics Data System (ADS)

    Kou, S.; Chen, C. P.

    1994-04-01

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

  11. Methylcellulose-Directed Synthesis of Nanocrystalline Zeolite NaA with High CO₂ Uptake.

    PubMed

    Shakarova, Dilshod; Ojuva, Arto; Bergström, Lennart; Akhtar, Farid

    2014-07-28

    Zeolite NaA nanocrystals with a narrow particle size distribution were prepared by template-free hydrothermal synthesis in thermo-reversible methylcellulose gels. The effects of the amount of methylcellulose, crystallization time and hydrothermal treatment temperature on the crystallinity and particle size distribution of the zeolite NaA nanocrystals were investigated. We found that the thermogelation of methylcellulose in the alkaline Na₂O-SiO₂-Al₂O₃-H₂O system played an important role in controlling the particle size. The synthesized zeolite nanocrystals are highly crystalline, as demonstrated by X-ray diffraction (XRD), and scanning electron microscopy (SEM) shows that the nanocrystals can also display a well-defined facetted morphology. Gas adsorption studies on the synthesized nanocrystalline zeolite NaA showed that nanocrystals with a size of 100 nm displayed a high CO₂ uptake capacity (4.9 mmol/g at 293 K at 100 kPa) and a relatively rapid uptake rate compared to commercially available, micron-sized particles. Low-cost nanosized zeolite adsorbents with a high and rapid uptake are important for large scale gas separation processes, e.g., carbon capture from flue gas.

  12. Chemical potential of water from measurements of optic axial angle of zeolites

    USGS Publications Warehouse

    Donald, Eberlein G.; Christ, C.L.

    1968-01-01

    Values of the uncorrected optic axial angle (2H??) of a crystal of the calcium zeolite stellerite (CaAl2Si7O 18 ?? 7H2O) immersed in calcium chloride solutions of known activity of water (aw) are directly proportional to log aw. A general relationship between the chemical potential of water in the crystal and the optic axial angle is obeyed.

  13. Investigating the Influence of Temperature on the Kaolinite-Base Synthesis of Zeolite and Urease Immobilization for the Potential Fabrication of Electrochemical Urea Biosensors.

    PubMed

    Anderson, David Ebo; Balapangu, Srinivasan; Fleischer, Heidimarie N A; Viade, Ruth A; Krampa, Francis D; Kanyong, Prosper; Awandare, Gordon A; Tiburu, Elvis K

    2017-08-08

    Temperature-dependent zeolite synthesis has revealed a unique surface morphology, surface area and pore size which influence the immobilization of urease on gold electrode supports for biosensor fabrication. XRD characterization has identified zeolite X (Na) at all crystallization temperatures tested. However, N₂ adsorption and desorption results showed a pore size and pore volume of zeolite X (Na) 60 °C, zeolite X (Na) 70 °C and zeolite X (Na) 90 °C to range from 1.92 nm to 2.45 nm and 0.012 cm³/g to 0.061 cm³/g, respectively, with no significant differences. The specific surface area of zeolite X (Na) at 60, 70 and 90 °C was 64 m²/g, 67 m²/g and 113 m²/g, respectively. The pore size, specific surface area and pore volumes of zeolite X (Na) 80 °C and zeolite X (Na) 100 °C were dramatically increased to 4.21 nm, 295 m²/g, 0.762 cm³/g and 4.92 nm, 389 m²/g, 0.837 cm³/g, in that order. The analytical performance of adsorbed urease on zeolite X (Na) surface was also investigated using cyclic voltammetry measurements, and the results showed distinct cathodic and anodic peaks by zeolite X (Na) 80 °C and zeolite X (Na) 100 °C. These zeolites' molar conductance was measured as a function of urea concentration and gave an average polynomial regression fit of 0.948. The findings in this study suggest that certain physicochemical properties, such as crystallization temperature and pH, are critical parameters for improving the morphological properties of zeolites synthesized from natural sources for various biomedical applications.

  14. Method for the growth of large low-defect single crystals

    NASA Technical Reports Server (NTRS)

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

    2008-01-01

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

  15. Capillarity creates single-crystal calcite nanowires from amorphous calcium carbonate.

    PubMed

    Kim, Yi-Yeoun; Hetherington, Nicola B J; Noel, Elizabeth H; Kröger, Roland; Charnock, John M; Christenson, Hugo K; Meldrum, Fiona C

    2011-12-23

    Single-crystal calcite nanowires are formed by crystallization of morphologically equivalent amorphous calcium carbonate (ACC) particles within the pores of track etch membranes. The polyaspartic acid stabilized ACC is drawn into the membrane pores by capillary action, and the single-crystal nature of the nanowires is attributed to the limited contact of the intramembrane ACC particle with the bulk solution. The reaction environment then supports transformation to a single-crystal product. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Titanium-containing zeolites and microporous molecular sieves as photovoltaic solar cells.

    PubMed

    Atienzar, Pedro; Valencia, Susana; Corma, Avelino; García, Hermenegildo

    2007-05-14

    Four titanium-containing zeolites and microporous molecular sieves differing on the crystal structure and particle size (Ti/Beta, Ti/Beta-60, TS-1 and ETS-10) are prepared, and their activity for solar cells after incorporating N3 (a commercially available ruthenium polypyridyl dye) is tested. All the zeolites exhibit photovoltaic activity, and the photoresponse is quite independent of the zeolite pore dimensions or particle size. The photoresponse increases with titanium content in the range 1-7% wt. In this way, cells are obtained that have open-circuit voltage Voc=560 mV and maximum short-circuit photocurrent density Isc=100 microA, measured for 1x1 cm2 surfaces with a solar simulator at 1000 W through and AM 1.5 filter. These values are promising and comparable to those obtained for current dye-sensitized titania solar cells.

  17. One-step synthesis of mesoporous pentasil zeolite with single-unit-cell lamellar structural features

    DOEpatents

    Tsapstsis, Michael; Zhang, Xueyi

    2015-11-17

    A method for making a pentasil zeolite material includes forming an aqueous solution that includes a structure directing agent and a silica precursor; and heating the solution at a sufficient temperature and for sufficient time to form a pentasil zeolite material from the silica precursor, wherein the structure directing agent includes a quaternary phosphonium ion.

  18. Large single domain 123 material produced by seeding with single crystal rare earth barium copper oxide single crystals

    DOEpatents

    Todt, V.; Miller, D.J.; Shi, D.; Sengupta, S.

    1998-07-07

    A method of fabricating bulk YBa{sub 2}Cu{sub 3}O{sub x} where compressed powder oxides and/or carbonates of Y and Ba and Cu present in mole ratios to form YBa{sub 2}Cu{sub 3}O{sub x} are heated in the presence of a Nd{sub 1+x}Ba{sub 2{minus}x}Cu{sub 3}O{sub y} seed crystal to a temperature sufficient to form a liquid phase in the YBa{sub 2}Cu{sub 3}O{sub x} while maintaining the seed crystal solid. The materials are slowly cooled to provide a YBa{sub 2}Cu{sub 3}O{sub x} material having a predetermined number of domains between 1 and 5. Crack-free single domain materials can be formed using either plate shaped seed crystals or cube shaped seed crystals with a pedestal of preferential orientation material. 7 figs.

  19. Large single domain 123 material produced by seeding with single crystal rare earth barium copper oxide single crystals

    DOEpatents

    Todt, Volker; Miller, Dean J.; Shi, Donglu; Sengupta, Suvankar

    1998-01-01

    A method of fabricating bulk YBa.sub.2 Cu.sub.3 O.sub.x where compressed powder oxides and/or carbonates of Y and Ba and Cu present in mole ratios to form YBa.sub.2 Cu.sub.3 O.sub.x are heated in the presence of a Nd.sub.1+x Ba.sub.2-x Cu.sub.3 O.sub.y seed crystal to a temperature sufficient to form a liquid phase in the YBa.sub.2 Cu.sub.3 O.sub.x while maintaining the seed crystal solid. The materials are slowly cooled to provide a YBa.sub.2 Cu.sub.3 O.sub.x material having a predetermined number of domains between 1 and 5. Crack-free single domain materials can be formed using either plate shaped seed crystals or cube shaped seed crystals with a pedestal of preferential orientation material.

  20. Analytical studies on the crystal melt interface shape in the Czochralski process for oxide single crystals

    NASA Astrophysics Data System (ADS)

    Jeong, Ja Hoon; Kang, In Seok

    2000-09-01

    Effects of the operating conditions on the crystal-melt interface shape are analytically investigated for the Czochralski process of the oxide single crystals. The ideas, which were used for the silicon single-crystal growth by Jeong et al. (J. Crystal Growth 177 (1997) 157), are extended to the oxide single-crystal growth problem by considering the internal radiation in the crystal phase and the melt phase heat transfer with the high Prandtl number. The interface shape is approximated in the simplest form as a quadratic function of radial position and an expression for the deviation from the flat interface shape is derived as a function of operating conditions. The radiative heat transfer rate between the interface and the ambient is computed by calculating the view factors for the curved interface shape with the assumption that the crystal phase is completely transparent. For the melt phase, the well-known results from the thermal boundary layer analysis are applied for the asymptotic case of high Prandtl number based on the idea that the flow field near the crystal-melt interface can be modeled as either a uniaxial or a biaxial flow. Through this work, essential information on the interface shape deformation and the effects of operating conditions are brought out for the oxide single-crystal growth.

  1. The Effect of an Ultrasound Radiation on the Synthesis of 4A Zeolite from Fly Ash

    NASA Astrophysics Data System (ADS)

    Susanto, H.; Imani, N. A. C.; Aslamiyah, N. R.; Istirokhatun, T.; Robbani, M. H.

    2018-05-01

    The use of coal as a fuel source generates a lot of solid waste fly ash. Thus, efforts to reduce or utilize the amount of fly ash are urgently needed. This paper presents zeolite synthesis from fly ash. The fly ash was activated by using NaOH solution prior to fusing process with a weight ratio of 1:2 and mixing with distilled water at a weight ratio of 1:5. Thereafter, the addition of alumina with a concentration of 0.71 %, 1.42 %, 2.12 %, and 2.8 % w/v was performed. The effects of heating and ultrasound radiation on the characteristic of zeolite products were investigated. The results showed that the addition of alumina 2.8 % w/v resulted in the Si/Al ratio of zeolite 4A is ∼1. SEM images demonstrated that the presence of ultrasound wave resulted in crystals structure morphology as also supported by XRD characterization. The average crystal size for the ultrasonic treatment was 42.46 nm.

  2. Zeolite formation from coal fly ash and its adsorption potential

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

    Duangkamol Ruen-ngam; Doungmanee Rungsuk; Ronbanchob Apiratikul

    The possibility in converting coal fly ash (CFA) to zeolite was evaluated. CFA samples from the local power plant in Prachinburi province, Thailand, were collected during a 3-month time span to account for the inconsistency of the CFA quality, and it was evident that the deviation of the quality of the raw material did not have significant effects on the synthesis. The zeolite product was found to be type X. The most suitable weight ratio of sodium hydroxide (NaOH) to CFA was approximately 2.25, because this gave reasonably high zeolite yield with good cation exchange capacity (CEC). The silica (Si)-to-aluminummore » (Al) molar ratio of 4.06 yielded the highest crystallinity level for zeolite X at 79% with a CEC of 240 meq/100 g and a surface area of 325 m{sup 2}/g. Optimal crystallization temperature and time were 90{sup o}C and 4 hr, respectively, which gave the highest CEC of approximately 305 meq/100 g. Yields obtained from all experiments were in the range of 50-72%. 29 refs., 5 tabs., 7 figs.« less

  3. Low-cost single-crystal turbine blades, volume 1

    NASA Technical Reports Server (NTRS)

    Strangman, T. E.; Heath, B.; Fujii, M.

    1983-01-01

    The exothermic casting process was successfully developed into a low cost nonproprietary method for producing single crystal (SC) castings. Casting yields were lower than expected, on the order of 20 percent, but it is felt that the casting yield could be significantly improved with minor modifications to the process. Single crystal Mar-M 247 and two derivative SC alloys were developed. NASAIR 100 and SC Alloy 3 were fully characterized through mechanical property testing. SC Mar-M 247 shows no significant improvement in strength over directionally solidified (DS) Mar-M 247, but the derivative alloys, NASAIR 100 and Alloy 3, show significant tensile and fatigue improvements. The 1000 hr/238 MPa (20 ksi) stress rupture capability compared to DS Mar-M 247 was improved over 28 C. Firtree testing, holography, and strain gauge rig testing were used to evaluate the effects of the anisotropic characteristics of single crystal materials. In general, the single crystal material behaved similarly to DS Mar-M 247. Two complete engine sets of SC HP turbine blades were cast using the exothermic casting process and fully machined.

  4. Single crystals of metal solid solutions

    NASA Technical Reports Server (NTRS)

    Miller, J. F.; Austin, A. E.; Richard, N.; Griesenauer, N. M.; Moak, D. P.; Mehrabian, M. R.; Gelles, S. H.

    1974-01-01

    The following definitions were sought in the research on single crystals of metal solid solutions: (1) the influence of convection and/or gravity present during crystallization on the substructure of a metal solid solution; (2) the influence of a magnetic field applied during crystallization on the substructure of a metal solid solution; and (3) requirements for a space flight experiment to verify the results. Growth conditions for the selected silver-zinc alloy system are described, along with pertinent technical and experimental details of the project.

  5. Template-Framework Interactions in Tetraethylammonium-Directed Zeolite Synthesis

    DOE PAGES

    Schmidt, Joel E.; Fu, Donglong; Deem, Michael W.; ...

    2016-11-22

    Zeolites, having widespread applications in chemical industries, are often synthesized using organic templates. These can be cost-prohibitive, motivating investigations into their role in promoting crystallization. Herein, the relationship between framework structure, chemical composition, synthesis conditions and the conformation of the occluded, economical template tetraethylammonium (TEA +) has been systematically examined by experimental and computational means. The results show two distinct regimes of occluded conformer tendencies: 1) In frameworks with a large stabilization energy difference, only a single conformer was found (BEA, LTA and MFI). 2) In the frameworks with small stabilization energy differences (AEI, AFI, CHA and MOR), less thanmore » the interconversion of TEA + in solution, a heteroatom-dependent (Al, B, Co, Mn, Ti, Zn) distribution of conformers was observed. Our findings demonstrate that host–guest chemistry principles, including electrostatic interactions and coordination chemistry, are as important as ideal pore-filling.« less

  6. Performance of Nitrogen and Phosphorus Removal in Petrochemical Wastewater by Zeolited Fly Ash

    NASA Astrophysics Data System (ADS)

    Li, Zheng; Gu, Guizhou; Ji, Shenghao

    2018-05-01

    The zeolitized fly ash was synthesized by alkali melt hydrothermal method. The cation exchange capacity of zeolitized fly ash was far greater than the raw material fly ash. The main component was NaP1 zeolite (Na6Al6Si10O32·12H2O), followed by mullite, and a small amount of heterozygous crystals. The effect of synthetic zeolite dosage, pH value, adsorption time and reaction temperature on the effect of nitrogen and phosphorus removal in petrochemical wastewater were investigated. The results showed that when the zeolitized fly ash dosage was 9 g/L, the petrochemical wastewater pH value was 6∼8, adsorption time was 30 min and the reaction temperature was 30°C, the synthetic zeolite had the best effect on the removal of TN and TP in petrochemical wastewater, and the removal was 65.5%, 91.4% respectively. Besides, the concentrations of TN and TP in the effluent were 11.04 mg/L, 0.31 mg/L respectively. The concentrations met the sewage discharge standard in petrochemical industry of "Liaoning sewage comprehensive discharge standard" (DB21 1627-2008). This study was to realize the comprehensive utilization of solid waste and achieve the purpose of waste and waste.

  7. Single crystal functional oxides on silicon

    PubMed Central

    Bakaul, Saidur Rahman; Serrao, Claudy Rayan; Lee, Michelle; Yeung, Chun Wing; Sarker, Asis; Hsu, Shang-Lin; Yadav, Ajay Kumar; Dedon, Liv; You, Long; Khan, Asif Islam; Clarkson, James David; Hu, Chenming; Ramesh, Ramamoorthy; Salahuddin, Sayeef

    2016-01-01

    Single-crystalline thin films of complex oxides show a rich variety of functional properties such as ferroelectricity, piezoelectricity, ferro and antiferromagnetism and so on that have the potential for completely new electronic applications. Direct synthesis of such oxides on silicon remains challenging because of the fundamental crystal chemistry and mechanical incompatibility of dissimilar interfaces. Here we report integration of thin (down to one unit cell) single crystalline, complex oxide films onto silicon substrates, by epitaxial transfer at room temperature. In a field-effect transistor using a transferred lead zirconate titanate layer as the gate insulator, we demonstrate direct reversible control of the semiconductor channel charge with polarization state. These results represent the realization of long pursued but yet to be demonstrated single-crystal functional oxides on-demand on silicon. PMID:26853112

  8. Investigating the Influence of Temperature on the Kaolinite-Base Synthesis of Zeolite and Urease Immobilization for the Potential Fabrication of Electrochemical Urea Biosensors

    PubMed Central

    Anderson, David Ebo; Balapangu, Srinivasan; Fleischer, Heidimarie N. A.; Viade, Ruth A.; Awandare, Gordon A.; Tiburu, Elvis K.

    2017-01-01

    Temperature-dependent zeolite synthesis has revealed a unique surface morphology, surface area and pore size which influence the immobilization of urease on gold electrode supports for biosensor fabrication. XRD characterization has identified zeolite X (Na) at all crystallization temperatures tested. However, N2 adsorption and desorption results showed a pore size and pore volume of zeolite X (Na) 60 °C, zeolite X (Na) 70 °C and zeolite X (Na) 90 °C to range from 1.92 nm to 2.45 nm and 0.012 cm3/g to 0.061 cm3/g, respectively, with no significant differences. The specific surface area of zeolite X (Na) at 60, 70 and 90 °C was 64 m2/g, 67 m2/g and 113 m2/g, respectively. The pore size, specific surface area and pore volumes of zeolite X (Na) 80 °C and zeolite X (Na) 100 °C were dramatically increased to 4.21 nm, 295 m2/g, 0.762 cm3/g and 4.92 nm, 389 m2/g, 0.837 cm3/g, in that order. The analytical performance of adsorbed urease on zeolite X (Na) surface was also investigated using cyclic voltammetry measurements, and the results showed distinct cathodic and anodic peaks by zeolite X (Na) 80 °C and zeolite X (Na) 100 °C. These zeolites’ molar conductance was measured as a function of urea concentration and gave an average polynomial regression fit of 0.948. The findings in this study suggest that certain physicochemical properties, such as crystallization temperature and pH, are critical parameters for improving the morphological properties of zeolites synthesized from natural sources for various biomedical applications. PMID:28786961

  9. Hydrogen induced fracture characteristics of single crystal nickel-based superalloys

    NASA Technical Reports Server (NTRS)

    Chen, Po-Shou; Wilcox, Roy C.

    1990-01-01

    A stereoscopic method for use with x ray energy dispersive spectroscopy of rough surfaces was adapted and applied to the fracture surfaces single crystals of PWA 1480E to permit rapid orientation determinations of small cleavage planes. The method uses a mathematical treatment of stereo pair photomicrographs to measure the angle between the electron beam and the surface normal. One reference crystal orientation corresponding to the electron beam direction (crystal growth direction) is required to perform this trace analysis. The microstructure of PWA 1480E was characterized before fracture analysis was performed. The fracture behavior of single crystals of the PWA 1480E nickel-based superalloy was studied. The hydrogen-induced fracture behavior of single crystals of the PWA 1480E nickel-based superalloy was also studied. In order to understand the temperature dependence of hydrogen-induced embrittlement, notched single crystals with three different crystal growth orientations near zone axes (100), (110), and (111) were tensile tested at 871 C (1600 F) in both helium and hydrogen atmospheres at 34 MPa. Results and conclusions are given.

  10. Mesopore quality determines the lifetime of hierarchically structured zeolite catalysts

    NASA Astrophysics Data System (ADS)

    Milina, Maria; Mitchell, Sharon; Crivelli, Paolo; Cooke, David; Pérez-Ramírez, Javier

    2014-05-01

    Deactivation due to coking limits the lifetime of zeolite catalysts in the production of chemicals and fuels. Superior performance can be achieved through hierarchically structuring the zeolite porosity, yet no relation has been established between the mesopore architecture and the catalyst lifetime. Here we introduce a top-down demetallation strategy to locate mesopores in different regions of MFI-type crystals with identical bulk porous and acidic properties. In contrast, well-established bottom-up strategies as carbon templating and seed silanization fail to yield materials with matching characteristics. Advanced characterization tools capable of accurately discriminating the mesopore size, distribution and connectivity are applied to corroborate the concept of mesopore quality. Positron annihilation lifetime spectroscopy proves powerful to quantify the global connectivity of the intracrystalline pore network, which, as demonstrated in the conversions of methanol or of propanal to hydrocarbons, is closely linked to the lifetime of zeolite catalysts. The findings emphasize the need to aptly tailor hierarchical materials for maximal catalytic advantage.

  11. Anisotropic Piezocomposite Actuator Incorporating Machined PMN-PT Single Crystal Fibers

    NASA Technical Reports Server (NTRS)

    Wilkie, W. Keats; Inman, Daniel J.; Lloyd, Justin M.; High, James W.

    2004-01-01

    The design, fabrication, and testing of a flexible, planar, anisotropic piezoelectric composite actuator utilizing machined PMN-32%PT single crystal fibers is presented. The device consists of a layer of rectangular single crystal piezoelectric fibers in an epoxy matrix, packaged between interdigitated electrode polyimide films. Quasistatic free-strain measurements of the single crystal device are compared with measurements from geometrically identical specimens incorporating polycrystalline PZT-5A and PZT-5H piezoceramic fibers. Free-strain actuation of the single crystal actuator at low bipolar electric fields (+/- 250 V/mm) is approximately 400% greater than that of the baseline PZT-5A piezoceramic device, and 200% greater than that of the PZT-5H device. Free-strain actuation under high unipolar electric fields (0-4kV/mm) is approximately 200% of the PZT-5A baseline device, and 150% of the PZT-5H alternate piezoceramic device. Performance increases at low field are qualitatively consistent with predicted increases based on scaling the low-field d(sub 33) piezoelectric constants of the respective piezoelectric materials. High-field increases are much less than scaled d(sub 33) estimates, but appear consistent with high-field freestrain measurements reported for similar bulk single-crystal and piezoceramic compositions. Measurements of single crystal actuator capacitance and coupling coefficient are also provided. These properties were poorly predicted using scaled bulk material dielectric and coupling coefficient data. Rules-of-mixtures calculations of the effective elastic properties of the single crystal device and estimated actuation work energy densities are also presented. Results indicate longitudinal stiffnesses significantly lower (50% less) than either piezoceramic device. This suggests that single-crystal piezocomposite actuators will be best suited to low induced-stress, high strain and deflection applications.

  12. Synthesis of ZSM-23/ZSM-22 intergrowth zeolite with a novel dual-template strategy

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

    Wang, Bingchun, E-mail: wangbc@dicp.ac.cn; Graduate University of Chinese Academy of Sciences, Beijing 100049; Tian, Zhijian, E-mail: tianz@dicp.ac.cn

    2009-12-15

    ZSM-23/ZSM-22 intergrowth zeolite with fixed proportion of 60%ZSM-23/40%ZSM-22 has been synthesized with a novel dual-template strategy. The products were characterized by X-ray diffraction and scanning electron microscopy. Dimethylamine and diethylamine were used together as a dual-template system. The molar ratio of diethylamine to dimethylamine, which was changed with the type of aluminum source, was the key factor for the synthesis of intergrowth zeolites. A molar ratio of diethylamine to dimethylamine of 1:24 could result in an ZSM-23/ZSM-22 intergrowth zeolite if aluminum sulfate was used as aluminum source, whereas a molar ratio of diethylamine to dimethylamine of 1:12 was required tomore » get an ZSM-23/ZSM-22 intergrowth zeolite if sodium metaaluminate was used. Furthermore, fluoride anion could be involved in the process as a crystallization promoter.« less

  13. A low temperature furnace for solution crystal growth on the International Space Station

    NASA Astrophysics Data System (ADS)

    Baç, Nurcan; Harpster, Joseph; Maston, Robert A.; Sacco, Albert

    2000-01-01

    The Zeolite Crystal Growth Furnace Unit (ZCG-FU) is the first module in an integrated payload designed for low temperature crystal growth in solutions on the International Space Station (ISS). This payload is scheduled to fly on the ISS flight 7A.1 in an EXPRESS rack. Its name originated from early shuttle flight experiments limited to the growth of zeolite crystals but has since grown to include other materials of significant commercial interest using the solution method of crystal growth. Zeolites, ferroelectrics, piezeoelectrics and silver halides are some of the materials considered. The ZCG-FU experiment consists of a furnace unit and its electronic control system, and mechanically complex, crystal growth autoclaves suitable for use with a particular furnace and solution. The ZCG facility is being designed to grow into four independent furnaces controlled by IZECS (Improved Zeolite Electronic Control System). IZECS provides monitoring of critical parameters, data logging, safety monitoring, air-to-ground control and operator interfacing. It is suitable for controlling the four furnaces either individually or all at one time. It also contains the power management solid-state drivers and switches for the ZCG-FU furnace. The furnace contains 19 tubes operating at three different temperature zones. .

  14. Single crystal micromechanical resonator and fabrication methods thereof

    DOEpatents

    Olsson, Roy H.; Friedmann, Thomas A.; Homeijer, Sara Jensen; Wiwi, Michael; Hattar, Khalid Mikhiel; Clark, Blythe; Bauer, Todd; Van Deusen, Stuart B.

    2016-12-20

    The present invention relates to a single crystal micromechanical resonator. In particular, the resonator includes a lithium niobate or lithium tantalate suspended plate. Also provided are improved microfabrication methods of making resonators, which does not rely on complicated wafer bonding, layer fracturing, and mechanical polishing steps. Rather, the methods allow the resonator and its components to be formed from a single crystal.

  15. Improved growth method of (SN) x single crystals

    NASA Astrophysics Data System (ADS)

    Nakada, Ichiroh

    1981-12-01

    The crystal growth of pure and sizable single crystals of polysulfur nitride (SN) x was improved by adopting a monitor system with a quadrapole mass spectrometer and a Pirani gauge. The mass spectrometer helped to find a temperature appropriate for trapping (SN) 2 selectively on a cold finger and removing other unnecessary or harmful materials produced by the thermal decomposition of (SN) 4 as well as out-gassing water vapour from the glass wall. Leakage of gasses in the vessel was monitored with the Pirani gauge. With a heat pipe the crystal tube is cooled locally so that only a small number of nuclei start to grow. (SN) x single crystals with dimensions of 1 to 6 mm in edge size have been obtained. The relation between the crystal habit and the crystallographic axes has also been determined.

  16. Hydraulic conductivity of compacted zeolites.

    PubMed

    Oren, A Hakan; Ozdamar, Tuğçe

    2013-06-01

    Hydraulic conductivities of compacted zeolites were investigated as a function of compaction water content and zeolite particle size. Initially, the compaction characteristics of zeolites were determined. The compaction test results showed that maximum dry unit weight (γ(dmax)) of fine zeolite was greater than that of granular zeolites. The γ(dmax) of compacted zeolites was between 1.01 and 1.17 Mg m(-3) and optimum water content (w(opt)) was between 38% and 53%. Regardless of zeolite particle size, compacted zeolites had low γ(dmax) and high w(opt) when compared with compacted natural soils. Then, hydraulic conductivity tests were run on compacted zeolites. The hydraulic conductivity values were within the range of 2.0 × 10(-3) cm s(-1) to 1.1 × 10(-7) cm s(-1). Hydraulic conductivity of all compacted zeolites decreased almost 50 times as the water content increased. It is noteworthy that hydraulic conductivity of compacted zeolite was strongly dependent on the zeolite particle size. The hydraulic conductivity decreased almost three orders of magnitude up to 39% fine content; then, it remained almost unchanged beyond 39%. Only one report was found in the literature on the hydraulic conductivity of compacted zeolite, which is in agreement with the findings of this study.

  17. 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.

  18. Tailored zeolites for the removal of metal oxyanions: overcoming intrinsic limitations of zeolites.

    PubMed

    Figueiredo, Hugo; Quintelas, Cristina

    2014-06-15

    This review aims to present a global view of the efforts conducted to convert zeolites into efficient supports for the removal of heavy metal oxyanions. Despite lacking affinity for these species, due to inherent charge repulsion between zeolite framework and anionic species, zeolites have still received considerable attention from the scientific community, since their versatility allowed tailoring them to answer specific requirements. Different processes for the removal and recovery of toxic metals based on zeolites have been presented. These processes resort to modification of the zeolite surface to allow direct adsorption of oxyanions, or by combination with reducing agents for oxyanions that allow ion-exchange with the converted species by the zeolite itself. In order to testify zeolite versatility, as well as covering the wide array of physicochemical constraints that oxyanions offer, chromium and arsenic oxyanions were selected as model compounds for a review of treatment/remediation strategies, based on zeolite modification. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Molecular simulation of water removal from simple gases with zeolite NaA.

    PubMed

    Csányi, Eva; Ható, Zoltán; Kristóf, Tamás

    2012-06-01

    Water vapor removal from some simple gases using zeolite NaA was studied by molecular simulation. The equilibrium adsorption properties of H(2)O, CO, H(2), CH(4) and their mixtures in dehydrated zeolite NaA were computed by grand canonical Monte Carlo simulations. The simulations employed Lennard-Jones + Coulomb type effective pair potential models, which are suitable for the reproduction of thermodynamic properties of pure substances. Based on the comparison of the simulation results with experimental data for single-component adsorption at different temperatures and pressures, a modified interaction potential model for the zeolite is proposed. In the adsorption simulations with mixtures presented here, zeolite exhibits extremely high selectivity of water to the investigated weakly polar/non-polar gases demonstrating the excellent dehydration ability of zeolite NaA in engineering applications.

  20. 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.

  1. 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.

  2. 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.

  3. The Load Capability of Piezoelectric Single Crystal Actuators

    NASA Technical Reports Server (NTRS)

    Xu, Tian-Bing; Su, Ji; Jiang, Xiaoning; Rehrig, Paul W.; Hackenberger, Wesley S.

    2006-01-01

    Piezoelectric lead magnesium niobate-lead titanate (PMN-PT) single crystal is one of the most promising materials for electromechanical device applications due to its high electrical field induced strain and high electromechanical coupling factor. PMN-PT single crystal-based multilayer stack actuators and multilayer stack-based flextensional actuators have exhibited high stroke and high displacement-voltage ratios. The actuation capabilities of these two actuators were evaluated using a newly developed method based upon a laser vibrometer system under various loading conditions. The measured displacements as a function of mechanical loads at different driving voltages indicate that the displacement response of the actuators is approximately constant under broad ranges of mechanical load. The load capabilities of these PMN-PT single crystal-based actuators and the advantages of the capability for applications will be discussed.

  4. The Load Capability of Piezoelectric Single Crystal Actuators

    NASA Technical Reports Server (NTRS)

    Xu, Tian-Bing; Su, Ji; Jiang, Xiaoning; Rehrig, Paul W.; Hackenberger, Wesley S.

    2007-01-01

    Piezoelectric lead magnesium niobate-lead titanate (PMN-PT) single crystal is one of the most promising materials for electromechanical device applications due to its high electrical field induced strain and high electromechanical coupling factor. PMN-PT single crystal-based multilayer stack actuators and multilayer stack-based flextensional actuators have exhibited high stroke and high displacement-voltage ratios. The actuation capabilities of these two actuators were evaluated using a newly developed method based upon a laser vibrometer system under various loading conditions. The measured displacements as a function of mechanical loads at different driving voltages indicate that the displacement response of the actuators is approximately constant under broad ranges of mechanical load. The load capabilities of these PMN-PT single crystal-based actuators and the advantages of the capability for applications will be discussed.

  5. Demonstration of single crystal growth via solid-solid transformation of a glass

    DOE PAGES

    Savytskii, Dmytro; Knorr, Brian; Dierolf, Volkmar; ...

    2016-03-18

    Many advanced technologies have relied on the availability of single crystals of appropriate material such as silicon for microelectronics or superalloys for turbine blades. Similarly, many promising materials could unleash their full potential if they were available in a single crystal form. However, the current methods are unsuitable for growing single crystals of these oftentimes incongruently melting, unstable or metastable materials. Here we demonstrate a strategy to overcome this hurdle by avoiding the gaseous or liquid phase, and directly converting glass into a single crystal. Specifically, Sb 2S 3 single crystals are grown in Sb-S-I glasses as an example ofmore » this approach. In this first unambiguous demonstration of an all-solid-state glass → crystal transformation, extraneous nucleation is avoided relative to crystal growth via spatially localized laser heating and inclusion of a suitable glass former in the composition. Lastly, the ability to fabricate patterned single-crystal architecture on a glass surface is demonstrated, providing a new class of micro-structured substrate for low cost epitaxial growth, active planar devices, etc.« less

  6. Effective removal of hydrogen sulfide using 4A molecular sieve zeolite synthesized from attapulgite.

    PubMed

    Liu, Xinpeng; Wang, Rui

    2017-03-15

    In this work, 4A molecular sieve zeolite was synthesized from attapulgite (ATP) in different conditions and was applied initially for H 2 S removal. The sorbent was characterized by scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectra and N 2 adsorption/desorption. The effects of the synthesis condition and adsorption temperature were studied by dynamic adsorption experiment. The optimal adsorption temperature is 50°C. The H 2 S adsorption results have showed that the optimal synthesis conditions are as follows: the ratio of silicon to aluminum and ratio of sodium to silicon are both 1.5, the ratio of water to sodium is 30, crystallization temperature and crystallization time is 90°C, 4h, respectively. The breakthrough and saturation sulfur sorption capacities of zeolite synthesized under optimum conditions are up to nearly 10 and 15mg/g-sorbent, respectively, and the H 2 S removal rate is nearly 100%. The adsorption kinetics nonlinear fitting results show that the adsorption system follows Bingham model. These results indicate that 4A molecular sieve zeolite synthesized from attapulgite can be used for H 2 S removal promisingly. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Laser-Heated Floating Zone Production of Single-Crystal Fibers

    NASA Technical Reports Server (NTRS)

    Ritzert, Frank; Westfall, Leonard

    1996-01-01

    This report describes how a laser-heated floating zone apparatus can be used to investigate single-crystal fibers of various compositions. A feedrod with a stoichiometric composition of high-purity powders was connected to a pedestal and fed into a laser scan where it combined with a single-crystal fiber seed. A molten zone was formed at this junction. As the feedrod was continuously fed into the laser scan, a single-crystal fiber of a prescribed orientation was withdrawn from the melt. The resultant fibers, whose diameters ranged from 100 to 250 gm, could then be evaluated on the basis of their growth behavior, physical properties, mechanical properties, and fiber perfection.

  8. 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.

  9. Single crystal and optical ceramic multicomponent garnet scintillators: A comparative study

    NASA Astrophysics Data System (ADS)

    Wu, Yuntao; Luo, Zhaohua; Jiang, Haochuan; Meng, Fang; Koschan, Merry; Melcher, Charles L.

    2015-04-01

    Multicomponent garnet materials can be made in optical ceramic as well as single crystal form due to their cubic crystal structure. In this work, high-quality Gd3Ga3Al2O12:0.2 at% Ce (GGAG:Ce) single crystal and (Gd,Lu)3Ga3Al2O12:1 at% Ce (GLuGAG:Ce) optical ceramics were fabricated by the Czochralski method and a combination of hot isostatic pressing (HIPing) and annealing treatment, respectively. Under optical and X-ray excitation, the GLuGAG:Ce optical ceramic exhibits a broad Ce3+ transition emission centered at 550 nm, while the emission peak of the GGAG:Ce single crystal is centered at 540 nm. A self-absorption effect in GLuGAG:Ce optical ceramic results in this red-shift of the Ce3+ emission peak compared to that in the GGAG:Ce single crystal. The light yield under 662 keV γ-ray excitation was 45,000±2500 photons/MeV and 48,200±2410 photons/MeV for the GGAG:Ce single crystal and GLuGAG:Ce optical ceramic, respectively. An energy resolution of 7.1% for 662 keV γ-rays was achieved in the GLuGAG:Ce optical ceramic with a Hamamatsu R6231 PMT, which is superior to the value of 7.6% for a GGAG:Ce single crystal. Scintillation decay time measurements under 137Cs irradiation show two exponential decay components of 58 ns (47%) and 504 ns (53%) for the GGAG:Ce single crystal, and 84 ns (76%) and 148 ns (24%) for the GLuGAG:Ce optical ceramic. The afterglow level after X-ray cutoff in the GLuGAG:Ce optical ceramic is at least one order of magnitude lower than in the GGAG:Ce single crystal.

  10. Polymethylated [4.1.1] Octanes Leading to Zeolite SSZ-50

    NASA Astrophysics Data System (ADS)

    Lee, Greg S.; Zones, Stacey I.

    2002-09-01

    In this communication, we report on the discovery of novel zeolite compositions, SSZ-50. The zeolite has the RTH topology but can be made over a large silica-to-alumina range including no aluminum at all. The surprising capability to produce a broad compositional range comes from the use of a single organo-cation guest molecule in the zeolite synthesis. The molecule is a specific derivative from within a family of 2-aza [4.1.1] bicyclo octanes that were prepared employing a sequence of organic synthesis steps from a starting ketone. Other cage-based zeolites like SSZ-35,-36,-39 and MTN arose from the use of the other derivatives in this series. We also comment on the tendency of a variety of polymethylated organo-cations to produce RTH, the closely related ITE, or the intergrowth structure, SSZ-36.

  11. Single-Crystal Structure of a Covalent Organic Framework

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

    Zhang, YB; Su, J; Furukawa, H

    2013-11-06

    The crystal structure of a new covalent organic framework, termed COF-320, is determined by single-crystal 3D electron diffraction using the rotation electron diffraction (RED) method for data collection. The COF crystals are prepared by an imine condensation of tetra-(4-anilyl)methane and 4,4'-biphenyldialdehyde in 1,4-dioxane at 120 degrees C to produce a highly porous 9-fold interwoven diamond net. COF-320 exhibits permanent porosity with a Langmuir surface area of 2400 m(2)/g and a methane total uptake of 15.0 wt % (176 cm(3)/cm(3)) at 25 degrees C and 80 bar. The successful determination of the structure of COF-320 directly from single-crystal samples is anmore » important advance in the development of COF chemistry.« less

  12. Anisotropy of Single-Crystal Silicon in Nanometric Cutting.

    PubMed

    Wang, Zhiguo; Chen, Jiaxuan; Wang, Guilian; Bai, Qingshun; Liang, Yingchun

    2017-12-01

    The anisotropy exhibited by single-crystal silicon in nanometric cutting is very significant. In order to profoundly understand the effect of crystal anisotropy on cutting behaviors, a large-scale molecular dynamics model was conducted to simulate the nanometric cutting of single-crystal silicon in the (100)[0-10], (100)[0-1-1], (110)[-110], (110)[00-1], (111)[-101], and (111)[-12-1] crystal directions in this study. The simulation results show the variations of different degrees in chip, subsurface damage, cutting force, and friction coefficient with changes in crystal plane and crystal direction. Shear deformation is the formation mechanism of subsurface damage, and the direction and complexity it forms are the primary causes that result in the anisotropy of subsurface damage. Structurally, chips could be classified into completely amorphous ones and incompletely amorphous ones containing a few crystallites. The formation mechanism of the former is high-pressure phase transformation, while the latter is obtained under the combined action of high-pressure phase transformation and cleavage. Based on an analysis of the material removal mode, it can be found that compared with the other crystal direction on the same crystal plane, the (100)[0-10], (110)[-110], and (111)[-101] directions are more suitable for ductile cutting.

  13. Fabrication of MTN-type zeolite by self-assembling of supramolecular compound

    NASA Astrophysics Data System (ADS)

    Huang, Aisheng; Caro, Jürgen

    2009-10-01

    MTN-type (Zeolite Socony Mobil Thirty-Nine) zeolite was prepared at 473 K by a novel method through self-assembling of a supramolecular compound called 2,4,6-tris (4-pyridyl) triazine (TPT) in DMF (N,N-dimethylformamide). The effects of fluoride, DMF and germanium on the synthesis of MTN-type zeolite were investigated. The crystallization was facilitated by adding fluoride to the synthesis solution, resulting in the formation of highly crystalline MTN samples, while some amorphous phase was observed in fluoride-free batches. DMF was required to obtain a highly crystalline MTN sample, since TPT dissolves easier in DMF than in water, thus facilitating the self-assembling of TPT into a 3D network to structure the MTN framework. The MTN structure could be synthesized at low germanium content (Ge/Si≤0.18), while AST (AlPO 4-sixteen) as a foreign phase is formed at high germanium substitution (Ge/Si≥0.5).

  14. Single crystalline hollow metal-organic frameworks: a metal-organic polyhedron single crystal as a sacrificial template.

    PubMed

    Kim, Hyehyun; Oh, Minhak; Kim, Dongwook; Park, Jeongin; Seong, Junmo; Kwak, Sang Kyu; Lah, Myoung Soo

    2015-02-28

    Single crystalline hollow metal-organic frameworks (MOFs) with cavity dimensions on the order of several micrometers and hundreds of micrometers were prepared using a metal-organic polyhedron single crystal as a sacrificial hard template. The hollow nature of the MOF crystal was confirmed by scanning electron microscopy of the crystal sliced using a focused ion beam.

  15. Zeolites in Eocene basaltic pillow lavas of the Siletz River Volcanics, Central Coast Range, Oregon

    USGS Publications Warehouse

    Keith, Terry E.C.; Staplese, Lloyd W.

    1985-01-01

    Zeolites and associated minerals occur in a tholeiitic basaltic pillow lava sequence that makes up part of the Eocene Siletz River Volcanics in the central Coast Range, Oregon. Regional zoning of zeolite assemblages is not apparent; the zeolites formed in joints, fractures, and interstices, although most occur in central cavities of basalt pillows. The zeolites and associated minerals identified, in general order of paragenetic sequence, are smectite, pyrite, calcite (small spheres), thomsonite, natrolite, analcime, scolecite, mesolite, stilbite, heulandite, apophyllite, chahazite, mordenite, calcite (scalenohedra and twinned rhombohedra), laumontite, and amethystine quartz. Common three-mineral assemblages are: natrolite-analcime-sfilbite, stilbite-heulandite-chabazite, stilbite-apophyllie-chabazite, and natrolite-mesolite-laumontite.Alteration of basaltic glass, which was initially abundant, appears to have been an important factor in formation of the zeolites. Isotopic data suggest that zeolitization occurred during a low-temperature (60 ~ 70°C submarine hydrothermal event, or by reactions of cold (~ 10°C meteoric water with basalt over a long time. The occurrence of different mineral assemblages in cavities of adjacent basalt pillows indicates that these minerals crystallized in dosed systems that were isolated as fractures and joints were sealed by deposition of smectite and early zeolites. Although the total chemical composition of the mineral assemblages in cavities is similar, different mineral species formed because of the sensitivity of zeolite minerals to slight variations in physical and chemical conditions within individual cavities.

  16. Synthesis of high-silica EU-1 zeolite in the presence of hexamethonium ions: a seeded approach for inhibiting ZSM-48.

    PubMed

    Xu, Qinghu; Gong, Yanjun; Xu, Wenjing; Xu, Jun; Deng, Feng; Dou, Tao

    2011-06-01

    A seeded approach was developed to synthesize high-silica EU-1 zeolite via inhibiting the co-crystallization of ZSM-48 in the presence of hexamethonium (HM) ions. A systematic study was carried out to determine factors such as seed content and SiO(2)/Al(2)O(3) ratio, which influenced the crystallization of high-silica EU-1 and transformation of EU-1 into ZSM-48. Using EU-1 seeds, not only well-crystallized pure EU-1 zeolites with SiO(2)/Al(2)O(3) ratios more than 500 were synthesized, but also the co-crystalline of ZSM-48/EU-1 or pure ZSM-48 was obtained in control from silica-rich mixture gels. Furthermore, the kinetic features of the seeded synthesis of EU-1 zeolites with SiO(2)/Al(2)O(3) ratios of 55, 190, and 500 were examined. It was found that seeds played crucial roles in the decrease of apparent activation energy of EU-1 nucleation and inhibiting the transformation of EU-1 into ZSM-48. The HM and Al species performed synergistic roles to inhibit the formation ZSM-48 during high-silica EU-1 nucleation and crystal growth. Copyright © 2011 Elsevier Inc. All rights reserved.

  17. Single-Crystal Diamond Nanobeam Waveguide Optomechanics

    NASA Astrophysics Data System (ADS)

    Khanaliloo, Behzad; Jayakumar, Harishankar; Hryciw, Aaron C.; Lake, David P.; Kaviani, Hamidreza; Barclay, Paul E.

    2015-10-01

    Single-crystal diamond optomechanical devices have the potential to enable fundamental studies and technologies coupling mechanical vibrations to both light and electronic quantum systems. Here, we demonstrate a single-crystal diamond optomechanical system and show that it allows excitation of diamond mechanical resonances into self-oscillations with amplitude >200 nm . The resulting internal stress field is predicted to allow driving of electron spin transitions of diamond nitrogen-vacancy centers. The mechanical resonances have a quality factor >7 ×105 and can be tuned via nonlinear frequency renormalization, while the optomechanical interface has a 150 nm bandwidth and 9.5 fm /√{Hz } sensitivity. In combination, these features make this system a promising platform for interfacing light, nanomechanics, and electron spins.

  18. Secondary orientation effects in a single crystal superalloy under mechanical and thermal loads

    NASA Technical Reports Server (NTRS)

    Kalluri, Sreeramesh; Abdul-Aziz, Ali; Mcgaw, Michael A.

    1991-01-01

    The nickel-base single crystal superalloy PWA 1480 is a candidate blading material for the advanced turbopump development program of the SSME. In order to improve thermal fatigue resistance of the turbine blades, the single crystal superalloy PWA 1480 is grown along the low modulus zone axes (001) crystal orientation by a directional solidification process. Since cubic single crystal materials such as PWA 1480 exhibit anisotropic elastic behavior, the stresses developed within the single crystal superalloy due to mechanical and thermal loads are likely to be affected by the exact orientation of the secondary crystallographic direction with respect to the geometry of the turbine blade. The effects of secondary crystal orientation on the elastic response of single crystal PWA 1480 superalloy were investigated.

  19. Seeded growth of boron arsenide single crystals with high thermal conductivity

    NASA Astrophysics Data System (ADS)

    Tian, Fei; Song, Bai; Lv, Bing; Sun, Jingying; Huyan, Shuyuan; Wu, Qi; Mao, Jun; Ni, Yizhou; Ding, Zhiwei; Huberman, Samuel; Liu, Te-Huan; Chen, Gang; Chen, Shuo; Chu, Ching-Wu; Ren, Zhifeng

    2018-01-01

    Materials with high thermal conductivities are crucial to effectively cooling high-power-density electronic and optoelectronic devices. Recently, zinc-blende boron arsenide (BAs) has been predicted to have a very high thermal conductivity of over 2000 W m-1 K-1 at room temperature by first-principles calculations, rendering it a close competitor for diamond which holds the highest thermal conductivity among bulk materials. Experimental demonstration, however, has proved extremely challenging, especially in the preparation of large high quality single crystals. Although BAs crystals have been previously grown by chemical vapor transport (CVT), the growth process relies on spontaneous nucleation and results in small crystals with multiple grains and various defects. Here, we report a controllable CVT synthesis of large single BAs crystals (400-600 μm) by using carefully selected tiny BAs single crystals as seeds. We have obtained BAs single crystals with a thermal conductivity of 351 ± 21 W m-1 K-1 at room temperature, which is almost twice as conductive as previously reported BAs crystals. Further improvement along this direction is very likely.

  20. Anisotropic Laminar Piezocomposite Actuator Incorporating Machined PMN-PT Single Crystal Fibers

    NASA Technical Reports Server (NTRS)

    Wilkie, W. Keats; Inman, Daniel J.; Lloyd, Justin M.; High, James W.

    2006-01-01

    The design, fabrication, and testing of a flexible, laminar, anisotropic piezoelectric composite actuator utilizing machined PMN-32%PT single crystal fibers is presented. The device consists of a layer of rectangular single crystal piezoelectric fibers in an epoxy matrix, packaged between interdigitated electrode polyimide films. Quasistatic free-strain measurements of the single crystal device are compared with measurements from geometrically identical specimens incorporating polycrystalline PZT-5A and PZT-5H piezoceramic fibers. Free-strain actuation of the single crystal actuator at low bipolar electric fields (+/- 250 V/mm) is approximately 400% greater than that of the baseline PZT-5A piezoceramic device, and 200% greater than that of the PZT-5H device. Free-strain actuation under high unipolar electric fields (0-4kV/mm) is approximately 200% of the PZT-5A baseline device, and 150% of the PZT-5H alternate piezoceramic device. Performance increases at low field are qualitatively consistent with predicted increases based on scaling the low-field d33 piezoelectric constants of the respective piezoelectric materials. High-field increases are much less than scaled d33 estimates, but appear consistent with high-field freestrain measurements reported for similar bulk single-crystal and piezoceramic compositions. Measurements of single crystal actuator capacitance and coupling coefficient are also provided. These properties were poorly predicted using scaled bulk material dielectric and coupling coefficient data. Rules-of-mixtures calculations of the effective elastic properties of the single crystal device and estimated actuation work energy densities are also presented. Results indicate longitudinal stiffnesses significantly lower (50% less) than either piezoceramic device. This suggests that single-crystal piezocomposite actuators will be best suited to low induced-stress, high strain and deflection applications.

  1. Investigation and characterization of ZnO single crystal microtubes

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

    Al-Naser, Qusay A.H.; Zhou, Jian, E-mail: jianzhou@whut.edu.cn; Liu, Guizhen

    2016-04-15

    Morphological, structural, and optical characterization of microwave synthesized ZnO single crystal microtubes were investigated in this work. The structure and morphology of the ZnO microtubes are characterized using X-ray diffraction (XRD), single crystal diffraction (SCD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM). The results reveal that the as-synthesized ZnO microtube has a highly regular hexagonal cross section and smooth surfaces with an average length of 650–700 μm, an average outer diameter of 50 μm and wall thickness of 1–3 μm, possessing a single crystal wurtzite hexagonal structure. Optical properties of ZnOmore » single crystal microtubes were investigated by photoluminescence (PL) and ultraviolet-visible (UV-vis) absorption techniques. Room-temperature PL spectrum of the microtube reveal a strong UV emission peak at around 375.89 nm and broad and a weak visible emission with a main peak identified at 577 nm, which was assigned to the nearest band-edge emission and the deep-level emission, respectively. The band gap energy of ZnO microtube was found to be 3.27 eV. - Highlights: • ZnO microtube length of 650–700 μm, diameter of 50 μm, wall thickness of 1–3 μm • ZnO microtube possesses a single crystal wurtzite hexagonal structure. • The crystal system is hexahedral oriented along a-axis with indices of (100). • A strong and sharp UV emission at 375.89 nm (3.29 eV) • One prominent absorption band around 378.88 nm (3.27 eV)« less

  2. Fretting Stresses in Single Crystal Superalloy Turbine Blade Attachments

    NASA Technical Reports Server (NTRS)

    Arakere, Nagaraj K.; Swanson, Gregory

    2000-01-01

    Single crystal nickel base superalloy turbine blades are being utilized in rocket engine turbopumps and turbine engines because of their superior creep, stress rupture, melt resistance and thermomechanical fatigue capabilities over polycrystalline alloys. Currently the most widely used single crystal nickel base turbine blade superalloys are PWA 1480/1493 and PWA 1484. These alloys play an important role in commercial, military and space propulsion systems. High Cycle Fatigue (HCF) induced failures in aircraft gas turbine and rocket engine turbopump blades is a pervasive problem. Blade attachment regions are prone to fretting fatigue failures. Single crystal nickel base superalloy turbine blades are especially prone to fretting damage because the subsurface shear stresses induced by fretting action at the attachment regions can result in crystallographic initiation and crack growth along octahedral planes. Furthermore, crystallographic crack growth on octahedral planes under fretting induced mixed mode loading can be an order of magnitude faster than under pure mode I loading. This paper presents contact stress evaluation in the attachment region for single crystal turbine blades used in the NASA alternate Advanced High Pressure Fuel Turbo Pump (HPFTP/AT) for the Space Shuttle Main Engine (SSME). Single crystal materials have highly orthotropic properties making the position of the crystal lattice relative to the part geometry a significant factor in the overall analysis. Blades and the attachment region are modeled using a large-scale 3D finite element (FE) model capable of accounting for contact friction, material orthotrophy, and variation in primary and secondary crystal orientation. Contact stress analysis in the blade attachment regions is presented as a function of coefficient of friction and primary and secondary crystal orientation, Stress results are used to discuss fretting fatigue failure analysis of SSME blades. Attachment stresses are seen to reach

  3. Heterogeneous Monolithic Integration of Single-Crystal Organic Materials.

    PubMed

    Park, Kyung Sun; Baek, Jangmi; Park, Yoonkyung; Lee, Lynn; Hyon, Jinho; Koo Lee, Yong-Eun; Shrestha, Nabeen K; Kang, Youngjong; Sung, Myung Mo

    2017-02-01

    Manufacturing high-performance organic electronic circuits requires the effective heterogeneous integration of different nanoscale organic materials with uniform morphology and high crystallinity in a desired arrangement. In particular, the development of high-performance organic electronic and optoelectronic devices relies on high-quality single crystals that show optimal intrinsic charge-transport properties and electrical performance. Moreover, the heterogeneous integration of organic materials on a single substrate in a monolithic way is highly demanded for the production of fundamental organic electronic components as well as complex integrated circuits. Many of the various methods that have been designed to pattern multiple heterogeneous organic materials on a substrate and the heterogeneous integration of organic single crystals with their crystal growth are described here. Critical issues that have been encountered in the development of high-performance organic integrated electronics are also addressed. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Epoxy Nanocomposites Containing Zeolitic Imidazolate Framework-8.

    PubMed

    Liu, Cong; Mullins, Michael; Hawkins, Spencer; Kotaki, Masaya; Sue, Hung-Jue

    2018-01-10

    Zeolitic imidazole framework-8 (ZIF-8) is utilized as a functional filler and a curing agent in the preparation of epoxy nanocomposites. The imidazole group on the surface of the ZIF-8 initiates epoxy curing, resulting in covalent bonding between the ZIF-8 crystals and epoxy matrix. A substantial reduction in dielectric constant and increase in tensile modulus were observed. The implication of the present study for utilization of metal-organic framework to improve physical and mechanical properties of polymeric matrixes is discussed.

  5. Investigation of mircroorganisms colonising activated zeolites during anaerobic biogas production from grass silage.

    PubMed

    Weiss, S; Zankel, A; Lebuhn, M; Petrak, S; Somitsch, W; Guebitz, G M

    2011-03-01

    The colonisation of activated zeolites (i.e. clinoptilolites) as carriers for microorganisms involved in the biogas process was investigated. Zeolite particle sizes of 1.0-2.5mm were introduced to anaerobic laboratory batch-cultures and to continuously operated bioreactors during biogas production from grass silage. Incubation over 5-84 days led to the colonisation of zeolite surfaces in small batch-cultures (500 ml) and even in larger scaled and flow-through disturbed bioreactors (28 l). Morphological insights were obtained by using scanning electron microscopy (SEM). Single strand conformation polymorphism (SSCP) analysis based on amplification of bacterial and archaeal 16S rRNA fragments demonstrated structurally distinct populations preferring zeolite as operational environment. via sequence analysis conspicuous bands from SSCP patterns were identified. Populations immobilised on zeolite (e.g. Ruminofilibacter xylanolyticum) showed pronounced hydrolytic enzyme activity (xylanase) shortly after re-incubation in sterilised sludge on model substrate. In addition, the presence of methanogenic archaea on zeolite particles was demonstrated. Copyright © 2010 Elsevier Ltd. All rights reserved.

  6. ZEOLITES: EFFECTIVE WATER PURIFIERS

    EPA Science Inventory

    Zeolites are known for their adsorption, ion exchange and catalytic properties. Various natural zeolites are used as odor and moisture adsorbents and water softeners. Due to their acidic nature, synthetic zeolites are commonly employed as solid acid catalysts in petrochemical ind...

  7. Growth of single crystals from solutions using semi-permeable membranes

    NASA Astrophysics Data System (ADS)

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

    1983-05-01

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

  8. Light emission from organic single crystals operated by electrolyte doping

    NASA Astrophysics Data System (ADS)

    Matsuki, Keiichiro; Sakanoue, Tomo; Yomogida, Yohei; Hotta, Shu; Takenobu, Taishi

    2018-03-01

    Light-emitting devices based on electrolytes, such as light-emitting electrochemical cells (LECs) and electric double-layer transistors (EDLTs), are solution-processable devices with a very simple structure. Therefore, it is necessary to apply this device structure into highly fluorescent organic materials for future printed applications. However, owing to compatibility problems between electrolytes and organic crystals, electrolyte-based single-crystal light-emitting devices have not yet been demonstrated. Here, we report on light-emitting devices based on organic single crystals and electrolytes. As the fluorescent materials, α,ω-bis(biphenylyl)terthiophene (BP3T) and 5,6,11,12-tetraphenylnaphthacene (rubrene) single crystals were selected. Using ionic liquids as electrolytes, we observed clear light emission from BP3T LECs and rubrene EDLTs.

  9. 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.

  10. Method for the preparation of inorganic single crystal and polycrystalline electronic materials

    NASA Technical Reports Server (NTRS)

    Groves, W. O. (Inventor)

    1969-01-01

    Large area, semiconductor crystals selected from group 3-5 compounds and alloys are provided for semiconductor device fabrication by the use of a selective etching operation which completely removes the substrate on which the desired crystal was deposited. The substrate, selected from the same group as the single crystal, has a higher solution rate than the epitaxial single crystal which is essentially unaffected by the etching solution. The preparation of gallium phosphide single crystals using a gallium arsenide substrate and a concentrated nitric acid etching solution is described.

  11. Stable Fe/ZSM-5 Nanosheet Zeolite Catalysts for the Oxidation of Benzene to Phenol

    PubMed Central

    2017-01-01

    Fe/ZSM-5 nanosheet zeolites of varying thickness were synthesized with di- and tetraquaternary ammonium structure directing agents and extensively characterized for their textural, structural, and catalytic properties. Introduction of Fe3+ ions in the framework of nanosheet zeolites was slightly less effective than in bulk ZSM-5 zeolite. Steaming was necessary to activate all catalysts for N2O decomposition and benzene oxidation. The higher the Fe content, the higher the degree of Fe aggregation was after catalyst activation. The degree of Fe aggregation was lower when the crystal domain size of the zeolite or the Fe content was decreased. These two parameters had a substantial influence on the catalytic performance. Decreasing the number of Fe sites along the b-direction strongly suppressed secondary reactions of phenol and, accordingly, catalyst deactivation. This together with the absence of diffusional limitations in nanosheet zeolites explains the much higher phenol productivity obtainable with nanostructured Fe/ZSM-5. Steamed Fe/ZSM-5 zeolite nanosheet synthesized using C22-6-3·Br2 (domain size in b-direction ∼3 nm) and containing 0.24 wt % Fe exhibited the highest catalytic performance. During the first 24 h on stream, this catalyst produced 185 mmolphenol g–1. Calcination to remove the coke deposits completely restored the initial activity. PMID:28413693

  12. Factors affecting adsorption characteristics of Zn2+ on two natural zeolites.

    PubMed

    Oren, Ali Hakan; Kaya, Abidin

    2006-04-17

    Mining-related and industrial wastes are primary sources of heavy metal contamination in soils and groundwater. The limitation of such waste in drinking water needs to meet government requirements in order to safeguard human health and environment. Zinc, one of the most preponderant pollutants, is difficult to remove from wastewater rather than other heavy metals (i.e. lead, copper and cadmium). This paper investigates Zn2+ adsorption characteristics of two natural zeolites found in the regions of Gordes and Bigadic, in western Turkey. The results show that the Zn2+ adsorption behavior of both zeolites is highly dependent on the pH. Adsorption dependence on lower pH values (pH<4) is explained by the dissolution of crystal structure and the competition of the zinc ions with the H+. Between pH 4 and 6, the basic mechanism is the ion exchange process. The results also showed that decrease in grain size does not increase the adsorption capacity of zeolite from Gordes, yet it increases that of zeolite from Bigadic about 23%. The results also reveal that an increase in the initial concentration of Zn2+ in the system causes an increase in the adsorption capacity to a degree, then it becomes more constant at higher concentrations. With this, the removal efficiency of Gordes zeolite is two times higher than that of Bigadic zeolite. Results show that an increase in slurry concentration results in a lower uptake of Zn2+. In the final part of the paper, we compared the experimental data with the Langmuir and Freundlich isotherms. The results show that there is a good fit between the experimental data and empirical isotherms.

  13. Mechanical properties of hydroxyapatite single crystals from nanoindentation data

    PubMed Central

    Zamiri, A.; De, S.

    2011-01-01

    In this paper we compute elasto-plastic properties of hydroxyapatite single crystals from nanindentation data using a two-step algorithm. In the first step the yield stress is obtained using hardness and Young’s modulus data, followed by the computation of the flow parameters. The computational approach is first validated with data from existing literature. It is observed that hydroxyapatite single crystals exhibit anisotropic mechanical response with a lower yield stress along the [1010] crystallographic direction compared to the [0001] direction. Both work hardening rate and work hardening exponent are found to be higher for indentation along the [0001] crystallographic direction. The stress-strain curves extracted here could be used for developing constitutive models for hydroxyapatite single crystals. PMID:21262492

  14. SEM-EDS Observation of Structure Changes in Synthetic Zeolites Modified for CO2 Capture Needs

    NASA Astrophysics Data System (ADS)

    Wdowin, Magdalena; Panek, Rafal; Franus, Wojciech

    Carbon dioxide is the main greenhouse gas and its amount still increase in the atmosphere. Air pollution and greenhouse effect caused by CO2 emission have become a major threat to the environment on a global scale. Carbon dioxide sequestration (i.e. capture and consequently geological storage) is the key strategy within the portfolio of actions to reduce CO2 emission to the atmosphere. The most costly stage is capture of CO2, therefore there is a need to search new solutions of this technology. For this purpose it was examined Na-X synthetic zeolites, that were silver and PEI (polyethyleneimine) activated. SEM-EDS investigation enable to find a changes in structure of this materials after treatment. Where, as a result of silver activation from EDS analysis it is seen that Ag occur in Na-X structure, what indicate a substitution of Ag2+ for Na+ ions in crystal lattice. Analysing wt% the EDS analysis has shown that zeolite Na-X after silver impregnation becomes Ag-X zeolite. For Na-X-PEI activated it is observed a distinct organic compound in the form of coatings on Na-X crystals causing a sealing of pores in tested zeolite. Further examination of these materials concern determination of surface properties and experiments of CO2 sorption. But SEM-EDS analysis enable to determine the extent of activation, what is very important in determination of optimal conditions for such treatment in order to obtain better sorbent of CO2.

  15. Ordered macro-microporous metal-organic framework single crystals

    NASA Astrophysics Data System (ADS)

    Shen, Kui; Zhang, Lei; Chen, Xiaodong; Liu, Lingmei; Zhang, Daliang; Han, Yu; Chen, Junying; Long, Jilan; Luque, Rafael; Li, Yingwei; Chen, Banglin

    2018-01-01

    We constructed highly oriented and ordered macropores within metal-organic framework (MOF) single crystals, opening up the area of three-dimensional–ordered macro-microporous materials (that is, materials containing both macro- and micropores) in single-crystalline form. Our methodology relies on the strong shaping effects of a polystyrene nanosphere monolith template and a double-solvent–induced heterogeneous nucleation approach. This process synergistically enabled the in situ growth of MOFs within ordered voids, rendering a single crystal with oriented and ordered macro-microporous structure. The improved mass diffusion properties of such hierarchical frameworks, together with their robust single-crystalline nature, endow them with superior catalytic activity and recyclability for bulky-molecule reactions, as compared with conventional, polycrystalline hollow, and disordered macroporous ZIF-8.

  16. Effect of the raw material type and the reaction time on the synthesis of halloysite based Zeolite Na-P1

    NASA Astrophysics Data System (ADS)

    Meftah, Mahdi; Oueslati, Walid; Chorfi, Nejmeddine; Ben Haj Amara, Abdesslem

    Zeolites are currently one of the most important classes of inorganic materials because of their multiple applications not only as ions exchangers and molecular sieves, but also as catalysts. This works focus the synthesis and the characterization of Zeolite Na-P1 using halloysite (collected near Ain Khemouda, western Tunisia) as the starting material. Two parameters, such as the host materials type (natural or treated) and the reaction time, involved in the synthesis process are investigated. The intermediate phases and final products were characterized by X-ray diffraction, Infrared IR spectroscopy, scanning electron microscopy and high-resolution 29Si and 27Al MAS NMR. Obtained results show that the hydrothermal synthesis from natural and heated-halloysite leads to formation of homogenous Zeolite Na-P1. The difference in the crystallization/transformation time process is explained by the effect of the dissolution rate of the starting materials in sodium hydroxide solution. In the case of heated halloysite, the synthesis reaction with alkali solution occurs very readily and achieved without prior thermal activation at high temperature. The optimal conditions of Zeolite Na-P1 crystallization, from heated-halloysite, are reached at 120 °C.

  17. A Quick Method for Determining the Density of Single Crystals.

    ERIC Educational Resources Information Center

    Roman, Pascual; Gutierrez-Zorrilla, Juan M.

    1985-01-01

    Shows how the Archimedes method is used to determine the density of a single crystal of ammonium oxalate monohydrate. Also shows how to calculate the density of other chemicals when they are available as single crystals. Experimental procedures and materials needed are included. (JN)

  18. SSME single-crystal turbine blade dynamics

    NASA Technical Reports Server (NTRS)

    Moss, Larry A.

    1988-01-01

    A study was performrd to determine the dynamic characteristics of the Space Shuttle Main Engine high pressure fuel turbopump (HPFTP) blades made of single crystal (SC) material. The first and second stage drive turbine blades of HPFTP were examined. The nonrotating natural frequencies were determined experimentally and analytically. The experimental results of the SC second stage blade were used to verify the analytical procedures. The study examined the SC first stage blade natural frequencies with respect to crystal orientation at typical operating conditions. The SC blade dynamic response was predicted to be less than the directionally solidified base. Crystal axis orientation optimization indicated that the third mode interference will exist in any SC orientation.

  19. SSME single crystal turbine blade dynamics

    NASA Technical Reports Server (NTRS)

    Moss, Larry A.; Smith, Todd E.

    1987-01-01

    A study was performed to determine the dynamic characteristics of the Space Shuttle main engine high pressure fuel turbopump (HPFTP) blades made of single crystal (SC) material. The first and second stage drive turbine blades of HPFTP were examined. The nonrotating natural frequencies were determined experimentally and analytically. The experimental results of the SC second stage blade were used to verify the analytical procedures. The analytical study examined the SC first stage blade natural frequencies with respect to crystal orientation at typical operating conditions. The SC blade dynamic response was predicted to be less than the directionally solidified blade. Crystal axis orientation optimization indicated the third mode interference will exist in any SC orientation.

  20. Shock Hugoniot of single crystal copper

    NASA Astrophysics Data System (ADS)

    Chau, R.; Stölken, J.; Asoka-Kumar, P.; Kumar, M.; Holmes, N. C.

    2010-01-01

    The shock Hugoniot of single crystal copper is reported for stresses below 66 GPa. Symmetric impact experiments were used to measure the Hugoniots of three different crystal orientations of copper, [100], [110], and [111]. The photonic doppler velocimetry (PDV) diagnostic was adapted into a very high precision time of arrival detector for these experiments. The measured Hugoniots along all three crystal directions were nearly identical to the experimental Hugoniot for polycrystalline Cu. The predicted orientation dependence of the Hugoniot from molecular dynamics calculations was not observed. At the lowest stresses, the sound speed in Cu was extracted from the PDV data. The measured sound speeds are in agreement with values calculated from the elastic constants for Cu.

  1. Bridgman growth and scintillation properties of calcium tungstate single crystal

    NASA Astrophysics Data System (ADS)

    Wang, Zhenhai; Jiang, Linwen; Chen, Yaping; Chen, Peng; Chen, Hongbing; Mao, Rihua

    2017-12-01

    CaWO4 single crystal with large size was grown by Bridgman method. The results of transmission spectra show that the transmittance of CaWO4 crystal reaches 79-85% in 320-800 nm wavelength range. The refraction index is near 1.80 in visible and infrared region. CaWO4 crystal shows a broad emission band centered at 424 nm under X-ray excitation and centered at 416 nm under ultraviolet (λex = 280 nm) excitation. The decay kinetics of CaWO4 single crystal shows double-exponential decay with fast decay constant τ1 = 5.4 μs and slow decay constant τ2 = 177.1 μs. The energy resolution of CaWO4 crystal was found to be 31.6% in the net peak of 545.9 channel. Meanwhile, the absolute output is at the lever of 19,000 ± 1000 photons/MeV. The results indicate the scintillator of CaWO4 single crystal has great potential in the applications of high-energy physics and nuclear physics due to its high light output and great energy resolution.

  2. Effect of Chain Conformation on the Single-Molecule Melting Force in Polymer Single Crystals: Steered Molecular Dynamics Simulations Study.

    PubMed

    Feng, Wei; Wang, Zhigang; Zhang, Wenke

    2017-02-28

    Understanding the relationship between polymer chain conformation as well as the chain composition within the single crystal and the mechanical properties of the corresponding single polymer chain will facilitate the rational design of high performance polymer materials. Here three model systems of polymer single crystals, namely poly(ethylene oxide) (PEO), polyethylene (PE), and nylon-66 (PA66) have been chosen to study the effects of chain conformation, helical (PEO) versus planar zigzag conformation (PE, PA66), and chain composition (PE versus PA66) on the mechanical properties of a single polymer chain. To do that, steered molecular dynamics simulations were performed on those polymer single crystals by pulling individual polymer chains out of the crystals. Our results show that the patterns of force-extension curve as well as the chain moving mode are closely related to the conformation of the polymer chain in the single crystal. In addition, hydrogen bonds can enhance greatly the force required to stretch the polymer chain out of the single crystal. The dynamic breaking and reformation of multivalent hydrogen bonds have been observed for the first time in PA66 at the single molecule level.

  3. High definition TV projection via single crystal faceplate technology

    NASA Astrophysics Data System (ADS)

    Kindl, H. J.; St. John, Thomas

    1993-03-01

    Single crystal phosphor faceplates are epitaxial phosphors grown on crystalline substrates with the advantages of high light output, resolution, and extended operational life. Single crystal phosphor faceplate industrial technology in the United States is capable of providing a faceplate appropriate to the projection industry of up to four (4) inches in diameter. Projection systems incorporating cathode ray tubes utilizing single crystal phosphor faceplates will produce 1500 lumens of white light with 1000 lines of resolution, non-interlaced. This 1500 lumen projection system will meet all of the currently specified luminance and resolution requirements of Visual Display systems for flight simulators. Significant logistic advantages accrue from the introduction of single crystal phosphor faceplate CRT's. Specifically, the full performance life of a CRT is expected to increase by a factor of five (5); ie, from 2000 to 10,000 hours of operation. There will be attendant reductions in maintenance time, spare CRT requirements, system down time, etc. The increased brightness of the projection system will allow use of lower gain, lower cost simulator screen material. Further, picture performance characteristics will be more balanced across the full simulator.

  4. Perovskite single crystals and thin films for optoelectronic devices (Conference Presentation)

    NASA Astrophysics Data System (ADS)

    Li, Gang; Han, Qifeng; Yang, Yang; Bae, Sang-Hoon; Sun, Pengyu

    2016-09-01

    Hybrid organolead trihalide perovskite (OTP) solar cells have developed as a promising candidate in photovoltaics due to their excellent properties including a direct bandgap, strong absorption coefficient, long carrier lifetime, and high mobility. Most recently, formamidinium (NH2CH=NH2+ or FA) lead iodide (FAPbI3) has attracted significant attention due to several advantages: (1) the larger organic FA cation can replace the MA cation and form a more symmetric crystal structure, (2) the smaller bandgap of FAPbI3 allows for near infrared (NIR) absorption, and (3) FAPbI3 has an elevated decomposition temperature and thus potential to improve stability. Single crystals provide an excellent model system to study the intrinsic electrical and optical properties of these materials due to their high purity, which is particularly important to understand the limits of these materials. In this work, we report the growth of large ( 5 millimeter size) single crystal FAPbI3 using a novel liquid based crystallization method. The single crystal FAPbI3 demonstrated a δ-phase to α-phase transition with a color change from yellow to black when heated to 185°C within approximately two minutes. The crystal structures of the two phases were identified and the PL emission peak of the α-phase FAPbI3 (820 nm) shows clear red-shift compared to the FAPbI3 thin film (805 nm). The FAPbI3 single crystal shows a long carrier lifetime of 484 ns, a high carrier mobility of 4.4 cm2·V-1·s-1, and even more interestingly a conductivity of 1.1 × 10-7(ohm·cm)-1, which is approximately one order of magnitude higher than that of the MAPbI3 single crystal. Finally, high performance photoconductivity type photodetectors were successfully demonstrated using the single crystal FAPbI3.

  5. Rotating lattice single crystal architecture on the surface of glass

    DOE PAGES

    Savytskii, D.; Jain, H.; Tamura, N.; ...

    2016-11-03

    Defying the requirements of translational periodicity in 3D, rotation of the lattice orientation within an otherwise single crystal provides a new form of solid. Such rotating lattice single (RLS) crystals are found, but only as spherulitic grains too small for systematic characterization or practical application. Here we report a novel approach to fabricate RLS crystal lines and 2D layers of unlimited dimensions via a recently discovered solid-to-solid conversion process using a laser to heat a glass to its crystallization temperature but keeping it below the melting temperature. The proof-of-concept including key characteristics of RLS crystals is demonstrated using the examplemore » of Sb 2S 3 crystals within the Sb-S-I model glass system for which the rotation rate depends on the direction of laser scanning relative to the orientation of initially formed seed. Lattice rotation in this new mode of crystal growth occurs upon crystallization through a well-organized dislocation/disclination structure introduced at the glass/ crystal interface. Implications of RLS growth on biomineralization and spherulitic crystal growth are noted.« less

  6. Effect of Crystal Orientation on Fatigue Failure of Single Crystal Nickel Base Turbine Blade Superalloys

    NASA Technical Reports Server (NTRS)

    Arakere, Nagaraj K.; Swanson, Gregory R.

    2000-01-01

    High Cycle Fatigue (HCF) induced failures in aircraft gas-turbine engines is a pervasive problem affecting a wide range of components and materials. HCF is currently the primary cause of component failures in gas turbine aircraft engines. Turbine blades in high performance aircraft and rocket engines are increasingly being made of single crystal nickel superalloys. Single-crystal Nickel-base superalloys were developed to provide superior creep, stress rupture, melt resistance and thermomechanical fatigue capabilities over polycrystalline alloys previously used in the production of turbine blades and vanes. Currently the most widely used single crystal turbine blade superalloys are PWA 1480/1493 and PWA 1484. These alloys play an important role in commercial, military and space propulsion systems. PWA1493, identical to PWA1480, but with tighter chemical constituent control, is used in the NASA SSME (Space Shuttle Main Engine) alternate turbopump, a liquid hydrogen fueled rocket engine. Objectives for this paper are motivated by the need for developing failure criteria and fatigue life evaluation procedures for high temperature single crystal components, using available fatigue data and finite element modeling of turbine blades. Using the FE (finite element) stress analysis results and the fatigue life relations developed, the effect of variation of primary and secondary crystal orientations on life is determined, at critical blade locations. The most advantageous crystal orientation for a given blade design is determined. Results presented demonstrates that control of secondary and primary crystallographic orientation has the potential to optimize blade design by increasing its resistance to fatigue crack growth without adding additional weight or cost.

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

    NASA Astrophysics Data System (ADS)

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

    2015-01-01

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

  8. 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

  9. Conventional hydrothermal synthesis of Na-A zeolite from cupola slag and aluminum sludge.

    PubMed

    Anuwattana, Rewadee; Khummongkol, Pojanie

    2009-07-15

    Na-A type zeolites were prepared from two industrial wastes: the solid by-product of cupola slag and aluminum sludge from an aluminum plating plant. Two preparation methods using the same starting material compositions were carried out. In the first method, alkaline fusion was introduced, followed by the hydrothermal treatment to obtain sodium aluminosilicate which was then crystallized in NaOH solution under the condition of 90+/-3 degrees C for 1-9h with different H(2)O/SiO2 ratios. The result shows that higher H(2)O/SiO2 ratio increases the rate of crystallization. The largest amount of crystallinity for Na-A was found at 3h. In the second method, alkaline hydrothermal treatment without fusion was carried out in the same condition as the first method. No Na-A zeolite was obtained by this method. The changes of the dissolved amounts of Si(4+) and Al(3+) in 3M NaOH were investigated during the hydrothermal reaction.

  10. 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.

  11. 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.

  12. Flexible single-crystal silicon nanomembrane photonic crystal cavity.

    PubMed

    Xu, Xiaochuan; Subbaraman, Harish; Chakravarty, Swapnajit; Hosseini, Amir; Covey, John; Yu, Yalin; Kwong, David; Zhang, Yang; Lai, Wei-Cheng; Zou, Yi; Lu, Nanshu; Chen, Ray T

    2014-12-23

    Flexible inorganic electronic devices promise numerous applications, especially in fields that could not be covered satisfactorily by conventional rigid devices. Benefits on a similar scale are also foreseeable for silicon photonic components. However, the difficulty in transferring intricate silicon photonic devices has deterred widespread development. In this paper, we demonstrate a flexible single-crystal silicon nanomembrane photonic crystal microcavity through a bonding and substrate removal approach. The transferred cavity shows a quality factor of 2.2×10(4) and could be bent to a curvature of 5 mm radius without deteriorating the performance compared to its counterparts on rigid substrates. A thorough characterization of the device reveals that the resonant wavelength is a linear function of the bending-induced strain. The device also shows a curvature-independent sensitivity to the ambient index variation.

  13. Magnetic field controlled floating-zone single crystal growth of intermetallic compounds

    NASA Astrophysics Data System (ADS)

    Hermann, R.; Gerbeth, G.; Priede, J.

    2013-03-01

    Radio-frequency (RF) floating zone single crystal growth is an important technique for the preparation of single bulk crystals. The advantage of the floating-zone method is the crucible-free growth of single crystals of reactive materials with high melting points. The strong heat diffusion on the surface, as well as the melt convection in the molten zone due to induction heating, often leads to an undesired solid-liquid interface geometry with a concave (towards the solid phase) outer rim. These concave parts aggravate the single crystal growth over the full cross-section. A two-phase stirrer was developed at IFW Dresden in order to avoid the problems connected with these concave parts. It acts as a magnetic field pump and changes the typical double vortex structure to a single roll structure, thus pushing hot melt into the regions where the concave parts may arise. The current in the secondary coil is induced by the primary coil, and the capacitor and the resistance of the secondary circuit are adjusted to get a stable 90 degree phase-shift between the coil currents. Single crystal growth of industrial relevant RuAl and TiAl intermetallic compounds was performed based on the material parameters and using the adjusted two-phase stirrer. Very recently, the magnetic system was applied to the crystal growth of biocompatible TiNb alloys and antiferromagnetic Heusler MnSi compounds.

  14. High Performance Relaxor-Based Ferroelectric Single Crystals for Ultrasonic Transducer Applications

    PubMed Central

    Chen, Yan; Lam, Kwok-Ho; Zhou, Dan; Yue, Qingwen; Yu, Yanxiong; Wu, Jinchuan; Qiu, Weibao; Sun, Lei; Zhang, Chao; Luo, Haosu; Chan, Helen L. W.; Dai, Jiyan

    2014-01-01

    Relaxor-based ferroelectric single crystals Pb(Mg1/3Nb2/3)O3-PbTiO3 (PMN-PT) have drawn much attention in the ferroelectric field because of their excellent piezoelectric properties and high electromechanical coupling coefficients (d33∼2000 pC/N, kt∼60%) near the morphotropic phase boundary (MPB). Ternary Pb(In1/2Nb1/2)O3-Pb(Mg1/3Nb2/3)O3-PbTiO3 (PIN-PMN-PT) single crystals also possess outstanding performance comparable with PMN-PT single crystals, but have higher phase transition temperatures (rhombohedral to tetragonal Trt, and tetragonal to cubic Tc) and larger coercive field Ec. Therefore, these relaxor-based single crystals have been extensively employed for ultrasonic transducer applications. In this paper, an overview of our work and perspectives on using PMN-PT and PIN-PMN-PT single crystals for ultrasonic transducer applications is presented. Various types of single-element ultrasonic transducers, including endoscopic transducers, intravascular transducers, high-frequency and high-temperature transducers fabricated using the PMN-PT and PIN-PMN-PT crystals and their 2-2 and 1-3 composites are reported. Besides, the fabrication and characterization of the array transducers, such as phased array, cylindrical shaped linear array, high-temperature linear array, radial endoscopic array, and annular array, are also addressed. PMID:25076222

  15. 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.

  16. Quantification of thickness and wrinkling of exfoliated two-dimensional zeolite nanosheets

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

    Kumar, Prashant; Agrawal, Kumar Varoon; Tsapatsis, Michael

    Some two-dimensional (2D) exfoliated zeolites are single- or near single-unit cell thick silicates that can function as molecular sieves. Although they have already found uses as catalysts, adsorbents and membranes precise determination of their thickness and wrinkling is critical as these properties influence their functionality. Here we demonstrate a method to accurately determine the thickness and wrinkles of a 2D zeolite nanosheet by comprehensive 3D mapping of its reciprocal lattice. Since the intensity modulation of a diffraction spot on tilting is a fingerprint of the thickness, and changes in the spot shape are a measure of wrinkling, this mapping ismore » achieved using a large-angle tilt-series of electron diffraction patterns. As a result, application of the method to a 2D zeolite with MFI structure reveals that the exfoliated MFI nanosheet is 1.5 unit cells (3.0 nm) thick and wrinkled anisotropically with up to 0.8 nm average surface roughness.« less

  17. Quantification of thickness and wrinkling of exfoliated two-dimensional zeolite nanosheets

    DOE PAGES

    Kumar, Prashant; Agrawal, Kumar Varoon; Tsapatsis, Michael; ...

    2015-05-11

    Some two-dimensional (2D) exfoliated zeolites are single- or near single-unit cell thick silicates that can function as molecular sieves. Although they have already found uses as catalysts, adsorbents and membranes precise determination of their thickness and wrinkling is critical as these properties influence their functionality. Here we demonstrate a method to accurately determine the thickness and wrinkles of a 2D zeolite nanosheet by comprehensive 3D mapping of its reciprocal lattice. Since the intensity modulation of a diffraction spot on tilting is a fingerprint of the thickness, and changes in the spot shape are a measure of wrinkling, this mapping ismore » achieved using a large-angle tilt-series of electron diffraction patterns. As a result, application of the method to a 2D zeolite with MFI structure reveals that the exfoliated MFI nanosheet is 1.5 unit cells (3.0 nm) thick and wrinkled anisotropically with up to 0.8 nm average surface roughness.« less

  18. Removal of paraquat solution onto zeolite material

    NASA Astrophysics Data System (ADS)

    Sirival, Rujikarn; Patdhanagul, Nopbhasinthu; Preecharram, Sutthidech; Photharin, Somkuan

    2018-04-01

    The purpose of this research was to study the adsorption of paraquat herbicides onto zeolite Y materials by the batch method. Three adsorbents material: Zeolite-3, Zeolite-10, and Zeolite-100 were Si/Al ratio at 3.58, 8.57 and 154.37, respectively. The factors for adsorption of paraquat as follows, adsorption time, initial concentrations of paraquat, pH and adsorption isotherm were investigated. The results showed that zeolite-10 had higher adsorption capacity than zeolite-3 and zeolite-100. The appropriate conditions for adsorption were 24 h., Zeolite 0.1 g., Initial paraquat concentration 100 ppm at pH 6. The adsorption isotherm was found to correspond with Langmuir Isotherm and the maximum paraquat adsorption is 26.38 mg/g for zeolite-10, 21.41 mg/g and 9.60 mg/g for zeolite-3 and zeolite-100, respectively. The characterization of zeolite material with XRD, XRF and BET. Furthermore, the zeolite materials applied to remove other organic and inorganic wastewater.

  19. Converting ceria polyhedral nanoparticles into single-crystal nanospheres.

    PubMed

    Feng, Xiangdong; Sayle, Dean C; Wang, Zhong Lin; Paras, M Sharon; Santora, Brian; Sutorik, Anthony C; Sayle, Thi X T; Yang, Yi; Ding, Yong; Wang, Xudong; Her, Yie-Shein

    2006-06-09

    Ceria nanoparticles are one of the key abrasive materials for chemical-mechanical planarization of advanced integrated circuits. However, ceria nanoparticles synthesized by existing techniques are irregularly faceted, and they scratch the silicon wafers and increase defect concentrations. We developed an approach for large-scale synthesis of single-crystal ceria nanospheres that can reduce the polishing defects by 80% and increase the silica removal rate by 50%, facilitating precise and reliable mass-manufacturing of chips for nanoelectronics. We doped the ceria system with titanium, using flame temperatures that facilitate crystallization of the ceria yet retain the titania in a molten state. In conjunction with molecular dynamics simulation, we show that under these conditions, the inner ceria core evolves in a single-crystal spherical shape without faceting, because throughout the crystallization it is completely encapsulated by a molten 1- to 2-nanometer shell of titania that, in liquid state, minimizes the surface energy. The principle demonstrated here could be applied to other oxide systems.

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

    NASA Astrophysics Data System (ADS)

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

    1988-09-01

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

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

    NASA Technical Reports Server (NTRS)

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

    1988-01-01

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

  2. 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.

  3. Thermal collapse and hierarchy of polymorphs in a faujasite-type zeolite and its analogous melt-quenched glass

    NASA Astrophysics Data System (ADS)

    Palenta, Theresia; Fuhrmann, Sindy; Greaves, G. Neville; Schwieger, Wilhelm; Wondraczek, Lothar

    2015-02-01

    We examine the route of structural collapse and re-crystallization of faujasite-type (Na,K)-LSX zeolite. As the first step, a rather stable amorphous high density phase HDAcollapse is generated through an order-disorder transition from the original zeolite via a low density phase LDAcollapse, at around 790 °C. We find that the overall amorphization is driven by an increase in the bond angle distribution within T-O-T and a change in ring statistics to 6-membered TO4 (T = Si4+, Al3+) rings at the expense of 4-membered rings. The HDAamorph transforms into crystalline nepheline, though, through an intermediate metastable carnegieite phase. In comparison, the melt-derived glass of similar composition, HDAMQ, crystallizes directly into the nepheline phase without the occurrence of intermediate carnegieite. This is attributed to the higher structural order of the faujasite-derived HDAcollapse which prefers the re-crystallization into the highly symmetric carnegieite phase before transformation into nepheline with lower symmetry.

  4. A Fiber Optic Interferometric Sensor Platform for Determining Gas Diffusivity in Zeolite Films.

    PubMed

    Yang, Ruidong; Xu, Zhi; Zeng, Shixuan; Jing, Wenheng; Trontz, Adam; Dong, Junhang

    2018-04-04

    Fiber optic interferometer (FOI) sensors have been fabricated by directly growing pure-silica MFI-type zeolite (i.e., silicalite) films on straight-cut endfaces of single-mode communication optical fibers. The FOI sensor has been demonstrated for determining molecular diffusivity in the zeolite by monitoring the temporal response of light interference from the zeolite film during the dynamic process of gas adsorption. The optical thickness of the zeolite film depends on the amount of gas adsorption that causes the light interference to shift upon loading molecules into the zeolitic channels. Thus, the time-dependence of the optical signal reflected from the coated zeolite film can represent the adsorption uptake curve, which allows computation of the diffusivity using models derived from the Fick’s Law equations. In this study, the diffusivity of isobutane in silicalite has been determined by the new FOI sensing method, and the results are in good agreement with literature values obtained by various conventional macroscopic techniques. The FOI sensor platform, because of its robustness and small size, could be useful for studying molecular diffusion in zeolitic materials under conditions that are inaccessible to the existing techniques.

  5. Ductile-to-Brittle transition in <111> hadfield steel single crystals

    NASA Astrophysics Data System (ADS)

    Astafurova, E. G.; Chumlyakov, Yu. I.

    2010-10-01

    The deformation mechanism and the character of fracture of <111> austenitic Hadfield steel single crystals are studied during tension in the temperature range 77-673 K by scanning and transmission electron microscopy. It is found that a change in the fracture mechanism from ductile to brittle fracture according to the fractography criterion takes place at a higher temperature than that determined from a change in the elongation to failure of the single crystals. The ductile-to-brittle transition in the Hadfield steel single crystals is shown to be related to a high level of deforming stresses induced by solid-solution hardening and to mechanical twinning.

  6. Molecular simulations for energy, environmental and pharmaceutical applications of nanoporous materials: from zeolites, metal-organic frameworks to protein crystals.

    PubMed

    Jiang, Jianwen; Babarao, Ravichandar; Hu, Zhongqiao

    2011-07-01

    Nanoporous materials have widespread applications in chemical industry, but the pathway from laboratory synthesis and testing to practical utilization of nanoporous materials is substantially challenging and requires fundamental understanding from the bottom up. With ever-growing computational resources, molecular simulations have become an indispensable tool for material characterization, screening and design. This tutorial review summarizes the recent simulation studies in zeolites, metal-organic frameworks and protein crystals, and provides a molecular overview for energy, environmental and pharmaceutical applications of nanoporous materials with increasing degree of complexity in building blocks. It is demonstrated that molecular-level studies can bridge the gap between physical and engineering sciences, unravel microscopic insights that are otherwise experimentally inaccessible, and assist in the rational design of new materials. The review is concluded with major challenges in future simulation exploration of novel nanoporous materials for emerging applications.

  7. 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.

  8. Laser generation in opal-like single-crystal and heterostructure photonic crystals

    NASA Astrophysics Data System (ADS)

    Kuchyanov, A. S.; Plekhanov, A. I.

    2016-11-01

    This study describes the laser generation of a 6Zh rhodamine in artificial opals representing single-crystal and heterostructure films. The spectral and angular properties of emission and the threshold characteristics of generation are investigated. In the case where the 6Zh rhodamine was in a bulk opal, the so-called random laser generation was observed. In contrast to this, the laser generation caused by a distributed feedback inside the structure of the photonic bandgap was observed in photonic-crystal opal films.

  9. Mesoscale martensitic transformation in single crystals of topological defects

    PubMed Central

    Martínez-González, José A.; Ramírez-Hernández, Abelardo; Zhou, Ye; Sadati, Monirosadat; Zhang, Rui; Nealey, Paul F.; de Pablo, Juan J.

    2017-01-01

    Liquid-crystal blue phases (BPs) are highly ordered at two levels. Molecules exhibit orientational order at nanometer length scales, while chirality leads to ordered arrays of double-twisted cylinders over micrometer scales. Past studies of polycrystalline BPs were challenged by the existence of grain boundaries between randomly oriented crystalline nanodomains. Here, the nucleation of BPs is controlled with precision by relying on chemically nanopatterned surfaces, leading to macroscopic single-crystal BP specimens where the dynamics of mesocrystal formation can be directly observed. Theory and experiments show that transitions between two BPs having a different network structure proceed through local reorganization of the crystalline array, without diffusion of the double-twisted cylinders. In solid crystals, martensitic transformations between crystal structures involve the concerted motion of a few atoms, without diffusion. The transformation between BPs, where crystal features arise in the submicron regime, is found to be martensitic in nature when one considers the collective behavior of the double-twist cylinders. Single-crystal BPs are shown to offer fertile grounds for the study of directed crystal nucleation and the controlled growth of soft matter. PMID:28874557

  10. Method for preparing homogeneous single crystal ternary III-V alloys

    DOEpatents

    Ciszek, Theodore F.

    1991-01-01

    A method for producing homogeneous, single-crystal III-V ternary alloys of high crystal perfection using a floating crucible system in which the outer crucible holds a ternary alloy of the composition desired to be produced in the crystal and an inner floating crucible having a narrow, melt-passing channel in its bottom wall holds a small quantity of melt of a pseudo-binary liquidus composition that would freeze into the desired crystal composition. The alloy of the floating crucilbe is maintained at a predetermined lower temperature than the alloy of the outer crucible, and a single crystal of the desired homogeneous alloy is pulled out of the floating crucible melt, as melt from the outer crucible flows into a bottom channel of the floating crucible at a rate that corresponds to the rate of growth of the crystal.

  11. Method of making macrocrystalline or single crystal semiconductor material

    NASA Technical Reports Server (NTRS)

    Shlichta, P. J. (Inventor); Holliday, R. J. (Inventor)

    1986-01-01

    A macrocrystalline or single crystal semiconductive material is formed from a primary substrate including a single crystal or several very large crystals of a relatively low melting material. This primary substrate is deposited on a base such as steel or ceramic, and it may be formed from such metals as zinc, cadmium, germanium, aluminum, tin, lead, copper, brass, magnesium silicide, or magnesium stannide. These materials generally have a melting point below about 1000 C and form on the base crystals the size of fingernails or greater. The primary substrate has an epitaxial relationship with a subsequently applied layer of material, and because of this epitaxial relationship, the material deposited on the primary substrate will have essentially the same crystal size as the crystals in the primary substrate. If required, successive layers are formed, each of a material which has an epitaxial relationship with the previously deposited layer, until a layer is formed which has an epitaxial relationship with the semiconductive material. This layer is referred to as the epitaxial substrate, and its crystals serve as sites for the growth of large crystals of semiconductive material. The primary substrate is passivated to remove or otherwise convert it into a stable or nonreactive state prior to deposition of the seconductive material.

  12. Neutron Transmission of Single-crystal Sapphire Filters

    NASA Astrophysics Data System (ADS)

    Adib, M.; Kilany, M.; Habib, N.; Fathallah, M.

    2005-05-01

    An additive formula is given that permits the calculation of the nuclear capture, thermal diffuse and Bragg scattering cross-sections as a function of sapphire temperature and crystal parameters. We have developed a computer program that allows calculations of the thermal neutron transmission for the sapphire rhombohedral structure and its equivalent trigonal structure. The calculated total cross-section values and effective attenuation coefficient for single-crystalline sapphire at different temperatures are compared with measured values. Overall agreement is indicated between the formula and experimental data. We discuss the use of sapphire single crystal as a thermal neutron filter in terms of the optimum cystal thickness, mosaic spread, temperature, cutting plane and tuning for efficient transmission of thermal-reactor neutrons.

  13. g-Tensor determination from single-crystal ESR data

    NASA Astrophysics Data System (ADS)

    Byrn, Marianne P.; Strouse, Charles E.

    A general method is presented for extraction of the g tensor from single-crystal electron spin resonance data. This method does not depend on knowledge of crystal morphology or on the presence of crystallographic symmetry. The g values are obtained from rotations around three arbitrarily chosen but accurately known axes.

  14. Micro-pulling-down furnace modification and single crystal fibers growth

    NASA Astrophysics Data System (ADS)

    Yuan, Dongsheng; Jia, Zhitai; Li, Yang; Wu, Baiyi; Tao, Xutang

    2016-03-01

    Single crystal fiber (SCF) combines the excellent instinct properties of conventional bulk laser crystals, and the special geometry advantage of active optical fibers. YAG and LuAG are proper host candidates for single crystal fiber laser with high thermal conductivity. Despite a lower thermal conductivity for pure crystal than YAG, LuAG crystal is easier to obtain homogeneous optical quality, and has a thermal conductivity nearly independent from the doping level. Micropulling- down (μ-PD) has relatively small thermal gradient, and here we use μ-PD to carry out high quality SCFs. Through the μ-PD furnace manufactured by ourselves, crystal fibers with different diameters have been grown successfully. We designed and fabricated a method to adjust the thermal distribution, and with the favor of pulling-down rate, the specific diameter can be controlled perfectly. The crystalline quality and homogeneity along the whole fiber were investigated, and LuAG SCF was confirmed to have a fine crystal quality for laser.

  15. Method for harvesting rare earth barium copper oxide single crystals

    DOEpatents

    Todt, Volker R.; Sengupta, Suvankar; Shi, Donglu

    1996-01-01

    A method of preparing high temperature superconductor single crystals. The method of preparation involves preparing precursor materials of a particular composition, heating the precursor material to achieve a peritectic mixture of peritectic liquid and crystals of the high temperature superconductor, cooling the peritectic mixture to quench directly the mixture on a porous, wettable inert substrate to wick off the peritectic liquid, leaving single crystals of the high temperature superconductor on the porous substrate. Alternatively, the peritectic mixture can be cooled to a solid mass and reheated on a porous, inert substrate to melt the matrix of peritectic fluid while leaving the crystals melted, allowing the wicking away of the peritectic liquid.

  16. Structural analysis of hierarchically organized zeolites

    PubMed Central

    Mitchell, Sharon; Pinar, Ana B.; Kenvin, Jeffrey; Crivelli, Paolo; Kärger, Jörg; Pérez-Ramírez, Javier

    2015-01-01

    Advances in materials synthesis bring about many opportunities for technological applications, but are often accompanied by unprecedented complexity. This is clearly illustrated by the case of hierarchically organized zeolite catalysts, a class of crystalline microporous solids that has been revolutionized by the engineering of multilevel pore architectures, which combine unique chemical functionality with efficient molecular transport. Three key attributes, the crystal, the pore and the active site structure, can be expected to dominate the design process. This review examines the adequacy of the palette of techniques applied to characterize these distinguishing features and their catalytic impact. PMID:26482337

  17. Iron single crystal growth from a lithium-rich melt

    NASA Astrophysics Data System (ADS)

    Fix, M.; Schumann, H.; Jantz, S. G.; Breitner, F. A.; Leineweber, A.; Jesche, A.

    2018-03-01

    α -Fe single crystals of rhombic dodecahedral habit were grown from a Li84N12Fe∼3 melt. Crystals of several millimeter along a side form at temperatures around T ≈ 800 ° C. Upon further cooling the growth competes with the formation of Fe-doped Li3N. The b.c.c. structure and good sample quality of α -Fe single crystals were confirmed by X-ray and electron diffraction as well as magnetization measurements and chemical analysis. A nitrogen concentration of 90 ppm was detected by means of carrier gas hot extraction. Scanning electron microscopy did not reveal any sign of iron nitride precipitates.

  18. Dry-growth of silver single-crystal nanowires from porous Ag structure

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

    Chen, Chuantong, E-mail: chenchuantong@sanken.osaka-u.ac.jp; Nagao, Shijo; Jiu, Jinting

    A fabrication method of single crystal Ag nanowires in large scale is introduced without any chemical synthesis in wet processes, which usually generates fivefold twinned nanowires of fcc metals. Dense single-crystal nanowires grow on a mechanically polished surface of micro-porous Ag structure, which is created from Ag micro-particles. The diameter and the length of the nanowires can be controlled simply by changing the temperature and the time of the heating during the nanowire growth in air. Unique growth mechanism is described in detail, based on stress-induced migration accelerated by the micro-porous structure where the origin of Ag nanowires growth ismore » incubated. Transmission electron microscopy analysis on the single crystal nanowires is also presented. This simple method offered an alternative preparation for metallic nanowires, especially with the single crystal structure in numerous applications.« less

  19. Synthesis, crystal structure, and magnetic properties of two-dimensional divalent metal glutarate/dipyridylamine coordination polymers, with a single crystal-to-single crystal transformation in the copper derivative

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

    Montney, Matthew R.; Supkowski, Ronald M.; Staples, Richard J.

    Hydrothermal reaction of divalent metal chlorides with glutaric acid and 4,4'-dipyridylamine (dpa) has afforded an isostructural family of coordination polymers with formulation [M(glu)(dpa)]{sub n} (M=Co (1), Ni (2), Cu (3); glu=glutarate). Square pyramidal coordination is seen in 1-3, with semi-ligation of a sixth donor to produce a '5+1' extended coordination sphere. Neighboring metal atoms are linked into 1D [M(glu)]{sub n} neutral chains through chelating/monodentate bridging glutarate moieties with a syn-anti binding mode, and semi-chelation of the pendant carboxylate oxygen. These chains further connect into 2D layers through dipodal dpa ligands. Neighboring layers stack into the pseudo 3D crystal structure ofmore » 1-3 through supramolecular hydrogen bonding between dpa amine units and the semi-chelated glutarate oxygen atoms. The variable temperature magnetic behavior of 1-3 was explored and modeled as infinite 1D Heisenberg chains. Notably, complex 3 undergoes a thermally induced single crystal-to-single crystal transformation between centric and acentric space groups, with a conformationally disordered unilayer structure at 293 K and an ordered bilayer structure at 173 K. All materials were further characterized via infrared spectroscopy and elemental and thermogravimetric analyses. - Graphical abstract: The coordination polymers [M(glu)(dpa)]{sub n} (M=Co (1), Ni (2), Cu (3); glu=glutarate, dpa=4,4'-dipyridylamine) exhibit 2D layer structures based on 1D [M(glu)]{sub n} chains linked through dpa tethers. Antiferromagnetic coupling is observed for 2 and 3, while ferromagnetism is predominant in 1. Compound 3 undergoes a thermally induced single crystal-to-single crystal transformation from an acentric to a centrosymmetric space group.« less

  20. Dual-mesoporous ZSM-5 zeolite with highly b-axis-oriented large mesopore channels for the production of benzoin ethyl ether.

    PubMed

    Zhou, Xiaoxia; Chen, Hangrong; Zhu, Yan; Song, Yudian; Chen, Yu; Wang, Yongxia; Gong, Yun; Zhang, Guobin; Shu, Zhu; Cui, Xiangzhi; Zhao, Jinjin; Shi, Jianlin

    2013-07-22

    Dual-mesoporous ZSM-5 zeolite with highly b axis oriented large mesopores was synthesized by using nonionic copolymer F127 and cationic surfactant CTAB as co-templates. The product contains two types of mesopores--smaller wormlike ones of 3.3 nm in size and highly oriented larger ones of 30-50 nm in diameter along the b axis--and both of them interpenetrate throughout the zeolite crystals and interconnect with zeolite microporosity. The dual-mesoporous zeolite exhibits excellent catalytic performance in the condensation of benzaldehyde with ethanol and greater than 99 % selectivity for benzoin ethyl ether at room temperature, which can be ascribed to the zeolite lattice structure offering catalytically active sites and the hierarchical and oriented mesoporous structure providing fast access of reactants to these sites in the catalytic reaction. The excellent recyclability and high catalytic stability of the catalyst suggest prospective applications of such unique mesoporous zeolites in the chemical industry. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Ultrasonic assisted synthesis of Bikitaite zeolite: A potential material for hydrogen storage application.

    PubMed

    Roy, Priyanka; Das, Nandini

    2017-05-01

    Li containing Bikitaite zeolite has been synthesized by an ultrasound-assisted method and used as a potential material for hydrogen storage application. The Sonication energy was varied from 150W to 250W and irradiation time from 3h to 6h. The Bikitaite nanoparticles were characterized by X-ray diffraction (XRD), infrared (IR) spectral analysis, and field-emission scanning electron microscopy (FESEM) thermo-gravimetrical analysis and differential thermal analysis (TGA, DTA). XRD and IR results showed that phase pure, nano crystalline Bikitaite zeolites were started forming after 3h irradiation and 72h of aging with a sonication energy of 150W and nano crystalline Bikitaite zeolite with prominent peaks were obtained after 6h irradiation of 250W sonic energy. The Brunauer-Emmett-Teller (BET) surface area of the powder by N 2 adsorption-desorption measurements was found to be 209m 2 /g. The TEM micrograph and elemental analysis showed that desired atomic ratio of the zeolite was obtained after 6h irradiation. For comparison, sonochemical method, followed by the hydrothermal method, with same initial sol composition was studied. The effect of ultrasonic energy and irradiation time showed that with increasing sonication energy, and sonication time phase formation was almost completed. The FESEM images revealed that 50nm zeolite crystals were formed at room temperature. However, agglomerated particles having woollen ball like structure was obtained by sonochemical method followed by hydrothermal treatment at 100°C for 24h. The hydrogen adsorption capacity of Bikitaite zeolite with different Li content, has been investigated. Experimental results indicated that the hydrogen adsorption capacities were dominantly related to their surface areas as well as total pore volume of the zeolite. The hydrogen adsorption capacity of 143.2c.c/g was obtained at 77K and ambient pressure of (0.11MPa) for the Bikitaite zeolite with 100% Li, which was higher than the reported values for

  2. Zeolite formation from coal fly ash and heavy metal ion removal characteristics of thus-obtained Zeolite X in multi-metal systems.

    PubMed

    Jha, Vinay Kumar; Nagae, Masahiro; Matsuda, Motohide; Miyake, Michihiro

    2009-06-01

    Zeolitic materials have been prepared from coal fly ash as well as from a SiO(2)-Al(2)O(3) system upon NaOH fusion treatment, followed by subsequent hydrothermal processing at various NaOH concentrations and reaction times. During the preparation process, the starting material initially decomposed to an amorphous form, and the nucleation process of the zeolite began. The carbon content of the starting material influenced the formation of the zeolite by providing an active surface for nucleation. Zeolite A (Na-A) was transformed into zeolite X (Na-X) with increasing NaOH concentration and reaction time. The adsorption isotherms of the obtained Na-X based on the characteristics required to remove heavy ions such as Ni(2+), Cu(2+), Cd(2+) and Pb(2+) were examined in multi-metal systems. Thus obtained experimental data suggests that the Langmuir and Freundlich models are more accurate compared to the Dubinin-Kaganer-Radushkevich (DKR) model. However, the sorption energy obtained from the DKR model was helpful in elucidating the mechanism of the sorption process. Further, in going from a single- to multi-metal system, the degree of fitting for the Freundlich model compared with the Langmuir model was favored due to its basic assumption of a heterogeneity factor. The Extended-Langmuir model may be used in multi-metal systems, but gives a lower value for equilibrium sorption compared with the Langmuir model.

  3. Single-crystal-to-single-crystal transformation and solvochromic luminescence of a dinuclear gold(I)-(aza-[18]crown-6)dithiocarbamate compound.

    PubMed

    Tzeng, Biing-Chiau; Chao, An

    2015-01-26

    The treatment of [AuCl(SMe2 )] with an equimolar amount of NaO5 NCS2 (O5 NCS2 =(aza-[18]crown-6)dithiocarbamate) in CH3 CN gave [Au2 (O5 NCS2 )2 ]⋅2 CH3 CN (2⋅2 CH3 CN), and its crystal structure displays a dinuclear gold(I)-azacrown ether ring and an intermolecular gold(I)⋅⋅⋅gold(I) contact of 2.8355(3) Å in crystal lattices. It is noted that two other single crystals of 2⋅tert-butylbenzene⋅H2 O and 2⋅0.5 m-xylene can be successfully obtained from a single-crystal-to-single-crystal (SCSC) transformation process by immersing single crystals of 2⋅2 CH3 CN in the respective solvents, and both also show intermolecular gold(I)⋅⋅⋅gold(I) contacts of 2.9420(5) and 2.890(2)-2.902(2) Å, respectively. Significantly, the emissions of all three 2⋅solvates are well correlated with their respective intermolecular gold(I)⋅⋅⋅gold(I) contacts, where such contacts increase with 2⋅2 CH3 CN (2.8355(3) Å)<2⋅0.5 m-xylene (2.890(2)-2.902(2) Å)<2⋅tert-butylbenzene⋅H2 O (2.9420(5) Å), and their emission energies increase with 2⋅2 CH3 CN (602 nm)<2⋅0.5 m-xylene (583 nm)<2⋅tert-butylbenzene⋅H2 O (546 nm) as well. In this regard, we further examine the solvochromic luminescence for some other aromatics, and finally their emissions are within 546-602 nm. Obviously, the above results are mostly ascribed to the occurrence of intermolecular gold(I)⋅⋅⋅gold(I) contacts in 2⋅solvates, which are induced by the presence of various solvates in the solid state, as a key role to be responsible for their solvochromic luminescence. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. The evolution of machining-induced surface of single-crystal FCC copper via nanoindentation

    NASA Astrophysics Data System (ADS)

    Zhang, Lin; Huang, Hu; Zhao, Hongwei; Ma, Zhichao; Yang, Yihan; Hu, Xiaoli

    2013-05-01

    The physical properties of the machining-induced new surface depend on the performance of the initial defect surface and deformed layer in the subsurface of the bulk material. In this paper, three-dimensional molecular dynamics simulations of nanoindentation are preformed on the single-point diamond turning surface of single-crystal copper comparing with that of pristine single-crystal face-centered cubic copper. The simulation results indicate that the nucleation of dislocations in the nanoindentation test on the machining-induced surface and pristine single-crystal copper is different. The dislocation embryos are gradually developed from the sites of homogeneous random nucleation around the indenter in the pristine single-crystal specimen, while the dislocation embryos derived from the vacancy-related defects are distributed in the damage layer of the subsurface beneath the machining-induced surface. The results show that the hardness of the machining-induced surface is softer than that of pristine single-crystal copper. Then, the nanocutting simulations are performed along different crystal orientations on the same crystal surface. It is shown that the crystal orientation directly influences the dislocation formation and distribution of the machining-induced surface. The crystal orientation of nanocutting is further verified to affect both residual defect generations and their propagation directions which are important in assessing the change of mechanical properties, such as hardness and Young's modulus, after nanocutting process.

  5. Zeolite scaffolds for cultures of human breast cancer cells. Part II: Effect of pure and hybrid zeolite membranes on neoplastic and metastatic activity control.

    PubMed

    Tavolaro, Palmira; Martino, Guglielmo; Andò, Sebastiano; Tavolaro, Adalgisa

    2016-11-01

    This work is focused on the response of two invasive phenotypes of human breast cancer cells, MCF-7 and MDA-MB-231, grown on synthesized zeolite scaffolds in order to study the influence of those biomaterials in controlled conditions with and without anti-tumoral drug treatments. Our research was directed to the use of doxorubicin (DOX) and bergapten (5-MOP). The former is broadly considered the most active single agent available for the treatment of breast cancer, the second is a natural psoralen with an apoptotic effect. The results indicate that both drugs inhibit the cell viability of all cell lines grown on all zeolite scaffolds and that all Pure Zeolite Membranes are more responsive with respect to all Mixed Matrix Membranes. Moreover, the results after treatment with DOX at a concentration of 7.4μM for 24h, show that the expression of the matrix metalloproteinases (MMP-2 and MMP-9) is greatly reduced in both cell lines, especially in those adherent on Pure Zeolite Scaffolds. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Crystal structures of carbonates up to Mbar pressures determined by single crystal synchrotron radiation diffraction

    NASA Astrophysics Data System (ADS)

    Merlini, M.

    2013-12-01

    The recent improvements at synchrotron beamlines, currently allow single crystal diffraction experiments at extreme pressures and temperatures [1,2] on very small single crystal domains. We successfully applied such technique to determine the crystal structure adopted by carbonates at mantle pressures. The knowledge of carbon-bearing phases is in fact fundamental for any quantitative modelling of global carbon cycle. The major technical difficulty arises after first order transitions or decomposition reactions, since original crystal (apx. 10x10x5 μm3) is transformed in much smaller crystalline domains often with random orientation. The use of 3D reciprocal space visualization software and the improved resolution of new generation flat panel detectors, however, allow both identification and integration of each single crystal domain, with suitable accuracy for ab-initio structure solution, performed with direct and charge-flipping methods and successive structure refinements. The results obtained on carbonates, indicate two major crystal-chemistry trends established at high pressures. The CO32- units, planar and parallel in ambient pressure calcite and dolomite structures, becomes non parallel in calcite- and dolomite-II and III phases, allowing more flexibility in the structures with possibility to accommodate strain arising from different cation sizes (Ca and Mg in particular). Dolomite-III is therefore also observed to be thermodynamically stable at lower mantle pressures and temperatures, differently from dolomite, which undergoes decomposition into pure end-members in upper mantle. At higher pressure, towards Mbar (lowermost mantle and D'' region) in agreement with theoretical calculations [3,4] and other experimental results [5], carbon coordination transform into 4-fold CO4 units, with different polymerisation in the structure depending on carbonate composition. The second important crystal chemistry feature detected is related to Fe2+ in Fe

  7. Nano-sized zeolites as modulators of thiacloprid toxicity on Chironomus riparius

    PubMed Central

    Wicht, Anna-Jorina; Guluzada, Leyla; Crone, Barbara; Karst, Uwe; Lee, Hwa Jun; Triebskorn, Rita; Haderlein, Stefan B.; Huhn, Carolin; Köhler, Heinz-R.

    2017-01-01

    This study investigated whether zeolites of different size (Y30 (nano-sized) and H-Beta(OH)-III (forming large aggregates/agglomerates composed of 50 nm small primary particles)) exerted acute toxicity on larvae of the non-biting midge, Chironomus riparius, and whether such zeolites are able to modulate the toxicity of a common insecticide, thiacloprid, by means of adsorption of a dissolved toxicant. We conducted acute toxicity tests with fourth instar larvae of C. riparius. In these tests, larvae were exposed to zeolites or thiacloprid solely, or to mixtures of both compounds. The mixtures comprised 1.0 µg/L thiacloprid in addition to low (5.2 mg/L), medium (18.2 mg/L), and high (391.7 mg/L) zeolite concentrations, resulting in different adsorption rates of thiacloprid. As biological endpoints, changes in mortality rates and in behavior were monitored every 24 h over a total investigation period of 96 h. Furthermore, we conducted chemical analyses of thiacloprid in the medium and the larvae and located the zeolite particles within the larvae by LA-ICP-MS imaging techniques. Our results demonstrate that both types of zeolites did not exert acute toxicity when applied as single-substances, but led to reduced acute toxicity of thiacloprid when applied together with thiacloprid. These results are in line with the sorption properties of zeolites indicating reduced bioavailability of thiacloprid, although our data indicate that thiacloprid can desorb from zeolites to some extent. While freely dissolved (i.e., non-sorbed) fraction of thiacloprid was a good parameter to roughly estimate toxic effects, it did not correlate with measured internal thiacloprid concentrations. Moreover, it was shown that both zeolite types were ingested by the larvae, but no indication for cellular uptake of them was found. PMID:28729952

  8. A first-principle model of 300 mm Czochralski single-crystal Si production process for predicting crystal radius and crystal growth rate

    NASA Astrophysics Data System (ADS)

    Zheng, Zhongchao; Seto, Tatsuru; Kim, Sanghong; Kano, Manabu; Fujiwara, Toshiyuki; Mizuta, Masahiko; Hasebe, Shinji

    2018-06-01

    The Czochralski (CZ) process is the dominant method for manufacturing large cylindrical single-crystal ingots for the electronics industry. Although many models and control methods for the CZ process have been proposed, they were only tested with small equipment and only a few industrial application were reported. In this research, we constructed a first-principle model for controlling industrial CZ processes that produce 300 mm single-crystal silicon ingots. The developed model, which consists of energy, mass balance, hydrodynamic, and geometrical equations, calculates the crystal radius and the crystal growth rate as output variables by using the heater input, the crystal pulling rate, and the crucible rise rate as input variables. To improve accuracy, we modeled the CZ process by considering factors such as changes in the positions of the crucible and the melt level. The model was validated with the operation data from an industrial 300 mm CZ process. We compared the calculated and actual values of the crystal radius and the crystal growth rate, and the results demonstrated that the developed model simulated the industrial process with high accuracy.

  9. Construction of Zeolite-Like Cluster Organic Frameworks from 3 d-4 d/3 d-3 d Heterometallic Supertetrahedral Secondary Building Units: Syntheses, Structures, and Properties.

    PubMed

    Lin, Li-Dan; Deng, Chu-Chu; Zhao, D; Li, Xin-Xiong; Zheng, Shou-Tian

    2018-01-02

    Two zeolite-like cluster organic frameworks based on Cd-Cu/Mn-Cu heterometallic supertetrahedral secondary building units have been successfully constructed under solvothermal conditions, namely, Cu[Cd 4 Cu 6 (L) 4 (H 2 O) 18 ](Ac) 9 ⋅DMA⋅3 H 2 O (1), and Cu[Mn 4 Cu 6 (L) 4 (Ac) 3 (H 2 O) 12 ](Ac) 6 ⋅CH 3 CN⋅13 H 2 O (2), where H 3 L=2-(hydroxymethyl)-2-(pyridin-4-yl)-1,3-propanediol, Ac=CH 3 COO - , DMA=N,N'-dimethylacetamide. Single-crystal X-ray structural analysis reveals that both 1 and 2 exhibit 3-dimensional zeolite-like architectures with similar 4-connected components, but possess definitely different topologies of diamondoid (dia) and uncommon lonsdaleite (lon), respectively. 1 and 2 represent the first cases of zeolite-like cluster organic frameworks containing Cd-Cu/Mn-Cu heterometallic supertetrahedral secondary building units. Furthermore, the magnetic properties and porous nature of 1 and 2 were also studied. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Positron annihilation lifetime spectroscopy (PALS) study of the as prepared and calcined MFI zeolites

    NASA Astrophysics Data System (ADS)

    Bosnar, Sanja; Vrankić, Martina; Bosnar, Damir; Ren, Nan; Šarić, Ankica

    2017-11-01

    The synthesis of high silica zeolites in many cases implies the usage of organic structural direction agents (SDA). However, to manifest their functionalities, the SDA occluded inside the channels of the as-synthesized structure should be removed, usually by a high temperature treatment (calcination). In this paper, the positron annihilation lifetime spectroscopy (PALS) was used to monitor the development of accessible spaces, their sizes and distributions in MFI zeolites, ZSM-5 and silicalite-1 in order to give an additional insight in the process of the SDA removal. For that purpose, a conventional PALS setup with 22Na positron source was applied. It was established that there is a pronounced difference between positron annihilation data for these two zeolites of the same structural type. The samples were additionally analysed by X-ray powder diffraction at room temperature with a crystal structure refinement and thermogravimetry.

  11. 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.

  12. DDR-type zeolite membrane synthesis, modification and gas permeation studies

    DOE PAGES

    Yang, Shaowei; Cao, Zishu; Arvanitis, Antonios; ...

    2016-01-22

    DDR-type zeolite membrane was synthesized on porous α-alumina substrate by hydrothermal treatment of a ball-milled Sigmal-1 crystal seed layer in an aluminum-free precursor solution containing 1-Adamantylamine as the structure directing agent (SDA). The as-synthesized DDR zeolite membranes were defect-free but the supported zeolite layers were susceptible to crack development during the subsequent high-temperature SDA removal process. The cracks were effectively eliminated by the liquid phase chemical deposition method using tetramethoxysilane as the precursor for silica deposits. The modified membrane was extensively studied for H 2, He, O 2, N 2, CO 2, CH 4, and i-C 4H 10 pure gasmore » permeation and CO 2/CH 4 mixture separation. At 297 K and 2-bar feed gas pressure, the membrane achieved a CO 2/CH 4 separation factor of ~92 for a feed containing 90% CO 2, which decreased to 62 for a feed containing 10% CO 2 with the CO 2 permeance virtually unchanged at ~1.8×10 –7 mol/m• sup>2 s • Pa regardless of the feed composition. It also exhibited an O 2/N 2 permselectivity of 1.8 at 297 K. Furthermore, the gas permeation behaviors of the current aluminum-containing DDR type zeolite membrane are generally in good agreement with the findings in both experimental and theoretical studies on the pure-silica DDR membranes in recent literature.« less

  13. Method for harvesting rare earth barium copper oxide single crystals

    DOEpatents

    Todt, V.R.; Sengupta, S.; Shi, D.

    1996-04-02

    A method of preparing high temperature superconductor single crystals is disclosed. The method of preparation involves preparing precursor materials of a particular composition, heating the precursor material to achieve a peritectic mixture of peritectic liquid and crystals of the high temperature superconductor, cooling the peritectic mixture to quench directly the mixture on a porous, wettable inert substrate to wick off the peritectic liquid, leaving single crystals of the high temperature superconductor on the porous substrate. Alternatively, the peritectic mixture can be cooled to a solid mass and reheated on a porous, inert substrate to melt the matrix of peritectic fluid while leaving the crystals melted, allowing the wicking away of the peritectic liquid. 2 figs.

  14. 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.

  15. Synthesis of Engineered Zeolitic Materials: From Classical Zeolites to Hierarchical Core-Shell Materials.

    PubMed

    Masoumifard, Nima; Guillet-Nicolas, Rémy; Kleitz, Freddy

    2018-04-01

    The term "engineered zeolitic materials" refers to a class of materials with a rationally designed pore system and active-sites distribution. They are primarily made of crystalline microporous zeolites as the main building blocks, which can be accompanied by other secondary components to form composite materials. These materials are of potential importance in many industrial fields like catalysis or selective adsorption. Herein, critical aspects related to the synthesis and modification of such materials are discussed. The first section provides a short introduction on classical zeolite structures and properties, and their conventional synthesis methods. Then, the motivating rationale behind the growing demand for structural alteration of these zeolitic materials is discussed, with an emphasis on the ongoing struggles regarding mass-transfer issues. The state-of-the-art techniques that are currently available for overcoming these hurdles are reviewed. Following this, the focus is set on core-shell composites as one of the promising pathways toward the creation of a new generation of highly versatile and efficient engineered zeolitic substances. The synthesis approaches developed thus far to make zeolitic core-shell materials and their analogues, yolk-shell, and hollow materials, are also examined and summarized. Finally, the last section concisely reviews the performance of novel core-shell, yolk-shell, and hollow zeolitic materials for some important industrial applications. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Fe-Al alloy single-crystal thin film preparation for basic magnetic measurements

    NASA Astrophysics Data System (ADS)

    Abe, Tatsuya; Kawai, Tetsuroh; Futamoto, Masaaki; Ohtake, Mitsuru; Inaba, Nobuyuki

    2018-04-01

    Fe100-xAlx (x = 0, 4, 10, 20, 30 at. %) alloy films of 40 nm thickness are prepared on MgO(001) single-crystal substrates by varying substrate temperature from room temperature to 600 °C. Single-crystal films of (001) orientation with bcc-based disordered A2 structure are obtained for the Al content range of x = 0 - 20 at. %. An ordered phase of DO3 structure is observed in Fe70Al30 films prepared at temperatures higher than 200 °C, whereas (001) oriented single-crystal films of A2 structure are obtained when prepared at room temperature. The film surface profile does not depend much on the film composition, while the surface roughness increases with increasing substrate temperature. Island-like crystals are observed for films prepared at 600°C for all compositions. Difference in lattice spacing measured parallel and perpendicular to the substrate is noted for the single-crystal thin films and it increases with increasing Al content. The lattice strain in single-crystal film is caused possibly to accommodate the lattice mismatch with the MgO substrate. The (001)-oriented single-crystal films with A2 structure show four-fold symmetries in in-plane magnetic anisotropy with the easy magnetization axis A2[100] and the hard magnetization axis A2[110], whereas the films with DO3 ordered structure show almost isotropic magnetic properties.

  17. Study of structural and optical properties of YAG and Nd:YAG single crystals

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

    Kostić, S.; Lazarević, Z.Ž., E-mail: lzorica@yahoo.com; Radojević, V.

    2015-03-15

    Highlights: • Transparent YAG and pale pink Nd:YAG single crystals were produced by the Czochralski technique. • Growth mechanisms and shape of the liquid/solid interface and incorporation of Nd{sup 3+} were studied. • The structure of the crystals was investigated by X-ray diffraction, Raman and IR spectroscopy. • The 15 Raman and 17 IR modes were observed. • The obtained YAG and Nd:YAG single crystals were without core and of good optical quality. - Abstract: Yttrium aluminum garnet (YAG, Y{sub 3}Al{sub 5}O{sub 12}) and yttrium aluminum garnet doped with neodymium (Nd:YAG) single crystals were grown by the Czochralski technique. Themore » critical diameter and the critical rate of rotation were calculated. Suitable polishing and etching solutions were determined. As a result of our experiments, the transparent YAG and pale pink Nd:YAG single crystals were produced. The obtained crystals were studied by X-ray diffraction, Raman and IR spectroscopy. The crystal structure was confirmed by XRD. The 15 Raman and 17 IR modes were observed. The Raman and IR spectroscopy results are in accordance with X-ray diffraction analysis. The obtained YAG and Nd:YAG single crystals were without core and of good optical quality. The absence of a core was confirmed by viewing polished crystal slices. Also, it is important to emphasize that the obtained Nd:YAG single crystal has a concentration of 0.8 wt.% Nd{sup 3+} that is characteristic for laser materials.« less

  18. Special Features of the Structure of Single-Crystal Refractory Nickel Alloy Under Directed Crystallization

    NASA Astrophysics Data System (ADS)

    Bondarenko, Yu. A.; Echin, A. B.; Surova, V. A.; Kolodyazhnyi, M. Yu.

    2017-05-01

    The effect of the conditions of directed crystallization (the temperature gradient and the crystallization rate) on the dendrite spacing, on the size of the particles of the hardening γ'-phase in the arms and arm spaces of the dendrites, on the volume fraction and size of the pores, on the size of the particles of the eutectic γ/γ'-phase, and on the features of dendritic segregation in a single-crystal castable refractory alloy is studied.

  19. Disappearing Enantiomorphs: Single Handedness in Racemate Crystals.

    PubMed

    Parschau, Manfred; Ernst, Karl-Heinz

    2015-11-23

    Although crystallization is the most important method for the separation of enantiomers of chiral molecules in the chemical industry, the chiral recognition involved in this process is poorly understood at the molecular level. We report on the initial steps in the formation of layered racemate crystals from a racemic mixture, as observed by STM at submolecular resolution. Grown on a copper single-crystal surface, the chiral hydrocarbon heptahelicene formed chiral racemic lattice structures within the first layer. In the second layer, enantiomerically pure domains were observed, underneath which the first layer contained exclusively the other enantiomer. Hence, the system changed from a 2D racemate into a 3D racemate with enantiomerically pure layers after exceeding monolayer-saturation coverage. A chiral bias in form of a small enantiomeric excess suppressed the crystallization of one double-layer enantiomorph so that the pure minor enantiomer crystallized only in the second layer. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Reliability analysis of single crystal NiAl turbine blades

    NASA Technical Reports Server (NTRS)

    Salem, Jonathan; Noebe, Ronald; Wheeler, Donald R.; Holland, Fred; Palko, Joseph; Duffy, Stephen; Wright, P. Kennard

    1995-01-01

    As part of a co-operative agreement with General Electric Aircraft Engines (GEAE), NASA LeRC is modifying and validating the Ceramic Analysis and Reliability Evaluation of Structures algorithm for use in design of components made of high strength NiAl based intermetallic materials. NiAl single crystal alloys are being actively investigated by GEAE as a replacement for Ni-based single crystal superalloys for use in high pressure turbine blades and vanes. The driving force for this research lies in the numerous property advantages offered by NiAl alloys over their superalloy counterparts. These include a reduction of density by as much as a third without significantly sacrificing strength, higher melting point, greater thermal conductivity, better oxidation resistance, and a better response to thermal barrier coatings. The current drawback to high strength NiAl single crystals is their limited ductility. Consequently, significant efforts including the work agreement with GEAE are underway to develop testing and design methodologies for these materials. The approach to validation and component analysis involves the following steps: determination of the statistical nature and source of fracture in a high strength, NiAl single crystal turbine blade material; measurement of the failure strength envelope of the material; coding of statistically based reliability models; verification of the code and model; and modeling of turbine blades and vanes for rig testing.

  1. 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.

  2. Design and characterization of chitosan/zeolite composite films--Effect of zeolite type and zeolite dose on the film properties.

    PubMed

    Barbosa, Gustavo P; Debone, Henrique S; Severino, Patrícia; Souto, Eliana B; da Silva, Classius F

    2016-03-01

    Chitosan films can be used as wound dressings for the treatment of chronic wounds and severe burns. The antimicrobial properties of these films may be enhanced by the addition of silver. Despite the antimicrobial activity of silver, several studies have reported the cytotoxicity as a factor limiting its biomedical applications. This problem may, however, be circumvented by the provision of sustained release of silver. Silver zeolites can be used as drug delivery platforms to extend the release of silver. The objective of this study was to evaluate the addition of clinoptilolite and A-type zeolites in chitosan films. Sodium zeolites were initially subjected to ion-exchange in a batch reactor. Films were prepared by casting technique using a 2% w/w chitosan solution and two zeolite doses (0.1 or 0.2% w/w). Films were characterized by thermal analysis, color analysis, scanning electron microscopy, X-ray diffraction, and water vapor permeation. The results showed that films present potential for application as dressing. The water vapor permeability is one of the main properties in wound dressings, the best results were obtained for A-type zeolite/chitosan films, which presented a brief reduction of this property in relation to zeolite-free chitosan film. On the other hand, the films containing clinoptilolite showed lower water vapor permeation, which may be also explained by the best distribution of the particles into the polymer which also promoted greater thermal resistance.

  3. Synthesis, crystal growth, structural, thermal, optical and mechanical properties of solution grown 4-methylpyridinium 4-hydroxybenzoate single crystal.

    PubMed

    Sudhahar, S; Krishna Kumar, M; Sornamurthy, B M; Mohan Kumar, R

    2014-01-24

    Organic nonlinear optical material, 4-methylpyridinium 4-hydroxybenzoate (4MPHB) was synthesized and single crystal was grown by slow evaporation solution growth method. Single crystal and powder X-ray diffraction analyses confirm the structure and crystalline perfection of 4MPHB crystal. Infrared, Raman and NMR spectroscopy techniques were used to elucidate the functional groups present in the compound. TG-DTA analysis was carried out in nitrogen atmosphere to study the decomposition stages, endothermic and exothermic reactions. UV-visible and Photoluminescence spectra were recorded for the grown crystal to estimate the transmittance and band gap energy respectively. Linear refractive index, birefringence, and SHG efficiency of the grown crystal were studied. Laser induced surface damage threshold and mechanical properties of grown crystal were studied to assess the suitability of the grown crystals for device applications. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. Self-cavity lasing in optically pumped single crystals of p-sexiphenyl

    NASA Astrophysics Data System (ADS)

    Yanagi, Hisao; Tamura, Kenji; Sasaki, Fumio

    2016-08-01

    Organic single-crystal self-cavities are prepared by solution growth of p-sexiphenyl (p-6P). Based on Fabry-Pérot feedback inside a quasi-lozenge-shaped platelet crystal, edge-emitting laser is obtained under optical pumping. The multimode lasing band appears at the 0-1 or 0-2 vibronic progressions depending on the excitation conditions which affect the self-absorption effect. Cavity-size dependence of amplified spontaneous emission (ASE) is investigated with laser-etched single crystals of p-6P. As the cavity length of square-shaped crystal is reduced from 100 to 10 μm, ASE threshold fluence is decreased probably due to size-dependent light confinement in the crystal cavity.

  5. Environmental Qualification of a Single-Crystal Silicon Mirror for Spaceflight Use

    NASA Technical Reports Server (NTRS)

    Hagopian, John; Chambers, John; Rohrback. Scott; Bly, Vincent; Morell, Armando; Budinoff, Jason

    2013-01-01

    This innovation is the environmental qualification of a single-crystal silicon mirror for spaceflight use. The single-crystal silicon mirror technology is a previous innovation, but until now, a mirror of this type has not been qualified for spaceflight use. The qualification steps included mounting, gravity change measurements, vibration testing, vibration- induced change measurements, thermal cycling, and testing at the cold operational temperature of 225 K. Typical mirrors used for cold applications for spaceflight instruments include aluminum, beryllium, glasses, and glass-like ceramics. These materials show less than ideal behavior after cooldown. Single-crystal silicon has been demonstrated to have the smallest change due to temperature change, but has not been spaceflight-qualified for use. The advantage of using a silicon substrate is with temperature stability, since it is formed from a stress-free single crystal. This has been shown in previous testing. Mounting and environmental qualification have not been shown until this testing.

  6. Micro pulling down growth of very thin shape memory alloys single crystals

    NASA Astrophysics Data System (ADS)

    López-Ferreño, I.; Juan, J. San; Breczewski, T.; López, G. A.; Nó, M. L.

    Shape memory alloys (SMAs) have attracted much attention in the last decades due to their thermo-mechanical properties such as superelasticity and shape memory effect. Among the different families of SMAs, Cu-Al-Ni alloys exhibit these properties in a wide range of temperatures including the temperature range of 100-200∘C, where there is a technological demand of these functional materials, and exhibit excellent behavior at small scale making them more competitive for applications in Micro Electro-Mechanical Systems (MEMS). However, polycrystalline alloys of Cu-based SMAs are very brittle so that they show their best thermo-mechanical properties in single-crystal state. Nowadays, conventional Bridgman and Czochralski methods are being applied to elaborate single-crystal rods up to a minimum diameter of 1mm, but no works have been reported for smaller diameters. With the aim of synthesizing very thin single-crystals, the Micro-Pulling Down (μ-PD) technique has been applied, for which the capillarity and surface tension between crucible and the melt play a critical role. The μ-PD method has been successfully applied to elaborate several cylindrical shape thin single-crystals down to 200μm in diameter. Finally, the martensitic transformation, which is responsible for the shape memory properties of these alloys, has been characterized for different single-crystals. The experimental results evidence the good quality of the grown single-crystals.

  7. Catalytic Fast Pyrolysis of Cellulose Using Nano Zeolite and Zeolite/Matrix Catalysts in a GC/Micro-Pyrolyzer.

    PubMed

    Lee, Kyong-Hwan

    2016-05-01

    Cellulose, as a model compound of biomass, was catalyzed over zeolite (HY,.HZSM-5) and zeolite/matrix (HY/Clay, HM/Clay) in a GC/micro-pyrolyzer at 500 degrees C, to produce the valuable products. The catalysts used were pure zeolite and zeolite/matrix including 20 wt% matrix content, which were prepared into different particle sizes (average size; 0.1 mm, 1.6 mm) to study the effect of the particle size of the catalyst for the distribution of product yields. Catalytic pyrolysis had much more volatile products as light components and less content of sugars than pyrolysis only. This phenomenon was strongly influenced by the particle size of the catalyst in catalytic fast pyrolysis. Also, in zeolite and zeolite/matrix catalysts the zeolite type gave the dominant impact on the distribution of product yields.

  8. Self-Aligned Growth of Organic Semiconductor Single Crystals by Electric Field.

    PubMed

    Kotsuki, Kenji; Obata, Seiji; Saiki, Koichiro

    2016-01-19

    We proposed a novel but facile method for growing organic semiconductor single-crystals via solvent vapor annealing (SVA) under electric field. In the conventional SVA growth process, nuclei of crystals appeared anywhere on the substrate and their crystallographic axes were randomly distributed. We applied electric field during the SVA growth of 2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene (C8-BTBT) on the SiO2/Si substrate on which a pair of electrodes had been deposited beforehand. Real-time observation of the SVA process revealed that rodlike single crystals grew with their long axes parallel to the electric field and bridged the prepatterned electrodes. As a result, C8-BTBT crystals automatically formed a field effect transistor (FET) structure and the mobility reached 1.9 cm(2)/(V s). Electric-field-assisted SVA proved a promising method for constructing high-mobility single-crystal FETs at the desired position by a low-cost solution process.

  9. 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.

  10. Elastic-plastic deformation of molybdenum single crystals shocked along [100

    DOE PAGES

    Mandal, A.; Gupta, Y. M.

    2017-01-24

    To understand the elastic-plastic deformation response of shock-compressed molybdenum (Mo) – a body-centered cubic (BCC) metal, single crystal samples were shocked along the [100] crystallographic orientation to an elastic impact stress of 12.5 GPa. Elastic-plastic wave profiles, measured at different propagation distances ranging between ~0.23 to 2.31 mm using laser interferometry, showed a time-dependent material response. Within experimental scatter, the measured elastic wave amplitudes were nearly constant over the propagation distances examined. These data point to a large and rapid elastic wave attenuation near the impact surface, before reaching a threshold value (elastic limit) of ~3.6 GPa. Numerical simulations ofmore » the measured wave profiles, performed using a dislocation-based continuum model, suggested that {110}<111> and/or {112}<111> slip systems are operative under shock loading. In contrast to shocked metal single crystals with close-packed structures, the measured wave profiles in Mo single crystals could not be explained in terms of dislocation multiplication alone. A dislocation generation mechanism, operative for shear stresses larger than that at the elastic limit, was required to model the rapid elastic wave attenuation and to provide a good overall match to the measured wave profiles. However, the physical basis for this mechanism was not established for the high-purity single crystal samples used in this study. As a result, the numerical simulations also suggested that Mo single crystals do not work harden significantly under shock loading in contrast to the behavior observed under quasi-static loading.« less

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

    NASA Astrophysics Data System (ADS)

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

    2008-01-01

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

  12. Life Prediction of Turbine Blade Nickel Base Superalloy Single Crystals.

    DTIC Science & Technology

    1986-08-01

    mechanical properties between single crystals and the DS version of Mar-M200. Soon it was recognized again through the mechanical property - structure ... property achievements demonstrated by screening and simulated engine tests. 1 Single crystals are the results of extensive investigation on the mechanical ...behavior, (especially fatigue and creep) of, and the structure - property correlations in the equiaxed and directionally solidified (DS) nickel-base

  13. Experimental Investigation of Orthoenstatite Single Crystal Rheology

    NASA Astrophysics Data System (ADS)

    fraysse, G.; Girard, J.; Holyoke, C. W.; Raterron, P.

    2013-12-01

    The plasticity of enstatite, upper mantle second most abundant mineral, is still poorly constrained, mostly because of its high-temperature (T) transformation into proto- and clino-enstatite at low pressure (P). Mackwell (1991, GRL, 18, 2027) reports a pioneer study of protoenstatite (Pbcn) single-crystal rheology, but the results do not directly apply to the orthorhombic (Pbca) mantle phase. Ohuchi et al. (2011, Contri. Mineral. Petrol , 161, 961) carried out deformation experiments at P=1.3 GPa on oriented orthoenstatite crystals, investigating the activity of [001](100) and [001](010) dislocation slip systems; they report the first rheological laws for orthoenstatite crystals. However, strain and stress were indirectly constrained in their experiments, which questioned whether steady state conditions of deformation were achieved. Also, data reported for [001](100) slip system were obtained after specimens had transformed by twinning into clinoenstatite. We report here new data from deformation experiments carried out at high T and P ranging from 3.5 to 6.2 GPa on natural Fe-bearing enstatite single crystals, using the Deformation-DIA apparatus (D-DIA) that equipped the X17B2 beamline of the NSLS (NY, USA). The applied stress and specimen strain rates were measured in situ by X-ray diffraction and imaging techniques (e.g., Raterron & Merkel, 2009, J. Sync. Rad., 16, 748; Raterron et al., 2013, Rev. Sci. Instr., 84, 043906). Three specimen orientations were tested: i) with the compression direction along [101]c crystallographic direction, which forms a 45° angle with both [100] and [001] axes, to investigate [001](100) slip-system activity; ii) along [011]c direction to investigate [001](010) system activity; iii) and along enstatite [125] axis, to activate both slip systems together. Crystals were deformed two by two, to compare slip system activities, or against enstatite aggregates or orientated olivine crystals of known rheology for comparison. Run products

  14. Trapezoidal diffraction grating beam splitters in single crystal diamond

    NASA Astrophysics Data System (ADS)

    Kiss, Marcell; Graziosi, Teodoro; Quack, Niels

    2018-02-01

    Single Crystal Diamond has been recognized as a prime material for optical components in high power applications due to low absorption and high thermal conductivity. However, diamond microstructuring remains challenging. Here, we report on the fabrication and characterization of optical diffraction gratings exhibiting a symmetric trapezoidal profile etched into a single crystal diamond substrate. The optimized grating geometry diffracts the transmitted optical power into precisely defined proportions, performing as an effective beam splitter. We fabricate our gratings in commercially available single crystal CVD diamond plates (2.6mm x 2.6mm x 0.3mm). Using a sputter deposited hard mask and patterning by contact lithography, the diamond is etched in an inductively coupled oxygen plasma with zero platen power. The etch process effectively reveals the characteristic {111} diamond crystal planes, creating a precisely defined angled (54.7°) profile. SEM and AFM measurements of the fabricated gratings evidence the trapezoidal shape with a pitch of 3.82μm, depth of 170 nm and duty cycle of 35.5%. Optical characterization is performed in transmission using a 650nm laser source perpendicular to the sample. The recorded transmitted optical power as function of detector rotation angle shows a distribution of 21.1% in the 0th order and 23.6% in each +/-1st order (16.1% reflected, 16.6% in higher orders). To our knowledge, this is the first demonstration of diffraction gratings with trapezoidal profile in single crystal diamond. The fabrication process will enable beam splitter gratings of custom defined optical power distribution profiles, while antireflection coatings can increase the efficiency.

  15. Lithium niobate single-crystal and photo-functional device

    DOEpatents

    Gopalan, Venkatraman; Mitchell, Terrence E.; Kitamura, Kenji; Furukawa, Yasunori

    2001-01-01

    Provided are lithium niobate single-crystal that requires a low voltage of not larger than 10 kV/nm for its ferroelectric polarization inversion and of which the polarization can be periodically inverted with accuracy even at such a low voltage, and a photo-functional device comprising the crystal. The crystal has a molar fraction of Li.sub.2 O/(Nb.sub.2 O.sub.5 +Li.sub.2 O) of falling between 0.49 and 0.52. The photo-functional device can convert a laser ray being incident thereon.

  16. New antiaxillary odour deodorant made with antimicrobial Ag-zeolite (silver-exchanged zeolite).

    PubMed

    Nakane, T; Gomyo, H; Sasaki, I; Kimoto, Y; Hanzawa, N; Teshima, Y; Namba, T

    2006-08-01

    The causative substances for axillary osmidrosis, which are often found in apocrine sweat, are the decomposed/denatured products of short-chain fatty acid and other biological metabolite compounds produced by axillary-resident bacteria. Conventional underarm deodorants suppress the process of odour production mostly by the following mechanism: (1) suppression of perspiration, (2) reduction in numbers of resident bacteria, (3) deodorization and (4) masking. The most important and effective method to reduce odour is to suppress the growth of resident bacteria with antimicrobials, which have several drawbacks, especially in their safety aspect. To solve these problems, we focused on Ag-zeolite (silver-exchanged zeolite) that hold stable Ag, an inorganic bactericidal agent, in its structure, and therefore, poses less risk in safety. Its bactericidal effect on skin-resident bacteria was found to be excellent and comparable with that of triclosan, a most frequently used organic antimicrobial in this product category. The dose-response study of Ag-zeolite powder spray (0-40 w/w%) using 39 volunteers revealed that 5-40 w/w% Ag-zeolite could show a sufficient antimicrobial effect against skin-resident bacteria. The comparison study using 0.2 w/w% triclosan as the control and 10 w/w% Ag-zeolite indicated that: (1) one application of the powder spray containing 10 w/w% Ag-zeolite could show a sufficient antimicrobial effect against the resident bacteria and its effect continued for 24 h, (2) a powder spray containing 0.2 w/w% triclosan was unable to show a sufficient antimicrobial effect, and (3) no adverse event was observed. These studies show that Ag-zeolite has a superior antimicrobial ability that is rarely found in conventional antimicrobials used in deodorant products and a strong antiaxillary odour deodorant ability because of its long-lasting effect. During clinical study, patch tests with humans and other clinical studies of this product showed no adverse events

  17. Carbon dots in zeolites: A new class of thermally activated delayed fluorescence materials with ultralong lifetimes

    PubMed Central

    Liu, Jiancong; Wang, Ning; Yu, Yue; Yan, Yan; Zhang, Hongyue; Li, Jiyang; Yu, Jihong

    2017-01-01

    Thermally activated delayed fluorescence (TADF) materials are inspiring intensive research in optoelectronic applications. To date, most of the TADF materials are limited to metal-organic complexes and organic molecules with lifetimes of several microseconds/milliseconds that are sensitive to oxygen. We report a facial and general “dots-in-zeolites” strategy to in situ confine carbon dots (CDs) in zeolitic matrices during hydrothermal/solvothermal crystallization to generate high-efficient TADF materials with ultralong lifetimes. The resultant CDs@zeolite composites exhibit high quantum yields up to 52.14% and ultralong lifetimes up to 350 ms at ambient temperature and atmosphere. This intriguing TADF phenomenon is due to the fact that nanoconfined space of zeolites can efficiently stabilize the triplet states of CDs, thus enabling the reverse intersystem crossing process for TADF. Meanwhile, zeolite frameworks can also hinder oxygen quenching to present TADF behavior at air atmosphere. This design concept introduces a new perspective to develop materials with unique TADF performance and various novel delayed fluorescence–based applications. PMID:28560347

  18. Bulk crystal growth and their effective third order nonlinear optical properties of 2-(4-fluorobenzylidene) malononitrile (FBM) single crystal

    NASA Astrophysics Data System (ADS)

    Priyadharshini, A.; Kalainathan, S.

    2018-04-01

    2-(4-fluorobenzylidene) malononitrile (FBM), an organic third order nonlinear (TONLO) single crystal with the dimensions of 32 × 7 × 11 mm3, has been successfully grown in acetone solution by slow evaporation technique at 35 °C. The crystal system (triclinic), space group (P-1) and crystalline purity of the titular crystal were measured by single crystal and powder X-ray diffraction, respectively. The molecular weight and the multiple functional groups of the FBM material were confirmed through the mass and FT-IR spectral analysis. UV-Vis-NIR spectral study enroles that the FBM crystal exhibits excellent transparency (83%) in the entire visible and near infra-red region with a wide bandgap 2.90 eV. The low dielectric constant (εr) value of FBM crystal is appreciable for microelectronics industry applications. Thermal stability and melting point (130.09 °C) were ascertained by TGA-DSC analysis. The laser-induced surface damage threshold (LDT) value of FBM specimen is found to be 2.14 GW/cm2, it is fairly good compared to other reported NLO crystals. The third - order nonlinear optical character of the FBM crystal was confirmed through the typical single beam Z-scan technique. All these finding authorized that the organic crystal of FBM is favorably suitable for NLO applications.

  19. Hydrothermal synthesis of zeolite T from kaolin using two different structure-directing agents

    NASA Astrophysics Data System (ADS)

    Arshad, Sazmal E.; Lutfor Rahman, M.; Sarkar, Shaheen M.; Yusslee, Eddy F.; Patuwan, Siti Z.

    2018-01-01

    Zeolite T was synthesized from the molar chemical composition of 1SiO2:0.04Al2O3:0.26Na2O:0.09K2O:14H2O in the form of a homogenous milky solution in the presence of the two different structure-directing agents TMAOH and TEAOH respectively. Modification of the composition of silica was undertaken using metakaolin from calcined kaolin at 750 °C for 4 h, while the molar composition of each different SDA was variated from 0.05, 0.10, 0.15, 0.20 and 0.25. The homogenous mixture was left at room temperature for 24 h before undergoing hydrothermal synthesis at 100 °C for 168 h. The synthesized samples were filtered and aged at 120 °C for 2 h and each sample was calcined at high temperatures (545 °C for TMAOH and 520 °C for TEAOH) for template removal before characterization using XRD and SEM. Crystallization of the zeolite T in its major form only took place at a molar ratio of 0.10 of TMAOH, while TEAOH showed the species evolution of zeolite T into zeolite L and W for other molar ratios.

  20. Deformation induced microtwins and stacking faults in aluminum single crystal.

    PubMed

    Han, W Z; Cheng, G M; Li, S X; Wu, S D; Zhang, Z F

    2008-09-12

    Microtwins and stacking faults in plastically deformed aluminum single crystal were successfully observed by high-resolution transmission electron microscope. The occurrence of these microtwins and stacking faults is directly related to the specially designed crystallographic orientation, because they were not observed in pure aluminum single crystal or polycrystal before. Based on the new finding above, we propose a universal dislocation-based model to judge the preference or not for the nucleation of deformation twins and stacking faults in various face-centered-cubic metals in terms of the critical stress for dislocation glide or twinning by considering the intrinsic factors, such as stacking fault energy, crystallographic orientation, and grain size. The new finding of deformation induced microtwins and stacking faults in aluminum single crystal and the proposed model should be of interest to a broad community.

  1. Characterization and antibacterial activity of silver exchanged regenerated NaY zeolite from surfactant-modified NaY zeolite.

    PubMed

    Salim, Mashitah Mad; Malek, Nik Ahmad Nizam Nik

    2016-02-01

    The antibacterial activity of regenerated NaY zeolite (thermal treatment from cetyltrimethyl ammonium bromide (CTAB)-modified NaY zeolite and pretreatment with Na ions) loaded with silver ions were examined using the broth dilution minimum inhibitory concentration (MIC) method against Escherichia coli (E. coli ATCC 11229) and Staphylococcus aureus (S. aureus ATCC 6538). X-ray diffraction (XRD), attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy, field emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX) and chemical elemental analyses were used to characterize the regenerated NaY and AgY zeolites. The XRD patterns indicated that the calcination and addition of silver ions on regenerated NaY zeolite did not affect the structure of the regenerated NaY zeolite as the characteristic peaks of the NaY zeolite were retained, and no new peaks were observed. The regenerated AgY zeolite showed good antibacterial activity against both bacteria strains in distilled water, and the antibacterial activity of the samples increased with increasing Ag loaded on the regenerated AgY zeolite; the regenerated AgY zeolite was more effective against E. coli than S. aureus. However, the antibacterial activity of the regenerated AgY was not effective in saline solution for both bacteria. The study showed that CTAB-modified NaY zeolite materials could be regenerated to NaY zeolite using thermal treatment (550°C, 5h) and this material has excellent performance as an antibacterial agent after silver ions loading. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Preparation, Processing, and Characterization of Oriented Polycrystalline Zeolite and Aluminophosphate Membranes

    NASA Astrophysics Data System (ADS)

    Stoeger, Jared Andrew

    Since the advent of zeolite membranes, speculation on their industrial applicability has been closely monitored, although widespread commercialization has been hampered by limitations in fabrication and post-synthesis processing. Economical, energy-efficient technology breakthroughs require an evaluation of a range of material candidates which show robustness and reliability. Straightforward manufacturing techniques should be devised to generate thousands of square meters of membrane area; however, this demands control of structural characteristics on the scale of nanometers. As described in this dissertation, the path forward will be forged by exploiting the intrinsic crystalline properties of zeolites or aluminophosphates for the next advancement in membrane technology. A facile method is described for the preparation of silicalite-1 (MFI zeolite type) membranes using the secondary growth technique on symmetric porous stainless steel tubes. Activation through rapid thermal processing (RTP), a lamp-based heat-treatment process used as a critical fabrication step in silicon integrated circuit manufacturing, is proven to reduce the density of non-zeolitic transport pathways which are detrimental to high-resolution molecular sieving. RTP-treated membranes are shown to have enhanced performance in the binary separation of vapor-phase isomers (p-/o-xylene), gas-phase isomers (n-/i-butane), and alcohol/water when compared to membranes activated at a much slower heating rate but otherwise similarly-prepared. The performance is discussed in the context of the market potential for industrially-attractive separations: the recovery of p-xylene from an isomeric mixture or alcohol biofuels from aqueous post-fermentation streams. Hydrothermal growth techniques for the preparation and characterization of continuous aluminophosphate (AFI zeolite type) membranes with a preferential crystallographic alignment on porous alpha-Al2O3 disc supports are demonstrated. A mechanism is

  3. Photochemical charge separation in zeolites: Electron transfer dynamics, nanocrystals and zeolitic membranes. Final technical report

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

    Dutta, Prabir K.

    2001-09-30

    Aluminosilicate zeolites provide an excellent host for photochemical charge separation. Because of the constraints provided by the zeolite, the back electron transfer from the reduced acceptor to the oxidized sensitizer is slowed down. This provides the opportunity to separate the charge and use it in a subsequent reaction for water oxidation and reduction. Zeolite-based ruthenium oxide catalysts have been found to be efficient for the water splitting process. This project has demonstrated the usefulness of zeolite hosts for photolytic splitting of water.

  4. Properties of pure single crystals of actinide compounds

    NASA Astrophysics Data System (ADS)

    Vogt, O.

    1989-07-01

    Actinide research started with substances of poor quality and a multitude of "unexplainable" results mostly found on powder samples of doubtful quality exerted some pressure on the crystal growers. As an example we may mention the measurements on UP. Type I antiferromagnetism was found below 123 K by neutron diffraction experiments on powdered samples. At 23 K another transition becomes apparent in susceptibility measurements. The change of the magnetic moments associated with this transition remained unexplained. It was only after the discovery of multi k structures in other actinide compounds that the need was seen to perform even inelastic neutron diffraction experiments on single crystals so that finally the true nature of the transition in UP could be revealed. NpAs is another illustrative example for the fact that sometimes it takes decades to get a clear understanding for things even so simple as macroscopic magnetic properties. The main reason for the need of single crystals is certainly the anisotropy of the magnetic moment encountered in all actinide compounds. Self-heating effects may prevent research on big crystals or might call for isotopic purity of certain samples.

  5. Synthesis, growth, crystal structure, optical and third order nonlinear optical properties of quinolinium derivative single crystal: PNQI

    NASA Astrophysics Data System (ADS)

    Karthigha, S.; Krishnamoorthi, C.

    2018-03-01

    An organic quinolinium derivative nonlinear optical (NLO) crystal, 1-ethyl-2-[2-(4-nitro-phenyl)-vinyl]-quinolinium iodide (PNQI) was synthesized and successfully grown by slow evaporation solution growth technique. Formation of a crystalline compound was confirmed by single crystal X-ray diffraction. The quinolinium compound PNQI crystallizes in the triclinic crystal system with a centrosymmetric space group of P-1 symmetry. The molecular structure of PNQI was confirmed by 1H NMR and 13C NMR spectral studies. The thermal properties of the crystal have been investigated by thermogravimetric (TG) and differential scanning calorimetry (DSC) studies. The optical characteristics obtained from UV-Vis-NIR spectral data were described and the cut-off wavelength observed at 506 nm. The etching study was performed to analyse the growth features of PNQI single crystal. The third order NLO properties such as nonlinear refractive index (n2), nonlinear absorption coefficient (β) and nonlinear susceptibility (χ (3)) of the crystal were investigated using Z-scan technique at 632.8 nm of Hesbnd Ne laser.

  6. 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

  7. Synthesis and structural characterization of bulk Sb2Te3 single crystal

    NASA Astrophysics Data System (ADS)

    Sultana, Rabia; Gahtori, Bhasker; Meena, R. S.; Awana, V. P. S.

    2018-05-01

    We report the growth and characterization of bulk Sb2Te3 single crystal synthesized by the self flux method via solid state reaction route from high temperature melt (850˚C) and slow cooling (2˚C/hour) of constituent elements. The single crystal X-ray diffraction pattern showed the 00l alignment and the high crystalline nature of the resultant sample. The rietveld fitted room temperature powder XRD revealed the phase purity and rhombohedral structure of the synthesized crystal. The formation and analysis of unit cell structure further verified the rhombohedral structure composed of three quintuple layers stacked one over the other. The SEM image showed the layered directional growth of the synthesized crystal carried out using the ZEISS-EVOMA-10 scanning electron microscope The electrical resistivity measurement was carried out using the conventional four-probe method on a quantum design Physical Property Measurement System (PPMS). The temperature dependent electrical resistivity plot for studied Sb2Te3 single crystal depicts metallic behaviour in the absence of any applied magnetic field. The synthesis as well as the structural characterization of as grown Sb2Te3 single crystal is reported and discussed in the present letter.

  8. Arc-melting preparation of single crystal LaB.sub.6 cathodes

    DOEpatents

    Gibson, Edwin D.; Verhoeven, John D.

    1977-06-21

    A method for preparing single crystals of lanthanum hexaboride (LaB.sub.6) by arc melting a rod of compacted LaB.sub.6 powder. The method is especially suitable for preparing single crystal LaB.sub.6 cathodes for use in scanning electron microscopes (SEM) and scanning transmission electron microscopes (STEM).

  9. A STUDY OF DISLOCATION STRUCTURE OF SUBBOUNDARIES IN MOLYBDENUM SINGLE CRYSTALS,

    DTIC Science & Technology

    MOLYBDENUM, *DISLOCATIONS), GRAIN STRUCTURES(METALLURGY), SINGLE CRYSTALS, ZONE MELTING, ELECTRON BEAM MELTING, GRAIN BOUNDARIES, MATHEMATICAL ANALYSIS, ETCHED CRYSTALS, ETCHING, ELECTROEROSIVE MACHINING, CHINA

  10. Atomistic simulations of CO2 and N2 within cage-type silica zeolites.

    PubMed

    Madison, Lindsey; Heitzer, Henry; Russell, Colin; Kohen, Daniela

    2011-03-01

    The behavior of CO(2) and N(2), both as single components and as binary mixtures, in two cage-type silica zeolites was studied using atomistic simulations. The zeolites considered, ITQ-3 and paradigm cage-type zeolite ZK4 (the all-silica analog of LTA), were chosen so that the principles illustrated can be generalized to other adsorbent/adsorbate systems with similar topology and types of interactions. N(2) was chosen both because of the potential uses of N(2)/CO(2) separations and because it differs from CO(2) most significantly in the magnitude of its Coulombic interactions with zeolites. Despite similarities between N(2) and CO(2) diffusion in other materials, we show here that the diffusion of CO(2) within cage-type zeolites is dominated by an energy barrier to diffusion located at the entrance to the narrow channels connecting larger cages. This barrier originates in Coulombic interactions between zeolites and CO(2)'s quadrupole and results in well-defined orientations for the diffusing molecules. Furthermore, CO(2)'s favorable electrostatic interactions with the zeolite framework result in preferential binding in the windows between cages. N(2)'s behavior, in contrast, is more consistent with that of molecules previously studied. Our analysis suggests that CO(2)'s behavior might be common for adsorbates with quadrupoles that interact strongly with a material that has narrow windows between cages.

  11. Effective simultaneous removal of Pb(II) and Cd(II) ions by a new magnetic zeolite prepared from stem sweep

    NASA Astrophysics Data System (ADS)

    Safinejad, A.; Goudarzi, N.; Arab Chamjangali, M.; Bagherian, G.

    2017-11-01

    In this work, we prepared a new magnetic zeolite (MZ), as a sorbent, from stem sweep and used for the removal of lead and cadmium ions from aqueous solutions. Then the effective parameters involved in the removal efficiency of the studied ions were investigated. The synthetic MZ was characterized using x-ray diffraction (XRD) and field emission-scanning electron microscopy (FE-SEM). The best conditions for the preparation of MZ were found to be as follow: %Fe3O4 loaded  =  25, Si/Al  =  1.5, Na2O/SiO2  =  2.0, H2O/Na2O  =  75.0, crystallization time  =  20.0 h, and crystallization temperature  =  110 °C. The magnetic adsorbent was obtained by coating the zeolite with iron oxide nanoparticles. To study the sorption performance of the synthetic adsorbent, the single and binary systems including Pb(II) and Cd(II) ions were used. The effects of various parameters such as the solution pH, initial metal ion concentrations, amount of adsorbent, and contact time on the removal efficiency of the metal ions were studied. The results obtained showed that the adsorption isotherm data fitted well to the Langmuir isotherm, and that the adsorption kinetics of the metal ions in a binary system followed a pseudo-second order kinetic model.

  12. Characterization of Zeolite in Zeolite-Geopolymer Hybrid Bulk Materials Derived from Kaolinitic Clays

    PubMed Central

    Takeda, Hayami; Hashimoto, Shinobu; Yokoyama, Hiroaki; Honda, Sawao; Iwamoto, Yuji

    2013-01-01

    Zeolite-geopolymer hybrid materials have been formed when kaolin was used as a starting material. Their characteristics are of interest because they can have a wide pore size distribution with micro- and meso-pores due to the zeolite and geopolymer, respectively. In this study, Zeolite-geopolymer hybrid bulk materials were fabricated using four kinds of kaolinitic clays (a halloysite and three kinds of kaolinite). The kaolinitic clays were first calcined at 700 °C for 3 h to transform into the amorphous aluminosilicate phases. Alkali-activation treatment of the metakaolin yielded bulk materials with different amounts and types of zeolite and different compressive strength. This study investigated the effects of the initial kaolinitic clays on the amount and types of zeolite in the resultant geopolymers as well as the strength of the bulk materials. The kaolinitic clays and their metakaolin were characterized by XRD analysis, chemical composition, crystallite size, 29Si and 27Al MAS NMR analysis, and specific surface area measurements. The correlation between the amount of zeolite formed and the compressive strength of the resultant hybrid bulk materials, previously reported by other researchers was not positively observed. In the studied systems, the effects of Si/Al and crystalline size were observed. When the atomic ratio of Si/Al in the starting kaolinitic clays increased, the compressive strength of the hybrid bulk materials increased. The crystallite size of the zeolite in the hybrid bulk materials increased with decreasing compressive strength of the hybrid bulk materials. PMID:28809241

  13. Properties and applications of zeolites.

    PubMed

    Rhodes, Christopher J

    2010-01-01

    Zeolites are aluminosilicate solids bearing a negatively charged honeycomb framework of micropores into which molecules may be adsorbed for environmental decontamination, and to catalyse chemical reactions. They are central to green-chemistry since the necessity for organic solvents is minimised. Proton-exchanged (H) zeolites are extensively employed in the petrochemical industry for cracking crude oil fractions into fuels and chemical feedstocks for other industrial processes. Due to their ability to perform cation-exchange, in which the cations that are originally present to counterbalance the framework negative charge may be exchanged out of the zeolite by cations present in aqueous solution, zeolites are useful as industrial water-softeners, in the removal of radioactive Cs+ and Sr2+ cations from liquid nuclear waste and in the removal of toxic heavy metal cations from groundwaters and run-off waters. Surfactant-modified zeolites (SMZ) find particular application in the co-removal of both toxic anions and organic pollutants. Toxic anions such as arsenite, arsenate, chromate, cyanide and radioactive iodide can also be removed by adsorption into zeolites that have been previously loaded with co-precipitating metal cations such as Ag+ and Pb2+ which form practically insoluble complexes that are contained within the zeolite matrix.

  14. Exploring the folding pattern of a polymer chain in a single crystal by combining single-molecule force spectroscopy and steered molecular dynamics simulations.

    PubMed

    Song, Yu; Feng, Wei; Liu, Kai; Yang, Peng; Zhang, Wenke; Zhang, Xi

    2013-03-26

    Understanding the folding pattern of a single polymer chain within its single crystal will shed light on the mechanism of crystallization. Here, we use the combined techniques of atomic force microscopy (AFM)-based single-molecule force spectroscopy (SMFS) and steered molecular dynamics (SMD) simulations to study the folding pattern of a polyethylene oxide (PEO) chain in its single crystal. Our results show that the folding pattern of a PEO chain in the crystal formed in dilute solution follows the adjacent re-entry folding model. While in the crystal obtained from the melt, the nonadjacent folding with large and irregular loops contributes to big force fluctuations in the force-extension curves. The method established here can offer a novel strategy to directly unravel the chain-folding pattern of polymer single crystals at single-molecule level.

  15. Crystal-field analysis of U3+ ions in K2LaX5 (X=Cl, Br or I) single crystals

    NASA Astrophysics Data System (ADS)

    Karbowiak, M.; Edelstein, N.; Gajek, Z.; Drożdżyński, J.

    1998-11-01

    An analysis of low temperature absorption spectra of U3+ ions doped in K2LaX5 (X=Cl, Br or I) single crystals is reported. The energy levels of the U3+ ion in the single crystals were assigned and fitted to a semiempirical Hamiltonian representing the combined atomic and crystal-field interactions at the Cs symmetry site. An analysis of the nephelauxetic effect and crystal-field splittings in the series of compounds is also reported.

  16. Constitutive Modeling of Superalloy Single Crystals and Directionally Solidified Materials

    NASA Technical Reports Server (NTRS)

    Walker, K. P.; Jordan, E. H.

    1985-01-01

    A unified viscoplastic constitutive relation based on crystallographic slip theory was developed for the deformation analysis of nickel base face centered cubic superalloy single crystals at elevated temperature. The single crystal theory is embedded in a self consistent method to derive a constitutive relation for a directionally solidified material comprised of a polycrystalline aggregate of columnar cylindrical grains. One of the crystallographic axes of the cylindrical crystals points in the columnar direction while the remaining crystallographic axes are oriented at random in the basal plane perpendicular to the columnar direction. These constitutive formulations are coded in FORTRAN for use in nonlinear finite element and boundary element programs.

  17. The influence of zeolites fly ash bead/TiO2 composite material surface morphologies on their adsorption and photocatalytic performance

    NASA Astrophysics Data System (ADS)

    Yang, Lu; Wang, Fazhou; Hakki, Amer; Macphee, Donald E.; Liu, Peng; Hu, Shuguang

    2017-01-01

    A low cost zeolite fly ash bead/TiO2 (ZFABT) composite materials with various surface structure features were prepared for describing those structures importance on TiO2 coating, adsorbability and photocatalytic performances. The results indicated that fly ash bead (FAB) surface was significantly altered by the precipitation/growth of secondary zeolite phases after alkali activation, which generates abundant open pores and stacked petal-liked spherical beads (∼2 μm, Sodalite zeolites). More importantly, this porosity increases as activation time was increased from 2 h to 12 h, through the precipitation of sodalite and then Na-P1 (lamellar crystals) and Na-X (octahedral crystals) zeolite structures. Compared to those of unsupported TiO2 or inactivated support/TiO2 samples, all of ZFABT samples exhibited a higher adsorption capacity and photocatalytic efficiency for RhB removal. However, adsorption is not only one factor to influence TiO2 surface reaction, the intraparticle diffusion rate of rhodamine B (RhB) molecules, and light penetration are also important parameters. Alkali activated 4 h ZFABT sample exhibited the highest photocatalytic activity, indicating its pore structure provided a better balance for those parameters to achieve a synergistic adsorption/photocatalytic process. The kinetics model suggested its high intraparticle diffusion rate allowed for more RhB molecules to easily reach the reaction surface, which is more important for high efficiency photocatalysis.

  18. Single-crystal diamond nanomechanical resonators with quality factors exceeding one million

    NASA Astrophysics Data System (ADS)

    Tao, Y.; Boss, J. M.; Moores, B. A.; Degen, C. L.

    2014-04-01

    Diamond has gained a reputation as a uniquely versatile material, yet one that is intricate to grow and process. Resonating nanostructures made of single-crystal diamond are expected to possess excellent mechanical properties, including high-quality factors and low dissipation. Here we demonstrate batch fabrication and mechanical measurements of single-crystal diamond cantilevers with thickness down to 85 nm, thickness uniformity better than 20 nm and lateral dimensions up to 240 μm. Quality factors exceeding one million are found at room temperature, surpassing those of state-of-the-art single-crystal silicon cantilevers of similar dimensions by roughly an order of magnitude. The corresponding thermal force noise for the best cantilevers is ~5·10-19 N Hz-1/2 at millikelvin temperatures. Single-crystal diamond could thus directly improve existing force and mass sensors by a simple substitution of resonator material. Presented methods are easily adapted for fabrication of nanoelectromechanical systems, optomechanical resonators or nanophotonic devices that may lead to new applications in classical and quantum science.

  19. Electron paramagnetic resonance study of radiation-induced paramagnetic centers in succinic anhydride single crystal

    NASA Astrophysics Data System (ADS)

    Caliskan, Betul; Caliskan, Ali Cengiz; Er, Emine

    2017-09-01

    Succinic anhydride single crystals were exposed to 60Co-gamma irradiation at room temperature. The irradiated single crystals were investigated at 125 K by Electron Paramagnetic Resonance (EPR) Spectroscopy. The investigation of EPR spectra of irradiated single crystals of succinic anhydride showed the presence of two succinic anhydride anion radicals. The anion radicals observed in gamma-irradiated succinic anhydride single crystal were created by the scission of the carbon-oxygen double bond. The structure of EPR spectra demonstrated that the hyperfine splittings arise from the same radical species. The reduction of succinic anhydride was identified which is formed by the addition of an electron to oxygen of the Csbnd O bond. The g values, the hyperfine structure constants and direction cosines of the radiation damage centers observed in succinic anhydride single crystal were obtained.

  20. Method for single crystal growth of photovoltaic perovskite material and devices

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

    Huang, Jinsong; Dong, Qingfeng

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

  1. Single-crystal charge transfer interfaces for efficient photonic devices (Conference Presentation)

    NASA Astrophysics Data System (ADS)

    Alves, Helena; Pinto, Rui M.; Maçôas, Ermelinda M. S.; Baleizão, Carlos; Santos, Isabel C.

    2016-09-01

    Organic semiconductors have unique optical, mechanical and electronic properties that can be combined with customized chemical functionality. In the crystalline form, determinant features for electronic applications such as molecular purity, the charge mobility or the exciton diffusion length, reveal a superior performance when compared with materials in a more disordered form. Combining crystals of two different conjugated materials as even enable a new 2D electronic system. However, the use of organic single crystals in devices is still limited to a few applications, such as field-effect transistors. In 2013, we presented the first system composed of single-crystal charge transfer interfaces presenting photoconductivity behaviour. The system composed of rubrene and TCNQ has a responsivity reaching 1 A/W, corresponding to an external quantum efficiency of nearly 100%. A similar approach, with a hybrid structure of a PCBM film and rubrene single crystal also presents high responsivity and the possibility to extract excitons generated in acceptor materials. This strategy led to an extended action towards the near IR. By adequate material design and structural organisation of perylediimides, we demonstrate that is possible to improve exciton diffusion efficiency. More recently, we have successfully used the concept of charge transfer interfaces in phototransistors. These results open the possibility of using organic single-crystal interfaces in photonic applications.

  2. Subsurface Stress Fields in FCC Single Crystal Anisotropic Contacts

    NASA Technical Reports Server (NTRS)

    Arakere, Nagaraj K.; Knudsen, Erik; Swanson, Gregory R.; Duke, Gregory; Ham-Battista, Gilda

    2004-01-01

    Single crystal superalloy turbine blades used in high pressure turbomachinery are subject to conditions of high temperature, triaxial steady and alternating stresses, fretting stresses in the blade attachment and damper contact locations, and exposure to high-pressure hydrogen. The blades are also subjected to extreme variations in temperature during start-up and shutdown transients. The most prevalent high cycle fatigue (HCF) failure modes observed in these blades during operation include crystallographic crack initiation/propagation on octahedral planes, and non-crystallographic initiation with crystallographic growth. Numerous cases of crack initiation and crack propagation at the blade leading edge tip, blade attachment regions, and damper contact locations have been documented. Understanding crack initiation/propagation under mixed-mode loading conditions is critical for establishing a systematic procedure for evaluating HCF life of single crystal turbine blades. This paper presents analytical and numerical techniques for evaluating two and three dimensional subsurface stress fields in anisotropic contacts. The subsurface stress results are required for evaluating contact fatigue life at damper contacts and dovetail attachment regions in single crystal nickel-base superalloy turbine blades. An analytical procedure is presented for evaluating the subsurface stresses in the elastic half-space, based on the adaptation of a stress function method outlined by Lekhnitskii. Numerical results are presented for cylindrical and spherical anisotropic contacts, using finite element analysis (FEA). Effects of crystal orientation on stress response and fatigue life are examined. Obtaining accurate subsurface stress results for anisotropic single crystal contact problems require extremely refined three-dimensional (3-D) finite element grids, especially in the edge of contact region. Obtaining resolved shear stresses (RSS) on the principal slip planes also involves

  3. A finite-strain homogenization model for viscoplastic porous single crystals: II - Applications

    NASA Astrophysics Data System (ADS)

    Song, Dawei; Ponte Castañeda, P.

    2017-10-01

    In part I of this work (Song and Ponte Castañeda, 2017a), a new homogenization-based constitutive model was developed for the finite-strain, macroscopic response of porous viscoplastic single crystals. In this second part, the new model is first used to investigate the instantaneous response and the evolution of the microstructure for porous FCC single crystals for a wide range of loading conditions. The loading orientation, Lode angle and stress triaxiality are found to have significant effects on the evolution of porosity and average void shape, which play crucial roles in determining the overall hardening/softening behavior of porous single crystals. The predictions of the model are found to be in fairly good agreement with numerical simulations available from the literature for all loadings considered, especially for low triaxiality conditions. The model is then used to investigate the strong effect of crystal anisotropy on the instantaneous response and the evolution of the microstructure for porous HCP single crystals. For uniaxial tension and compression, the overall hardening/softening behavior of porous HCP crystals is found to be controlled mostly by the evolution of void shape, and not so much by the evolution of porosity. In particular, porous HCP crystals exhibit overall hardening behavior with increasing porosity, while they exhibit overall softening behavior with decreasing porosity. This interesting behavior is consistent with corresponding results for porous FCC crystals, but is found to be more significant for porous HCP crystals with large anisotropy, such as porous ice, where the non-basal slip systems are much harder than the basal systems.

  4. Single-Crystal Germanium Core Optoelectronic Fibers

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

    Ji, Xiaoyu; Page, Ryan L.; Chaudhuri, Subhasis

    Synthesis and fabrication of high-quality, small-core single-crystal germanium fibers that are photosensitive at the near-infrared and have low optical losses ≈1 dB cm-1 at 2 μm are reported. These fibers have potential applications in fiber-based spectroscopic imaging, nonlinear optical devices, and photodetection at the telecommunication wavelengths.

  5. Advances in theory and their application within the field of zeolite chemistry.

    PubMed

    Van Speybroeck, Veronique; Hemelsoet, Karen; Joos, Lennart; Waroquier, Michel; Bell, Robert G; Catlow, C Richard A

    2015-10-21

    Zeolites are versatile and fascinating materials which are vital for a wide range of industries, due to their unique structural and chemical properties, which are the basis of applications in gas separation, ion exchange and catalysis. Given their economic impact, there is a powerful incentive for smart design of new materials with enhanced functionalities to obtain the best material for a given application. Over the last decades, theoretical modeling has matured to a level that model guided design has become within reach. Major hurdles have been overcome to reach this point and almost all contemporary methods in computational materials chemistry are actively used in the field of modeling zeolite chemistry and applications. Integration of complementary modeling approaches is necessary to obtain reliable predictions and rationalizations from theory. A close synergy between experimentalists and theoreticians has led to a deep understanding of the complexity of the system at hand, but also allowed the identification of shortcomings in current theoretical approaches. Inspired by the importance of zeolite characterization which can now be performed at the single atom and single molecule level from experiment, computational spectroscopy has grown in importance in the last decade. In this review most of the currently available modeling tools are introduced and illustrated on the most challenging problems in zeolite science. Directions for future model developments will be given.

  6. Relaxor-based ferroelectric single crystals: growth, domain engineering, characterization and applications

    PubMed Central

    Sun, Enwei; Cao, Wenwu

    2014-01-01

    In the past decade, domain engineered relaxor-PT ferroelectric single crystals, including (1-x)Pb(Mg1/3Nb2/3)O3-xPbTiO3 (PMN-PT), (1-x)Pb(Zn1/3Nb2/3)O3-xPbTiO3 (PZN-PT) and (1-x-y)Pb(In1/2Nb1/2)O3-yPb(Mg1/3Nb2/3)O3-xPbTiO3 (PIN-PMN-PT), with compositions near the morphotropic phase boundary (MPB) have triggered a revolution in electromechanical devices owing to their giant piezoelectric properties and ultra-high electromechanical coupling factors. Compared to traditional PbZr1-xTixO3 (PZT) ceramics, the piezoelectric coefficient d33 is increased by a factor of 5 and the electromechanical coupling factor k33 is increased from < 70% to > 90%. Many emerging rich physical phenomena, such as charged domain walls, multi-phase coexistence, domain pattern symmetries, etc., have posed challenging fundamental questions for scientists. The superior electromechanical properties of these domain engineered single crystals have prompted the design of a new generation electromechanical devices, including sensors, transducers, actuators and other electromechanical devices, with greatly improved performance. It took less than 7 years from the discovery of larger size PMN-PT single crystals to the commercial production of the high-end ultrasonic imaging probe “PureWave”. The speed of development is unprecedented, and the research collaboration between academia and industrial engineers on this topic is truly intriguing. It is also exciting to see that these relaxor-PT single crystals are being used to replace traditional PZT piezoceramics in many new fields outside of medical imaging. The new ternary PIN-PMN-PT single crystals, particularly the ones with Mn-doping, have laid a solid foundation for innovations in high power acoustic projectors and ultrasonic motors, hinting another revolution in underwater SONARs and miniature actuation devices. This article intends to provide a comprehensive review on the development of relaxor-PT single crystals, spanning material discovery

  7. Relaxor-based ferroelectric single crystals: growth, domain engineering, characterization and applications.

    PubMed

    Sun, Enwei; Cao, Wenwu

    2014-08-01

    In the past decade, domain engineered relaxor-PT ferroelectric single crystals, including (1- x )Pb(Mg 1/3 Nb 2/3 )O 3 - x PbTiO 3 (PMN-PT), (1- x )Pb(Zn 1/3 Nb 2/3 )O 3 - x PbTiO 3 (PZN-PT) and (1- x - y )Pb(In 1/2 Nb 1/2 )O 3 - y Pb(Mg 1/3 Nb 2/3 )O 3 - x PbTiO 3 (PIN-PMN-PT), with compositions near the morphotropic phase boundary (MPB) have triggered a revolution in electromechanical devices owing to their giant piezoelectric properties and ultra-high electromechanical coupling factors. Compared to traditional PbZr 1- x Ti x O 3 (PZT) ceramics, the piezoelectric coefficient d 33 is increased by a factor of 5 and the electromechanical coupling factor k 33 is increased from < 70% to > 90%. Many emerging rich physical phenomena, such as charged domain walls, multi-phase coexistence, domain pattern symmetries, etc., have posed challenging fundamental questions for scientists. The superior electromechanical properties of these domain engineered single crystals have prompted the design of a new generation electromechanical devices, including sensors, transducers, actuators and other electromechanical devices, with greatly improved performance. It took less than 7 years from the discovery of larger size PMN-PT single crystals to the commercial production of the high-end ultrasonic imaging probe "PureWave". The speed of development is unprecedented, and the research collaboration between academia and industrial engineers on this topic is truly intriguing. It is also exciting to see that these relaxor-PT single crystals are being used to replace traditional PZT piezoceramics in many new fields outside of medical imaging. The new ternary PIN-PMN-PT single crystals, particularly the ones with Mn-doping, have laid a solid foundation for innovations in high power acoustic projectors and ultrasonic motors, hinting another revolution in underwater SONARs and miniature actuation devices. This article intends to provide a comprehensive review on the development of relaxor

  8. Study on the temperature field of large-sized sapphire single crystal furnace

    NASA Astrophysics Data System (ADS)

    Zhai, J. P.; Jiang, J. W.; Liu, K. G.; Peng, X. B.; Jian, D. L.; Li, I. L.

    2018-01-01

    In this paper, the temperature field of large-sized (120kg, 200kg and 300kg grade) sapphire single crystal furnace was simulated. By keeping the crucible diameter ratio and the insulation system unchanged, the power consumption, axial and radial temperature gradient, solid-liquid surface shape, stress distribution and melt flow were studied. The simulation results showed that with the increase of the single crystal furnace size, the power consumption increased, the temperature field insulation effect became worse, the growth stress value increased and the stress concentration phenomenon occurred. To solve these problems, the middle and bottom insulation system should be enhanced during designing the large-sized sapphire single crystal furnace. The appropriate radial and axial temperature gradient was favorable to reduce the crystal stress and prevent the occurrence of cracking. Expanding the interface between the seed and crystal was propitious to avoid the stress accumulation phenomenon.

  9. ITQ-54: a multi-dimensional extra-large pore zeolite with 20 × 14 × 12-ring channels

    DOE PAGES

    Jiang, Jiuxing; Yun, Yifeng; Zou, Xiaodong; ...

    2015-01-01

    A multi-dimensional extra-large pore silicogermanate zeolite, named ITQ-54, has been synthesised by in situ decomposition of the N,N-dicyclohexylisoindolinium cation into the N-cyclohexylisoindolinium cation. Its structure was solved by 3D rotation electron diffraction (RED) from crystals of ca. 1 μm in size. The structure of ITQ-54 contains straight intersecting 20 × 14 × 12-ring channels along the three crystallographic axes and it is one of the few zeolites with extra-large channels in more than one direction. ITQ-54 has a framework density of 11.1 T atoms per 1000 Å 3, which is one of the lowest among the known zeolites. ITQ-54 wasmore » obtained together with GeO 2 as an impurity. A heavy liquid separation method was developed and successfully applied to remove this impurity from the zeolite. ITQ-54 is stable up to 600 °C and exhibits permanent porosity. The structure was further refined using powder X-ray diffraction (PXRD) data for both as-made and calcined samples.« less

  10. Ignition and growth modeling of detonation reaction zone experiments on single crystals of PETN and HMX

    NASA Astrophysics Data System (ADS)

    White, Bradley W.; Tarver, Craig M.

    2017-01-01

    It has long been known that detonating single crystals of solid explosives have much larger failure diameters than those of heterogeneous charges of the same explosive pressed or cast to 98 - 99% theoretical maximum density (TMD). In 1957, Holland et al. demonstrated that PETN single crystals have failure diameters of about 8 mm, whereas heterogeneous PETN charges have failure diameters of less than 0.5 mm. Recently, Fedorov et al. quantitatively determined nanosecond time resolved detonation reaction zone profiles of single crystals of PETN and HMX by measuring the interface particle velocity histories of the detonating crystals and LiF windows using a PDV system. The measured reaction zone time durations for PETN and HMX single crystal detonations were approximately 100 and 260 nanoseconds, respectively. These experiments provided the necessary data to develop Ignition and Growth (I&G) reactive flow model parameters for the single crystal detonation reaction zones. Using these parameters, the calculated unconfined failure diameter of a PETN single crystal was 7.5 +/- 0.5 mm, close to the 8 mm experimental value. The calculated failure diameter of an unconfined HMX single crystal was 15 +/- 1 mm. The unconfined failure diameter of an HMX single crystal has not yet been determined precisely, but Fedorov et al. detonated 14 mm diameter crystals confined by detonating a HMX-based plastic bonded explosive (PBX) without initially overdriving the HMX crystals.

  11. Crystal growth and electrical properties of CuFeO 2 single crystals

    NASA Astrophysics Data System (ADS)

    Dordor, P.; Chaminade, J. P.; Wichainchai, A.; Marquestaut, E.; Doumerc, J. P.; Pouchard, M.; Hagenmuller, P.; Ammar, A.

    1988-07-01

    Delafossite-type CuFeO 2 single crystals have been prepared by a flux method: crystals obtained in a Cu crucible with LiBO 2 as flux are n-type whereas those prepared in a Pt crucible with a Cu 2O flux are p-type. Electrical measurements have revealed that n-type crystals exhibit weak anisotropic conductivities with large activation energies and small mobilities (r.t. values perpendicular and parallel to the c-axis: μ⊥ = 5 × 10 -5 and μ‖ = 10 -7 cm -2 V -1 sec -1). p-type crystals, less anisotropic, are characterized by low activation energies and higher mobilities ( μ⊥ = 34 and μ‖ = 8.9 cm 2 V -1 sec -1). A two -conduction-band model is proposed to account for the difference observed between the energy gap value deduced from photoelectrochemical measurements and the activation energy of the electrical conductivity in the intrinsic domain.

  12. Single crystal to polycrystal neutron transmission simulation

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

    Dessieux, Luc Lucius; Stoica, Alexandru Dan; Bingham, Philip R.

    A collection of routines for calculation of the total cross section that determines the attenuation of neutrons by crystalline solids is presented. The total cross section is calculated semi-empirically as a function of crystal structure, neutron energy, temperature, and crystal orientation. The semi-empirical formula includes the contribution of parasitic Bragg scattering to the total cross section using both the crystal’s mosaic spread value and its orientation with respect to the neutron beam direction as parameters. These routines allow users to enter a distribution of crystal orientations for calculation of total cross sections of user defined powder or pseudo powder distributions,more » which enables simulation of non-uniformities such as texture and strain. In conclusion, the spectra for neutron transmission simulations in the neutron thermal energy range (2 meV–100 meV) are presented for single crystal and polycrystal samples and compared to measurements.« less

  13. Single crystal to polycrystal neutron transmission simulation

    DOE PAGES

    Dessieux, Luc Lucius; Stoica, Alexandru Dan; Bingham, Philip R.

    2018-02-02

    A collection of routines for calculation of the total cross section that determines the attenuation of neutrons by crystalline solids is presented. The total cross section is calculated semi-empirically as a function of crystal structure, neutron energy, temperature, and crystal orientation. The semi-empirical formula includes the contribution of parasitic Bragg scattering to the total cross section using both the crystal’s mosaic spread value and its orientation with respect to the neutron beam direction as parameters. These routines allow users to enter a distribution of crystal orientations for calculation of total cross sections of user defined powder or pseudo powder distributions,more » which enables simulation of non-uniformities such as texture and strain. In conclusion, the spectra for neutron transmission simulations in the neutron thermal energy range (2 meV–100 meV) are presented for single crystal and polycrystal samples and compared to measurements.« less

  14. Optical properties of Sulfur doped InP single crystals

    NASA Astrophysics Data System (ADS)

    El-Nahass, M. M.; Youssef, S. B.; Ali, H. A. M.

    2014-05-01

    Optical properties of InP:S single crystals were investigated using spectrophotometric measurements in the spectral range of 200-2500 nm. The absorption coefficient and refractive index were calculated. It was found that InP:S crystals exhibit allowed and forbidden direct transitions with energy gaps of 1.578 and 1.528 eV, respectively. Analysis of the refractive index in the normal dispersion region was discussed in terms of the single oscillator model. Some optical dispersion parameters namely: the dispersion energy (Ed), single oscillator energy (Eo), high frequency dielectric constant (ɛ∞), and lattice dielectric constant (ɛL) were determined. The volume and the surface energy loss functions (VELF & SELF) were estimated. Also, the real and imaginary parts of the complex conductivity were calculated.

  15. Oxygen and hydrogen isotope geochemistry of zeolites

    NASA Technical Reports Server (NTRS)

    Karlsson, Haraldur R.; Clayton, Robert N.

    1990-01-01

    Oxygen and hydrogen isotope ratios for natural samples of the zeolites analcime, chabazite, clinoptilolite, laumontite, mordenite, and natrolite have been obtained. The zeolite samples were classified into sedimentary, hydrothermal, and igneous groups. The ratios for each species of zeolite are reported. The results are used to discuss the origin of channel water, the role of zeolites in water-rock interaction, and the possibility that a calibrated zeolite could be used as a low-temperature geothermometer.

  16. EPR study of free radical in gamma-irradiated bis(cyclopentadienyl)zirconium dichloride single crystal

    NASA Astrophysics Data System (ADS)

    Caliskan, Betul; Caliskan, Ali Cengiz

    2017-06-01

    Bis(cyclopentadienyl)zirconium dichloride (BCZD; zirconocene dichloride) single crystals were exposed to 60Co-γ irradiation at room temperature. The irradiated single crystals were investigated between 125 and 470 K by electron paramagnetic resonance spectroscopy. The spectra of the crystals were found to be temperature independent. The paramagnetic center was attributed to the cyclopentadienyl radical. The g values of the radiation damage center observed in BCZD single crystal and the hyperfine structure constants of the free electron with nearby protons were obtained.

  17. Zeolites: Exploring Molecular Channels

    ScienceCinema

    Arslan, Ilke; Derewinski, Mirek

    2018-05-16

    Synthetic zeolites contain microscopic channels, sort of like a sponge. They have many uses, such as helping laundry detergent lather, absorbing liquid in kitty litter, and as catalysts to produce fuel. Of the hundreds of types of zeolites, only about 15 are used for catalysis. PNNL catalysis scientists Ilke Arslan and Mirek Derewinksi are studying these zeolites to understand what make them special. By exploring the mystery of these microscopic channels, their fundamental findings will help design better catalysts for applications such as biofuel production.

  18. Zeolites: Exploring Molecular Channels

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

    Arslan, Ilke; Derewinski, Mirek

    2015-05-22

    Synthetic zeolites contain microscopic channels, sort of like a sponge. They have many uses, such as helping laundry detergent lather, absorbing liquid in kitty litter, and as catalysts to produce fuel. Of the hundreds of types of zeolites, only about 15 are used for catalysis. PNNL catalysis scientists Ilke Arslan and Mirek Derewinksi are studying these zeolites to understand what make them special. By exploring the mystery of these microscopic channels, their fundamental findings will help design better catalysts for applications such as biofuel production.

  19. Cryogenic motion performances of a piezoelectric single crystal micromotor

    NASA Astrophysics Data System (ADS)

    Li, Xiaotian; Wu, Yuting; Chen, Zhijiang; Wei, Xiaoyong; Luo, Haosu; Dong, Shuxiang

    2014-04-01

    This study investigates the cryogenic performances of a millimeter-size piezoelectric ultrasonic linear micromotor. The piezoelectric vibrator of the micromotor is made of Pb(In1/2Nb1/2)O3 -Pb(Mg1/3Nb2/3)-PbTiO3 single crystal and operated in first-bending wobbling mode. Experiments show that the piezoelectric single crystal micromotor works effectively even at extremely low temperature of -175 °C, although its resonance peaks vary with temperature significantly. This work confirms the feasibility of cryogenic operation of the piezo-micromotor, which is meaningful for aerospace or superconducting microwave application.

  20. A finite-strain homogenization model for viscoplastic porous single crystals: I - Theory

    NASA Astrophysics Data System (ADS)

    Song, Dawei; Ponte Castañeda, P.

    2017-10-01

    This paper presents a homogenization-based constitutive model for the finite-strain, macroscopic response of porous viscoplastic single crystals. The model accounts explicitly for the evolution of the average lattice orientation, as well as the porosity, average shape and orientation of the voids (and their distribution), by means of appropriate microstructural variables playing the role of internal variables and serving to characterize the evolution of both the "crystallographic" and "morphological" anisotropy of the porous single crystals. The model makes use of the fully optimized second-order variational method of Ponte Castañeda (2015), together with the iterated homogenization approach of Agoras and Ponte Castañeda (2013), to characterize the instantaneous effective response of the porous single crystals with fixed values of the microstructural variables. Consistent homogenization estimates for the average strain rate and vorticity fields in the phases are then used to derive evolution equations for the associated microstructural variables. The model is 100% predictive, requiring no fitting parameters, and applies for porous viscoplastic single crystals with general crystal anisotropy and average void shape and orientation, which are subjected to general loading conditions. In Part II of this work (Song and Ponte Castañeda, 2017a), results for both the instantaneous response and the evolution of the microstructure will be presented for porous FCC and HCP single crystals under a wide range of loading conditions, and good agreement with available FEM results will be shown.

  1. A novel ultra-broadband single polarization single mode photonic crystal fiber

    NASA Astrophysics Data System (ADS)

    Jiang, Linghong; Zheng, Yi; Hou, Lantian; Zheng, Kai; Peng, Jiying; Zhao, Xingtao

    2017-08-01

    The concept of employing a central hole infiltrated with nematic liquid crystal (NLC) and two additional air holes in the core region is exploited to obtain an ultra-broadband single polarization single mode photonic crystal fiber (SPSM-PCF). The effects of structural parameters on the SPSM operation are studied using the full-vectorial finite element method. Numerical results show that the proposed structure can attain the SPSM operation bandwidth of 1610 nm (from 1.51 to 3.12 μm) with confinement loss lower than 0.01 dB/km. The SPSM operation range can also be widely tuned to shorter wavelengths by adjusting the structure parameters. And meanwhile, a broad dispersion-flattened SPSM PCF is also obtained around the communication wavelength. Moreover, the dual-core SPSM PCF has also been investigated, enabling potential applications in the wavelength splitter of 1.31 and 1.55 μm bands at a short fiber length of 1.629 mm with SPSM operation.

  2. Oxidative regeneration of toluene-saturated natural zeolite by gaseous ozone: the influence of zeolite chemical surface characteristics.

    PubMed

    Alejandro, Serguei; Valdés, Héctor; Manéro, Marie-Hélène; Zaror, Claudio A

    2014-06-15

    In this study, the effect of zeolite chemical surface characteristics on the oxidative regeneration of toluene saturated-zeolite samples is investigated. A Chilean natural zeolite (53% clinoptilolite, 40% mordenite and 7% quartz) was chemically modified by acid treatment with hydrochloric acid and by ion-exchange with ammonium sulphate. Thermal pre-treatments at 623 and 823K were applied and six zeolite samples with different chemical surface characteristics were generated. Chemical modification of natural zeolite followed by thermal out-gassing allows distinguishing the role of acidic surface sites on the regeneration of exhausted zeolites. An increase in Brønsted acid sites on zeolite surface is observed as a result of ammonium-exchange treatment followed by thermal treatment at 623K, thus increasing the adsorption capacity toward toluene. High ozone consumption could be associated to a high content of Lewis acid sites, since these could decompose ozone into atomic active oxygen species. Then, surface oxidation reactions could take part among adsorbed toluene at Brønsted acid sites and surface atomic oxygen species, reducing the amount of adsorbed toluene after the regenerative oxidation with ozone. Experimental results show that the presence of adsorbed oxidation by-products has a negative impact on the recovery of zeolite adsorption capacity. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. 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

  4. Anisotropic constitutive modeling for nickel-base single crystal superalloys. Ph.D. Thesis

    NASA Technical Reports Server (NTRS)

    Sheh, Michael Y.

    1988-01-01

    An anisotropic constitutive model was developed based on crystallographic slip theory for nickel base single crystal superalloys. The constitutive equations developed utilizes drag stress and back stress state variables to model the local inelastic flow. Specially designed experiments were conducted to evaluate the existence of back stress in single crystal superalloy Rene N4 at 982 C. The results suggest that: (1) the back stress is orientation dependent; and (2) the back stress state variable is required for the current model to predict material anelastic recovery behavior. The model was evaluated for its predictive capability on single crystal material behavior including orientation dependent stress-strain response, tension/compression asymmetry, strain rate sensitivity, anelastic recovery behavior, cyclic hardening and softening, stress relaxation, creep and associated crystal lattice rotation. Limitation and future development needs are discussed.

  5. Energetics of sodium-calcium exchanged zeolite A.

    PubMed

    Sun, H; Wu, D; Guo, X; Shen, B; Navrotsky, A

    2015-05-07

    A series of calcium-exchanged zeolite A samples with different degrees of exchange were prepared. They were characterized by powder X-ray diffraction (XRD) and differential scanning calorimetry (DSC). High temperature oxide melt drop solution calorimetry measured the formation enthalpies of hydrated zeolites CaNa-A from constituent oxides. The water content is a linear function of the degree of exchange, ranging from 20.54% for Na-A to 23.77% for 97.9% CaNa-A. The enthalpies of formation (from oxides) at 25 °C are -74.50 ± 1.21 kJ mol(-1) TO2 for hydrated zeolite Na-A and -30.79 ± 1.64 kJ mol(-1) TO2 for hydrated zeolite 97.9% CaNa-A. Dehydration enthalpies obtained from differential scanning calorimetry are 32.0 kJ mol(-1) H2O for hydrated zeolite Na-A and 20.5 kJ mol(-1) H2O for hydrated zeolite 97.9% CaNa-A. Enthalpies of formation of Ca-exchanged zeolites A are less exothermic than for zeolite Na-A. A linear relationship between the formation enthalpy and the extent of calcium substitution was observed. The energetic effect of Ca-exchange on zeolite A is discussed with an emphasis on the complex interactions between the zeolite framework, cations, and water.

  6. NaA zeolite derived from blast furnace slag: its application for ammonium removal.

    PubMed

    Guo, Hongwei; Tang, Lizhen; Yan, Bingji; Wan, Kang; Li, Peng

    2017-09-01

    In this paper, high value added NaA zeolite material was prepared from blast furnace (BF) slag by hydrothermal method and its adsorption behavior on the removal of ammonium ion was investigated. It was found out that the synthetic NaA cubic zeolite with smaller crystal size obtained at nSiO 2 /nAl 2 O 3 = 2 and nH 2 O/nNaOH = 20 showed better adsorption performance. The kinetics of the adsorption of ammonium ion by synthesized NaA zeolite was fitted by the pseudo-second-order kinetic model. The intra-particle diffusion modeling reveals that two mixed rate-controlling mechanisms were involved in the adsorption process. The relatively high value of activation energy of 92.3 kJ·mol -1 indicates a high impact of temperature on the adsorption rate, and the nature of ammonium adsorption is chemical reaction rather than physisorption. Based on the thermodynamics calculations, the adsorption of ammonium was found to be an endothermic, spontaneous process. The adsorption isothermal analysis showed that the Langmuir model could be well fitted and a maximum adsorption capacity of 83.3 mg·g -1 of NH 4 + was obtained. Thus, it was demonstrated that by forming low cost NaA zeolite and using it for environmental remediation, the synchronous minimization of BF slag and ammonia nitrogen contamination could be achieved.

  7. Process for Forming a High Temperature Single Crystal Canted Spring

    NASA Technical Reports Server (NTRS)

    DeMange, Jeffrey J (Inventor); Ritzert, Frank J (Inventor); Nathal, Michael V (Inventor); Dunlap, Patrick H (Inventor); Steinetz, Bruce M (Inventor)

    2017-01-01

    A process for forming a high temperature single crystal canted spring is provided. In one embodiment, the process includes fabricating configurations of a rapid prototype spring to fabricate a sacrificial mold pattern to create a ceramic mold and casting a canted coiled spring to form at least one canted coil spring configuration based on the ceramic mold. The high temperature single crystal canted spring is formed from a nickel-based alloy containing rhenium using the at least one coil spring configuration.

  8. Elastic response of (001)-oriented PWA 1480 single crystal - The influence of secondary orientation

    NASA Technical Reports Server (NTRS)

    Kalluri, Sreeramesh; Abdul-Azis, Ali; Mcgaw, Michael

    1991-01-01

    The influence of secondary orientation on the elastic response of a zone axis (001)-oriented nickel-base single-crystal superalloy, PWA 1480, was investigated under mechanical loading conditions by applying finite element techniques. Elastic stress analyses were performed with a commercially available finite element code. Secondary orientation of the single-crystal superalloy was offset with respect to the global coordinate system in increments from 0 to 90 deg and stresses developed within the single crystal were determined for each loading condition. The results indicated that the stresses were strongly influenced by the angular offset between the secondary crystal orientation and the global coordinate system. The degree of influence was found to vary with the type of loading condition (mechanical, thermal, or combined) imposed on the single-crystal superalloy.

  9. 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.

  10. Single Crystal Synthesis and STM Studies of High Temperature Superconductors

    NASA Technical Reports Server (NTRS)

    Barrientos, Alfonso

    1997-01-01

    This is a final report for the work initiated in September of 1994 under the grant NAG8-1085 - NASA/OMU, on the fabrication of bulk and single crystal synthesis, specific heat measuring and STM studies of high temperature superconductors. Efforts were made to fabricate bulk and single crystals of mercury based superconducting material. A systematic thermal analysis on the precursors for the corresponding oxides and carbonates were carried out to synthesized bulk samples. Bulk material was used as seed in an attempt to grow single crystals by a two-step self flux process. On the other hand bulk samples were characterized by x-ray diffraction, electrical resistivity and magnetic susceptibility, We studied the specific heat behavior in the range from 80 to 300 K. Some preliminary attempts were made to study the atomic morphology of our samples. As part of our efforts we built an ac susceptibility apparatus for measuring the transition temperature of our sintered samples.

  11. Enhanced selectivity of zeolites by controlled carbon deposition

    DOEpatents

    Nenoff, Tina M.; Thoma, Steven G.; Kartin, Mutlu

    2006-05-09

    A method for carbonizing a zeolite comprises depositing a carbon coating on the zeolite pores by flowing an inert carrier gas stream containing isoprene through a regenerated zeolite at elevated temperature. The carbonized zeolite is useful for the separation of light hydrocarbon mixtures due to size exclusion and the differential adsorption properties of the carbonized zeolite.

  12. 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

  13. Ultrathin solution-processed single crystals of thiophene-phenylene co-oligomers for organic field-effect devices

    NASA Astrophysics Data System (ADS)

    Glushkova, Anastasia V.; Poimanova, Elena Yu.; Bruevich, Vladimir V.; Luponosov, Yuriy N.; Ponomarenko, Sergei A.; Paraschuk, Dmitry Yu.

    2017-08-01

    Thiophene-phenylene co-oligomers (TPCO) single crystals are promising materials for organic light-emitting devices, e.g., light-emitting transistors (OLETs), due to their ability to combine high luminescence and efficient charge transport. However, optical confinement in platy single crystals strongly decreases light emission from their top surface degrading the device performance. To avoid optical waveguiding, single crystals thinner than 100 nm would be beneficial. Herein, we report on solution-processed ultrathin single crystals of TPCO and study their charge transport properties. As materials we used 1,4-bis(5'-hexyl-2,2'-bithiophene-5-yl)benzene (DH-TTPTT) and 1,4-bis(5'-decyl-2,2'-bithiophene-5-yl)benzene (DD-TTPTT). The ultrathin single crystals were studied by optical polarization, atomic-force, and transmission electron microscopies, and as active layers in organic field effect transistors (OFET). The OFET hole mobility was increased tenfold for the oligomer with longer alkyl substituents (DD-TTPTT) reaching 0.2 cm2/Vs. Our studies of crystal growth indicate that if the substrate is wetted, it has no significant effect on the crystal growth. We conclude that solution-processed ultrathin TPCO single crystals are a promising platform for organic optoelectronic field-effect devices.

  14. Advances in Large Grain/Single Crystal SC Resonators at DESY

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

    W. Singer; A. Brinkmann; A. Ermakov

    The main aim of the DESY large grain R&D program is to check whether this option is reasonable to apply for fabrication of ca. 1'000 XFEL cavities. Two aspects are being pursued. On one hand the basic material investigation, on the other hand the material availability, fabrication and preparation procedure. Several single cell large grain cavities of TESLA shape have been fabricated and tested. The best accelerating gradients of 41 MV/m was measured on electropolished cavity. First large grain nine-cell cavities worldwide have been produced under contract of DESY with ACCEL Instruments Co. All three cavities fulfil the XFEL specificationmore » already in first RF test after only BCP (Buffered Chemical Polishing) treatment and 800 degrees C annealing. Accelerating gradient of 27 - 29 MV/m was reached. A fabrication method of single crystal cavity of ILC like shape was proposed. A single cell single crystal cavity was build at the company ACCEL. Accelerating gradient of 37.5 MV/m reached after only 112 microns BCP and in situ baking 120 degrees C for 6 hrs with the quality factor higher as 2x1010. The developed method can be extended on fabrication of multi cell single crystal cavities.« less

  15. Ultra-precision process of CaF2 single crystal

    NASA Astrophysics Data System (ADS)

    Yin, Guoju; Li, Shengyi; Xie, Xuhui; Zhou, Lin

    2014-08-01

    This paper proposes a new chemical mechanical polishing (CMP) process method for CaF2 single crystal to get ultraprecision surface. The CMP processes are improving polishing pad and using alkaline SiO2 polishing slurry with PH=8, PH=11 two phases to polish, respectively, and the roughness can be 0.181nm Rq (10μm×10μm). The CMP process can't get high surface figure, so we use ion beam figuring (IBF) technology to obtain high surface figure. However, IBF is difficult to improve the CaF2 surface roughness. We optimize IBF process to improve surface figure and keep good surface roughness too. Different IBF incident ion energy from 400ev to 800ev does not affect on the surface roughness obviously but the depth of material removal is reverse. CaF2 single crystal can get high precision surface figure (RMS=2.251nm) and still keep ultra-smooth surface (Rq=0.207nm) by IBF when removal depth is less than 200nm. The researches above provide important information for CaF2 single crystal to realize ultra-precision manufacture.

  16. Microgravity

    NASA Image and Video Library

    1992-06-25

    Zeolites are crystalline aluminosilicates that have complex framework structures. However, there are several features of zeolite crystals that make unequivocal structure determinations difficult. The acquisition of reliable structural information on zeolites is greatly facilitated by the availability of high-quality specimens. For structure determinations by conventional diffraction techniques, large single-crystal specimens are essential. Alternatively, structural determinations by powder profile refinement methods relax the constraints on crystal size, but still require materials with a high degree of crystalline perfection. Studies conducted at CAMMP (Center for Advanced Microgravity Materials Processing) have demonstrated that microgravity processing can produce larger crystal sizes and fewer structural defects relative to terrestrial crystal growth. Principal Investigator: Dr. Albert Sacco

  17. Nanofluidics of Single-Crystal Diamond Nanomechanical Resonators.

    PubMed

    Kara, V; Sohn, Y-I; Atikian, H; Yakhot, V; Lončar, M; Ekinci, K L

    2015-12-09

    Single-crystal diamond nanomechanical resonators are being developed for countless applications. A number of these applications require that the resonator be operated in a fluid, that is, a gas or a liquid. Here, we investigate the fluid dynamics of single-crystal diamond nanomechanical resonators in the form of nanocantilevers. First, we measure the pressure-dependent dissipation of diamond nanocantilevers with different linear dimensions and frequencies in three gases, He, N2, and Ar. We observe that a subtle interplay between the length scale and the frequency governs the scaling of the fluidic dissipation. Second, we obtain a comparison of the surface accommodation of different gases on the diamond surface by analyzing the dissipation in the molecular flow regime. Finally, we measure the thermal fluctuations of the nanocantilevers in water and compare the observed dissipation and frequency shifts with theoretical predictions. These findings set the stage for developing diamond nanomechanical resonators operable in fluids.

  18. Dielectric and domain studies on Fe doped KNbO3 single crystal

    NASA Astrophysics Data System (ADS)

    Shamkuwar, Sanjaykumar H.; Patil, Naresh M.; Korde, Vivek B.; Pradnyakar, Namrata V.

    2018-05-01

    Synthesis of Fe doped KNbO3 single crystals by flux method is reported here. The effect of Fe-doping on phase transition temperatures of KNbO3 single crystals was investigated using dielectric studies. The phase transition temperatures were found to be 225°C and 425°C which almost same as reported by others. The domain studies were carried out using metallurgical microscope and it shows the presence of 60° and 90° domains in the grown crystals.

  19. Apparatus And Method For Producing Single Crystal Metallic Objects

    DOEpatents

    Huang, Shyh-Chin; Gigliotti, Jr., Michael Francis X.; Rutkowski, Stephen Francis; Petterson, Roger John; Svec, Paul Steven

    2006-03-14

    A mold is provided for enabling casting of single crystal metallic articles including a part-defining cavity, a sorter passage positioned vertically beneath and in fluid communication with the part-defining cavity, and a seed cavity positioned vertically beneath and in fluid communication with the sorter passage. The sorter passage includes a shape suitable for encouraging a single crystal structure in solidifying molten metal. Additionally, a portion of the mold between the sorter passage and the part-defining cavity includes a notch for facilitating breakage of a cast article proximate the notch during thermal stress build-up, so as to prevent mold breakage or the inclusion of part defects.

  20. Growth and studies of cyclohexylammonium 4-methoxy benzoate single crystal for nonlinear optical applications

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

    Sathya, P.; Gopalakrishnan, R., E-mail: krgkrishnan@annauniv.edu

    2015-06-24

    Cyclohexylammonium 4-Methoxy Benzoate (C4MB) was synthesised and the functional groups were confirmed by FTIR analysis. The purified C4MB (by repeated recrystallisation) was used for single crystal growth. Single crystal of cyclohexylammonium 4-methoxy benzoate was successfully grown by slow evaporation solution growth method at ambient temperature. Structural orientations were determined from single crystal X-ray diffractometer. Optical absorption and cut off wavelength were identified by UV-Visible spectroscopy. Thermal stability of the crystal was studied from thermogravimetric and differential thermal analyses curves. Mechanical stability of the grown crystal was analysed by Vicker’s microhardness tester. The Second Harmonic Generation (SHG) study revealed that themore » C4MB compound exhibits the SHG efficiency 3.3 times greater than KDP crystal.« less

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

    DOE PAGES

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

    2017-04-07

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

  2. Self-reporting inhibitors: single crystallization process to get two optically pure enantiomers.

    PubMed

    Wan, Xinhua; Ye, Xichong; Cui, Jiaxi; Li, Bowen; Li, Na; Zhang, Jie

    2018-05-22

    Collection of two optically pure enantiomers in a single crystallization process can significantly increase the chiral separation efficiency but it's hard to realize nowadays. Herein we describe, for the first time, a self-reporting strategy for visualizing the crystallization process by a kind of dyed self-assembled inhibitors made from the copolymers with tri(ethylene glycol)-grafting polymethylsiloxane as main chains and poly(N6-methacryloyl-L-lysine) as side chains. When applied with seeds together for the fractional crystallization of conglomerates, the inhibitors can label the formation of the secondary crystals and guide us to completely separate the crystallization process of two enantiomers with colorless crystals as the first product and red crystals as the secondary product. This method leads to high optical purity of D/L-Asn·H2O (99.9 ee% for D-crystals and 99.5 ee% for L-crystals) in a single crystallization process. Moreover, it requires low feeding amount of additives and shows excellent recyclability. We foresee its great potential in developing novel chiral separation methods that can be used in different scales. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. The effect of pressure on open-framework silicates: elastic behaviour and crystal-fluid interaction

    NASA Astrophysics Data System (ADS)

    Gatta, G. D.; Lotti, P.; Tabacchi, G.

    2018-02-01

    The elastic behaviour and the structural evolution of microporous materials compressed hydrostatically in a pressure-transmitting fluid are drastically affected by the potential crystal-fluid interaction, with a penetration of new molecules through the zeolitic cavities in response to applied pressure. In this manuscript, the principal mechanisms that govern the P-behaviour of zeolites with and without crystal-fluid interaction are described, on the basis of previous experimental findings and computational modelling studies. When no crystal-fluid interaction occurs, the effects of pressure are mainly accommodated by tilting of (quasi-rigid) tetrahedra around O atoms that behave as hinges. Tilting of tetrahedra is the dominant mechanism at low-mid P-regime, whereas distortion and compression of tetrahedra represent the mechanisms which usually dominate the mid-high P regime. One of the most common deformation mechanisms in zeolitic framework is the increase of channels ellipticity. The deformation mechanisms are dictated by the topological configuration of the tetrahedral framework; however, the compressibility of the cavities is controlled by the nature and bonding configuration of the ionic and molecular content, resulting in different unit-cell volume compressibility in isotypic structures. The experimental results pertaining to compression in "penetrating" fluids, and thus with crystal-fluid interaction, showed that not all the zeolites experience a P-induced intrusion of new monoatomic species or molecules from the P-transmitting fluids. For example, zeolites with well-stuffed channels at room conditions (e.g. natural zeolites) tend to hinder the penetration of new species through the zeolitic cavities. Several variables govern the sorption phenomena at high pressure, among those: the "free diameters" of the framework cavities, the chemical nature and the configuration of the extra-framework population, the partial pressure of the penetrating molecule in the

  4. Desolvation-Driven 100-Fold Slow-down of Tunneling Relaxation Rate in Co(II)-Dy(III) Single-Molecule Magnets through a Single-Crystal-to-Single-Crystal Process

    NASA Astrophysics Data System (ADS)

    Liu, Jun-Liang; Wu, Jie-Yi; Huang, Guo-Zhang; Chen, Yan-Cong; Jia, Jian-Hua; Ungur, Liviu; Chibotaru, Liviu F.; Chen, Xiao-Ming; Tong, Ming-Liang

    2015-11-01

    Single-molecule magnets (SMMs) are regarded as a class of promising materials for spintronic and ultrahigh-density storage devices. Tuning the magnetic dynamics of single-molecule magnets is a crucial challenge for chemists. Lanthanide ions are not only highly magnetically anisotropic but also highly sensitive to the changes in the coordination environments. We developed a feasible approach to understand parts of the magneto-structure correlations and propose to regulate the relaxation behaviors via rational design. A series of Co(II)-Dy(III)-Co(II) complexes were obtained using in situ synthesis; in this system of complexes, the relaxation dynamics can be greatly improved, accompanied with desolvation, via single-crystal to single-crystal transformation. The effective energy barrier can be increased from 293 cm-1 (422 K) to 416 cm-1 (600 K), and the tunneling relaxation time can be grown from 8.5 × 10-4 s to 7.4 × 10-2 s. These remarkable improvements are due to the change in the coordination environments of Dy(III) and Co(II). Ab initio calculations were performed to better understand the magnetic dynamics.

  5. Fabrication of 6FDA-durene membrane incorporated with zeolite T and aminosilane grafted zeolite T for CO2/CH4 separation

    NASA Astrophysics Data System (ADS)

    Jusoh, Norwahyu; Fong Yeong, Yin; Keong Lau, Kok; Shariff, Azmi Mohd

    2017-08-01

    In the present work, zeolite T and aminosilane grafted zeolite T are embedded into 6FDA-durene polyimide phase for the fabrication of mixed matrix membranes (MMMs). FESEM images demonstrated that the improvement of interfacial adhesion between zeolite and polymer phases in MMM loaded with aminosilane grafted zeolite T was not significant as compared to zeolite T/6FDA-durene MMM. From the gas permeation test, CO2/CH4 selectivity up to 26.4 was achieved using MMM containing aminosilane grafted zeolite T, while MMM loaded with ungrafted zeolite T showed CO2/CH4 selectivity of 19.1. In addition, MMM incorporated with aminosilane grafted zeolite T particles successfully lies on Robeson upper bound 2008, which makes it an attractive candidate for CO2/CH4 separation.

  6. Comparison of different zeolite framework types as carriers for the oral delivery of the poorly soluble drug indomethacin.

    PubMed

    Karavasili, Christina; Amanatiadou, Elsa P; Kontogiannidou, Eleni; Eleftheriadis, Georgios K; Bouropoulos, Nikolaos; Pavlidou, Eleni; Kontopoulou, Ioanna; Vizirianakis, Ioannis S; Fatouros, Dimitrios G

    2017-08-07

    Microporous zeolites of distinct framework types, textural properties and crystal morphologies namely BEA, ZSM and NaX, have been employed as carriers to assess their effect on modulating the dissolution behavior of a BCS II model drug (indomethacin). Preparation of the loaded carriers via the incipient wetness method induced significant drug amorphization for the BEA and NaX samples, as well as high drug payloads. The stability of the amorphous drug content was retained after stressing test evaluation of the porous carriers. The dissolution profile of loaded indomethacin was evaluated in simulated gastric fluid (pH 1.2) and simulated intestinal fluids FaSSIF (fasted) and FeSSIF (fed state) conditions and was found to be dependent on the aluminosilicate ratio of the zeolites and the degree of crystalline drug content. The feasibility of the zeolitic particles as oral drug delivery systems was appraised with cytocompatibility and cellular toxicity studies in Caco-2 cultures in a time- and dose-dependent manner by means of the MTT assay and flow cytometry analysis, respectively. Intracellular accumulation of the zeolite particles was observed with no apparent cytotoxic effects at the lower concentrations tested, rendering such microporous zeolites pertinent candidates in oral drug delivery applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. 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.

  8. Surfactant modified zeolite as amphiphilic and dual-electronic adsorbent for removal of cationic and oxyanionic metal ions and organic compounds.

    PubMed

    Tran, Hai Nguyen; Viet, Pham Van; Chao, Huan-Ping

    2018-01-01

    A hydrophilic Y zeolite was primarily treated with sodium hydroxide to enhance its cation exchange capacity (Na-zeolite). The organo-zeolite (Na-H-zeolite) was prepared by a modification process of the external surface of Na-zeolite with a cationic surfactant (hexadecyltrimethylammonium; HDTMA). Three adsorbents (i.e., pristine zeolite, Na-zeolite, and Na-H-zeolite) were characterized with nitrogen adsorption/desorption isotherms, scanning electron microscopy coupled with energy dispersive X-ray spectroscopy, cation exchange capacities, and zeta potential. Results demonstrated that HDTMA can be adsorbed on the surface of Na-zeolite to form patchy bilayers. The adsorption capacity of several hazardous pollutants (i.e., Pb 2+ , Cu 2+ , Ni 2+ , Cr 2 O 7 2- , propylbenzene, ethylbenzene, toluene, benzene, and phenol) onto Na-H-zeolite was investigated in a single system and multiple-components. Adsorption isotherm was measured to further understand the effects of the modification process on the adsorption behaviors of Na-H-zeolite. Adsorption performances indicated that Na-H-zeolite can simultaneously adsorb the metal cations (on the surface not covered by HDTMA), oxyanions (on the surface covered by HDTMA). Na-H-zeolite also exhibited both hydrophilic and hydrophobic surfaces to uptake organic compounds with various water solubilities (from 55 to 75,000mg/L). It was experimentally concluded that Na-H-zeolite is a potential dual-electronic and amphiphilic adsorbent for efficiently removing a wide range of potentially toxic pollutants from aquatic environments. Copyright © 2017 Elsevier Inc. All rights reserved.

  9. Postsynthetic Improvement of the Physical Properties in a Metal-Organic Framework through a Single Crystal to Single Crystal Transmetallation.

    PubMed

    Grancha, Thais; Ferrando-Soria, Jesús; Zhou, Hong-Cai; Gascon, Jorge; Seoane, Beatriz; Pasán, Jorge; Fabelo, Oscar; Julve, Miguel; Pardo, Emilio

    2015-05-26

    A single crystal to single crystal transmetallation process takes place in the three-dimensional (3D) metal-organic framework (MOF) of formula Mg(II) 2 {Mg(II) 4 [Cu(II) 2 (Me3 mpba)2 ]3 }⋅45 H2 O (1; Me3 mpba(4-) =N,N'-2,4,6-trimethyl-1,3-phenylenebis(oxamate)). After complete replacement of the Mg(II) ions within the coordination network and those hosted in the channels by either Co(II) or Ni(II) ions, 1 is transmetallated to yield two novel MOFs of formulae Co2 (II) {Co(II) 4 [Cu(II) 2 (Me3 mpba)2 ]3 }⋅56 H2 O (2) and Ni2 (II) {Ni(II) 4 [Cu(II) 2 (Me3 mpba)2 ]3 }⋅ 54 H2 O (3). This unique postsynthetic metal substitution affords materials with higher structural stability leading to enhanced gas sorption and magnetic properties. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Optical and Electrical Properties of Sn-Doped Zinc Oxide Single Crystals

    DOE PAGES

    Haseman, M. S.; Saadatkia, Pooneh; Warfield, J. T.; ...

    2017-11-28

    Here, Sn dopant in ZnO may significantly improve the n-type conductivity of ZnO through a characteristic double effect. However, studies on bulk Sn-doped ZnO are rare, and the effect of Sn doping on the optoelectronic properties of bulk ZnO is not well understood. In this work, the effect of Sn doping on the optical and electrical properties of ZnO bulk single crystals was investigated through optical absorption spectroscopy, Hall-effect measurements, and thermoluminescence (TL) spectroscopy. Undoped and Sn-doped ZnO single crystals were grown by chemical vapor transport method and characterized by x-ray diffraction analysis. The Sn doping level in the crystalsmore » was evaluated by inductively coupled plasma mass spectroscopy measurements. Hall-effect measurements revealed an increase in conductivity and carrier concentration with increasing Sn doping, while TL measurements identified a few donor species in the crystals with donor ionization energy ranging from 35 meV to 118 meV. Increasing Sn doping was also associated with a color change of single crystals from colorless to dark blue.« less

  11. 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.

  12. High performance zeolite LTA pervaporation membranes on ceramic hollow fibers by dipcoating-wiping seed deposition.

    PubMed

    Wang, Zhengbao; Ge, Qinqin; Shao, Jia; Yan, Yushan

    2009-05-27

    We demonstrate for the first time that by one single hydrothermal synthesis a zeolite LTA membrane with a high flux of 9.0 kg/m(2) h and high water/ethanol separation factor of 10,000 could be formed on a ceramic hollow fiber that is known for its ability to form a compact module. The flux is the highest reported in the literatures. A novel seeding method, dipcoating-wiping, is key to obtaining zeolite membranes with high separation performance because it reproducibly produces a uniform and trace seed layer on the support. This new seeding method is expected to have serious implications for making defect-free zeolite films and membranes for many applications. The membranes reported here have the potential to solve the key problems that have prevented zeolite membranes from widespread use for biofuel production.

  13. Shock wave-induced phase transition in RDX single crystals.

    PubMed

    Patterson, James E; Dreger, Zbigniew A; Gupta, Yogendra M

    2007-09-20

    The real-time, molecular-level response of oriented single crystals of hexahydro-1,3,5-trinitro-s-triazine (RDX) to shock compression was examined using Raman spectroscopy. Single crystals of [111], [210], or [100] orientation were shocked under stepwise loading to peak stresses from 3.0 to 5.5 GPa. Two types of measurements were performed: (i) high-resolution Raman spectroscopy to probe the material at peak stress and (ii) time-resolved Raman spectroscopy to monitor the evolution of molecular changes as the shock wave reverberated through the material. The frequency shift of the CH stretching modes under shock loading appeared to be similar for all three crystal orientations below 3.5 GPa. Significant spectral changes were observed in crystals shocked above 4.5 GPa. These changes were similar to those observed in static pressure measurements, indicating the occurrence of the alpha-gamma phase transition in shocked RDX crystals. No apparent orientation dependence in the molecular response of RDX to shock compression up to 5.5 GPa was observed. The phase transition had an incubation time of approximately 100 ns when RDX was shocked to 5.5 GPa peak stress. The observation of the alpha-gamma phase transition under shock wave loading is briefly discussed in connection with the onset of chemical decomposition in shocked RDX.

  14. Precipitation of thin-film organic single crystals by a novel crystal growth method using electrospray and ionic liquid film

    NASA Astrophysics Data System (ADS)

    Ueda, Hiroyuki; Takeuchi, Keita; Kikuchi, Akihiko

    2018-04-01

    We report an organic single crystal growth technique, which uses a nonvolatile liquid thin film as a crystal growth field and supplies fine droplets containing solute from the surface of the liquid thin film uniformly and continuously by electrospray deposition. Here, we investigated the relationships between the solute concentration of the supplied solution and the morphology and size of precipitated crystals for four types of fluorescent organic low molecule material [tris(8-hydroxyquinoline)aluminum (Alq3), 2-(4-biphenylyl)-5-(4-tert-butylphenyl)-1,3,4-oxadiazole (PBD), N,N‧-bis(3-methylphenyl)-N,N‧-diphenylbenzidine (TPD), and N,N-bis(naphthalene-1-yl)-N,N-diphenyl-benzidine (NPB)] using an ionic liquid as the nonvolatile liquid. As the concentration of the supplied solution decreased, the morphology of precipitated crystals changed from dendritic or leaf shape to platelike one. At the solution concentration of 0.1 mg/ml, relatively large platelike single crystals with a diagonal length of over 100 µm were obtained for all types of material. In the experiment using ionic liquid and dioctyl sebacate as nonvolatile liquids, it was confirmed that there is a clear positive correlation between the maximum volume of the precipitated single crystal and the solubility of solute under the same solution supply conditions.

  15. Load relaxation of olivine single crystals

    NASA Astrophysics Data System (ADS)

    Cooper, Reid F.; Stone, Donald S.; Plookphol, Thawatchai

    2016-10-01

    Single crystals of ferromagnesian olivine (San Carlos, AZ, peridot; Fo88-90) have been deformed in both uniaxial creep and load relaxation under conditions of ambient pressure, T = 1500°C and pO2 = 10-10 atm; creep stresses were in the range 40 ≤ σ1 (MPa) ≤ 220. The crystals were oriented such that the applied stress was parallel to [011]c, which promotes single slip on the slowest slip system in olivine, (010)[001]. The creep rates at steady state match well the results of earlier investigators, as does the stress sensitivity (a power law exponent of n = 3.6). Dislocation microstructures, including spatial distribution of low-angle (subgrain) boundaries, additionally confirm previous investigations. Inverted primary creep (an accelerating strain rate with an increase in stress) was observed. Load relaxation, however, produced a singular response—a single hardness curve—regardless of the magnitude of creep stress or total accumulated strain preceding relaxation. The log stress versus log strain rate data from load-relaxation and creep experiments overlap to within experimental error. The load-relaxation behavior is distinctly different than that described for other crystalline solids, where the flow stress is affected strongly by work hardening such that a family of distinct hardness curves is generated, which are related by a scaling function. The response of olivine for the conditions studied, we argue, indicates flow that is rate limited by dislocation glide, reflecting specifically a high intrinsic lattice resistance (Peierls stress).

  16. Load Relaxation of Olivine Single Crystals

    NASA Astrophysics Data System (ADS)

    Cooper, R. F.; Stone, D. S.; Plookphol, T.

    2016-12-01

    Single crystals of ferromagnesian olivine (San Carlos, AZ, peridot; Fo90-92) have been deformed in both uniaxial creep and load relaxation under conditions of ambient pressure, T = 1500ºC and pO2 = 10-10 atm; creep stresses were in the range 40 ≤ σ1 (MPa) ≤ 220. The crystals were oriented such that the applied stress was parallel to [011]c, which promotes single slip on the slowest slip system in olivine, (010)[001]. The creep rates at steady state match well the results of earlier investigators, as does the stress sensitivity (a power-law exponent of n = 3.6). Dislocation microstructures, including spatial distribution of low-angle (subgrain) boundaries, additionally confirm previous investigations. Inverted primary creep (an accelerating strain rate with an increase in stress) was observed. Load-relaxation, however, produced a singular response—a single hardness curve—regardless of the magnitude of creep stress or total accumulated strain preceding relaxation. The log-stress v. log-strain rate data from load-relaxation and creep experiments overlap to within experimental error. The load-relaxation behavior is distinctly different that that described for other crystalline solids, where the flow stress is affected strongly by work hardening such that a family of distinct hardness curves is generated, which are related by a scaling function. The response of olivine for the conditions studied, thus, indicates flow that is rate-limited by dislocation glide, reflecting specifically a high intrinsic lattice resistance (Peierls stress).

  17. Single-crystal diffraction instrument TriCS at SINQ

    NASA Astrophysics Data System (ADS)

    Schefer, J.; Könnecke, M.; Murasik, A.; Czopnik, A.; Strässle, Th; Keller, P.; Schlumpf, N.

    2000-03-01

    The single-crystal diffractometer TriCS at the Swiss Continuous Spallation Source (SINQ) is presently in the commissioning phase. A two-dimensional wire detector produced by EMBL was delivered in March 1999. The instrument is presently tested with a single detector. First measurements on magnetic structures have been performed. The instrument is remotely controlled using JAVA-based software and a UNIX DEC-α host computer.

  18. Microwave Induced Direct Bonding of Single Crystal Silicon Wafers

    NASA Technical Reports Server (NTRS)

    Budraa, N. K.; Jackson, H. W.; Barmatz, M.

    1999-01-01

    We have heated polished doped single-crystal silicon wafers in a single mode microwave cavity to temperatures where surface to surface bonding occurred. The absorption of microwaves and heating of the wafers is attributed to the inclusion of n-type or p-type impurities into these substrates. A cylindrical cavity TM (sub 010) standing wave mode was used to irradiate samples of various geometry's at positions of high magnetic field. This process was conducted in vacuum to exclude plasma effects. This initial study suggests that the inclusion of impurities in single crystal silicon significantly improved its microwave absorption (loss factor) to a point where heating silicon wafers directly can be accomplished in minimal time. Bonding of these substrates, however, occurs only at points of intimate surface to surface contact. The inclusion of a thin metallic layer on the surfaces enhances the bonding process.

  19. Fabrication and evaluation of novel zeolite membranes to control the neoplastic activity and anti-tumoral drug treatments in human breast cancer cells. Part 1: Synthesis and characterization of Pure Zeolite Membranes and Mixed Matrix Membranes for adhesion and growth of cancer cells.

    PubMed

    Tavolaro, Palmira; Martino, Guglielmo; Andò, Sebastiano; Tavolaro, Adalgisa

    2016-12-01

    Novel pure and hybrid zeolite membranes were prepared with appropriate different physicochemical characteristics such as frameworks, hydrophilicity, crystal size, chemical composition, acid-base properties (Point of Zero Charge, PZC) and surface morphology and used in inorganic cell/scaffold constructs. Because the control of cell interactions, as the adhesion, proliferation, remodelling and mobility, is important for differentiation and progression of tumors, this work focused on response of cancer cells adhered and grown on synthesized zeolite surfaces in order to study the influence of these scaffolds in controlled conditions. We have selected the MCF-7 and MDA-MB-231 human breast cancer cell line as model tumor cell lines. This study showed that all the zeolite membranes synthesized are excellent scaffolds because they are very selective materials to support the adhesion and growth of neoplastic cells. All zeolite scaffolds were characterized by FESEM, FTIR ATR, XRD, AFM, PZC and contact angle analyses. Cell adhesion, viability and morphology were measured by count, MTT assay and FESEM microphotography analysis, at various incubation times. Copyright © 2016. Published by Elsevier B.V.

  20. Scanning electron microscope study of polytetrafluoroethylene sliding on aluminum single crystals

    NASA Technical Reports Server (NTRS)

    Brainard, W. A.; Buckley, D. H.

    1973-01-01

    Friction experiments were conducted in air with polytetrafluoroethylene (PTFE) sliding on aluminum single crystals. Mechanical scoring of the crystals with (110) and (100) orientations was observed with a single pass of the PTFE slider. No scoring was observed on the (111). The degree of scoring of the crystals is related to the hardness, with the hardest surface (111) showing no damage and the softest surface (110) showing the most severe scoring. Scoring is caused by work-hardened pieces of aluminum which, as a consequence of the adhesion between PTFE and aluminum, were pulled out of the bulk and became embedded in the PTFE polymer.

  1. Analysis of synthetic diamond single crystals by X-ray topography and double-crystal diffractometry

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

    Prokhorov, I. A., E-mail: igor.prokhorov@mail.ru; Ralchenko, V. G.; Bolshakov, A. P.

    2013-12-15

    Structural features of diamond single crystals synthesized under high pressure and homoepitaxial films grown by chemical vapor deposition (CVD) have been analyzed by double-crystal X-ray diffractometry and topography. The conditions of a diffraction analysis of diamond crystals using Ge monochromators have been optimized. The main structural defects (dislocations, stacking faults, growth striations, second-phase inclusions, etc.) formed during crystal growth have been revealed. The nitrogen concentration in high-pressure/high-temperature (HPHT) diamond substrates is estimated based on X-ray diffraction data. The formation of dislocation bundles at the film-substrate interface in the epitaxial structures has been revealed by plane-wave topography; these dislocations are likelymore » due to the relaxation of elastic macroscopic stresses caused by the lattice mismatch between the substrate and film. The critical thicknesses of plastic relaxation onset in CVD diamond films are calculated. The experimental techniques for studying the real diamond structure in optimizing crystal-growth technology are proven to be highly efficient.« less

  2. 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.

  3. Levitation effect in zeolites: Quasielastic neutron scattering and molecular dynamics study of pentane isomers in zeolite NaY.

    PubMed

    Borah, Bhaskar J; Jobic, H; Yashonath, S

    2010-04-14

    We report the quasielastic neutron scattering (QENS) and molecular dynamics (MD) investigations into diffusion of pentane isomers in zeolite NaY. The molecular cross section perpendicular to the long molecular axis varies for the three isomers while the mass and the isomer-zeolite interaction remains essentially unchanged. Both QENS and MD results show that the branched isomers neopentane and isopentane have higher self-diffusivities as compared with n-pentane at 300 K in NaY zeolite. This result provides direct experimental evidence for the existence of nonmonotonic, anomalous dependence of self-diffusivity on molecular diameter known as the levitation effect. The energetic barrier at the bottleneck derived from MD simulations exists for n-pentane which lies in the linear regime while no such barrier is seen for neopentane which is located clearly in the anomalous regime. Activation energy is in the order E(a)(n-pentane)>E(a)(isopentane)>E(a)(neopentane) consistent with the predictions of the levitation effect. In the liquid phase, it is seen that D(n-pentane)>D(isopentane)>D(neopentane) and E(a)(n-pentane)single exponential decay for neopentane and isopentane. For n-pentane, a single exponential fit provides a poor fit especially at short times. Cage residence time is largest for n-pentane and lowest for neopentane. For neopentane, the width of the self-part of the dynamic structure factor shows a near monotonic decrease with wavenumber. For n-pentane a minimum is seen near k=0.5 A(-1) suggesting a slowing down of motion around the 12-ring window, the bottleneck for diffusion. Finally, the result that the branched isomer has a higher diffusivity as compared with the linear analog is at variation from what is normally seen.

  4. Levitation effect in zeolites: Quasielastic neutron scattering and molecular dynamics study of pentane isomers in zeolite NaY

    NASA Astrophysics Data System (ADS)

    Borah, Bhaskar J.; Jobic, H.; Yashonath, S.

    2010-04-01

    We report the quasielastic neutron scattering (QENS) and molecular dynamics (MD) investigations into diffusion of pentane isomers in zeolite NaY. The molecular cross section perpendicular to the long molecular axis varies for the three isomers while the mass and the isomer-zeolite interaction remains essentially unchanged. Both QENS and MD results show that the branched isomers neopentane and isopentane have higher self-diffusivities as compared with n-pentane at 300 K in NaY zeolite. This result provides direct experimental evidence for the existence of nonmonotonic, anomalous dependence of self-diffusivity on molecular diameter known as the levitation effect. The energetic barrier at the bottleneck derived from MD simulations exists for n-pentane which lies in the linear regime while no such barrier is seen for neopentane which is located clearly in the anomalous regime. Activation energy is in the order Ea(n-pentane)>Ea(isopentane)>Ea(neopentane) consistent with the predictions of the levitation effect. In the liquid phase, it is seen that D(n-pentane)>D(isopentane)>D(neopentane) and Ea(n-pentane)single exponential decay for neopentane and isopentane. For n-pentane, a single exponential fit provides a poor fit especially at short times. Cage residence time is largest for n-pentane and lowest for neopentane. For neopentane, the width of the self-part of the dynamic structure factor shows a near monotonic decrease with wavenumber. For n-pentane a minimum is seen near k =0.5 Å-1 suggesting a slowing down of motion around the 12-ring window, the bottleneck for diffusion. Finally, the result that the branched isomer has a higher diffusivity as compared with the linear analog is at variation from what is normally seen.

  5. Flux growth of high-quality CoFe 2O 4 single crystals and their characterization

    NASA Astrophysics Data System (ADS)

    Wang, W. H.; Ren, X.

    2006-04-01

    We report the growth of high-quality CoFe 2O 4 single crystals using a borax flux method. The crystals were characterized by powder X-ray diffraction, electron probe microanalysis and Raman spectroscopy. We found the crystals are flux-free and highly homogeneous in composition. X-ray rocking curves of the CoFe 2O 4 single crystals showed a full-width at half-maximum of 0.15°. The saturation magnetization of the CoFe 2O 4 single crystals was measured to be 90 emu/g or equivalently 3.65 μ B/f.u. at 5 K.

  6. [What a physician should know about zeolites].

    PubMed

    Boranić, M

    2000-01-01

    Zeolites are natural and synthetic hydrated crystalline aluminosilicates endowed with absorptive and ion exchange properties. They have found numerous and multifarous applications--in industry as catalysts and absorbents, in water sanitation for the removal of ammonia and heavy metals, in agriculture as fertilizers, and in animal husbandry as the absorbents of excreted material and as food additives. Medical applications have included the use in filtration systems for anesthesia or dialysis and as the contrast materials in NMR imaging. Recently, zeolite powders for external use have found application as deodorants, antimycotic agents and wound dressings. Peroral use of encapsulated zeolite powders enriched with vitamins, oligoelements or other ingredients has been claimed to exert beneficial medical effects. Ingestion of zeolites may be considered analogous to the clay eating (geophagia), considered in traditional medicine as a remedy for various illnesses. Being amphoteric, zeolites are partly soluble in acid or alkaline media, but within the physiological pH range the solubility is generally low. Minimal amounts of free aluminium or silicium from the ingested zeolites are resorbed from the gut. The bulk of ingested zeolite probably remains undissolved in the gut. In view of the ion exchange properties, zeolites may be expected to change the ionic content, pH and buffering capacity of the gastrointestinal secretions and to affect the transport through the intestinal epithelium. In addition, zeolites could affect the bacterial flora and the resorption of bacterial products, vitamins and oligoelements. The contact of zeolite particles with gastrointestinal mucosa may elicit the secretion of cytokines with local and systemic actions. Reactive silicium ions might react with biomolecules of the intestinal epithelium, and if resorbed, do so in other cells. Mutagenic and carcinogenic effects of zeolite particles have been described, resembling such effects of asbestos

  7. Eutectic Formation During Solidification of Ni-Based Single-Crystal Superalloys with Additional Carbon

    NASA Astrophysics Data System (ADS)

    Wang, Fu; Ma, Dexin; Bührig-Polaczek, Andreas

    2017-11-01

    γ/ γ' eutectics' nucleation behavior during the solidification of a single-crystal superalloy with additional carbon was investigated by using directional solidification quenching method. The results show that the nucleation of the γ/ γ' eutectics can directly occur on the existing γ dendrites, directly in the remaining liquid, or on the primary MC-type carbides. The γ/γ' eutectics formed through the latter two mechanisms have different crystal orientations than that of the γ matrix. This suggests that the conventional Ni-based single-crystal superalloy castings with additional carbon only guarantee the monocrystallinity of the γ matrix and some γ/ γ' eutectics and, in addition to the carbides, there are other misoriented polycrystalline microstructures existing in macroscopically considered "single-crystal" superalloy castings.

  8. UTILITY OF ZEOLITES IN ARSENIC REMOVAL FROM WATER

    EPA Science Inventory

    Zeolites are well known for their ion exchange and adsorption properties. So far the cation exchanger properties of zeolites have been extensively studied and utilized. The anion exchanger properties of zeolites are less studied. Zeolite Faujasite Y has been used to remove arseni...

  9. Characterisation of irradiation-induced defects in ZnO single crystals

    NASA Astrophysics Data System (ADS)

    Prochazka, I.; Cizek, J.; Lukac, F.; Melikhova, O.; Valenta, J.; Havranek, V.; Anwand, W.; Skuratov, V. A.; Strukova, T. S.

    2016-01-01

    Positron annihilation spectroscopy (PAS) combined with optical methods was employed for characterisation of defects in the hydrothermally grown ZnO single crystals irradiated by 167 MeV Xe26+ ions to fluences ranged from 3×1012 to 1×1014 cm-2. The positron lifetime (LT), Doppler broadening as well as slow-positron implantation spectroscopy (SPIS) techniques were involved. The ab-initio theoretical calculations were utilised for interpretation of LT results. The optical transmission and photoluminescence measurements were conducted, too. The virgin ZnO crystal exhibited a single component LT spectrum with a lifetime of 182 ps which is attributed to saturated positron trapping in Zn vacancies associated with hydrogen atoms unintentionally introduced into the crystal during the crystal growth. The Xe ion irradiated ZnO crystals have shown an additional component with a longer lifetime of ≈ 360 ps which comes from irradiation-induced larger defects equivalent in size to clusters of ≈10 to 12 vacancies. The concentrations of these clusters were estimated on the basis of combined LT and SPIS data. The PAS data were correlated with irradiation induced changes seen in the optical spectroscopy experiments.

  10. Dynamic actuation of single-crystal diamond nanobeams

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

    Sohn, Young-Ik; Burek, Michael J.; Lončar, Marko, E-mail: loncar@seas.harvard.edu

    2015-12-14

    We show the dielectrophoretic actuation of single-crystal diamond nanomechanical devices. Gradient radio-frequency electromagnetic forces are used to achieve actuation of both cantilever and doubly clamped beam structures, with operation frequencies ranging from a few MHz to ∼50 MHz. Frequency tuning and parametric actuation are also studied.

  11. 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.

  12. Identification of Some Zeolite Group Minerals by Application of Artificial Neural Network and Decision Tree Algorithm Based on SEM-EDS Data

    NASA Astrophysics Data System (ADS)

    Akkaş, Efe; Evren Çubukçu, H.; Akin, Lutfiye; Erkut, Volkan; Yurdakul, Yasin; Karayigit, Ali Ihsan

    2016-04-01

    Identification of zeolite group minerals is complicated due to their similar chemical formulas and habits. Although the morphologies of various zeolite crystals can be recognized under Scanning Electron Microscope (SEM), it is relatively more challenging and problematic process to identify zeolites using their mineral chemical data. SEMs integrated with energy dispersive X-ray spectrometers (EDS) provide fast and reliable chemical data of minerals. However, considering elemental similarities of characteristic chemical formulae of zeolite species (e.g. Clinoptilolite ((Na,K,Ca)2 -3Al3(Al,Si)2Si13O3612H2O) and Erionite ((Na2,K2,Ca)2Al4Si14O36ṡ15H2O)) EDS data alone does not seem to be sufficient for correct identification. Furthermore, the physical properties of the specimen (e.g. roughness, electrical conductivity) and the applied analytical conditions (e.g. accelerating voltage, beam current, spot size) of the SEM-EDS should be uniform in order to obtain reliable elemental results of minerals having high alkali (Na, K) and H2O (approx. %14-18) contents. This study which was funded by The Scientific and Technological Research Council of Turkey (TUBITAK Project No: 113Y439), aims to construct a database as large as possible for various zeolite minerals and to develop a general prediction model for the identification of zeolite minerals using SEM-EDS data. For this purpose, an artificial neural network and rule based decision tree algorithm were employed. Throughout the analyses, a total of 1850 chemical data were collected from four distinct zeolite species, (Clinoptilolite-Heulandite, Erionite, Analcime and Mordenite) observed in various rocks (e.g. coals, pyroclastics). In order to obtain a representative training data set for each minerals, a selection procedure for reference mineral analyses was applied. During the selection procedure, SEM based crystal morphology data, XRD spectra and re-calculated cationic distribution, obtained by EDS have been used for the

  13. Total Synthesis of Eleutherobin and Analogs and Study of Anti-Cancer Mechanism

    DTIC Science & Technology

    2001-05-01

    storage of the samples in our prenmiscs for five months at into 25- 35 nmn large single crystals of zeolite Y. Further 78"C. crystallization of the...5, , " Sevcrl ib6kcular sieves, including zeolite A, Y, L, ZSM -5, d) R. E. Ireland, L. Liu, J. Org. Chem. 3993,58,2899; review of TPAP/ NMO oxidation

  14. Zeolite Nanoparticles for Selective Sorption of Plasma Proteins

    NASA Astrophysics Data System (ADS)

    Rahimi, M.; Ng, E.-P.; Bakhtiari, K.; Vinciguerra, M.; Ahmad, H. Ali; Awala, H.; Mintova, S.; Daghighi, M.; Bakhshandeh Rostami, F.; de Vries, M.; Motazacker, M. M.; Peppelenbosch, M. P.; Mahmoudi, M.; Rezaee, F.

    2015-11-01

    The affinity of zeolite nanoparticles (diameter of 8-12 nm) possessing high surface area and high pore volume towards human plasma proteins has been investigated. The protein composition (corona) of zeolite nanoparticles has been shown to be more dependent on the plasma protein concentrations and the type of zeolites than zeolite nanoparticles concentration. The number of proteins present in the corona of zeolite nanoparticles at 100% plasma (in vivo state) is less than with 10% plasma exposure. This could be due to a competition between the proteins to occupy the corona of the zeolite nanoparticles. Moreover, a high selective adsorption for apolipoprotein C-III (APOC-III) and fibrinogen on the zeolite nanoparticles at high plasma concentration (100%) was observed. While the zeolite nanoparticles exposed to low plasma concentration (10%) exhibited a high selective adsorption for immunoglobulin gamma (i.e. IGHG1, IGHG2 and IGHG4) proteins. The zeolite nanoparticles can potentially be used for selectively capture of APOC-III in order to reduce the activation of lipoprotein lipase inhibition during hypertriglyceridemia treatment. The zeolite nanoparticles can be adapted to hemophilic patients (hemophilia A (F-VIII deficient) and hemophilia B (F-IX deficient)) with a risk of bleeding, and thus might be potentially used in combination with the existing therapy.

  15. Zeolite Nanoparticles for Selective Sorption of Plasma Proteins.

    PubMed

    Rahimi, M; Ng, E-P; Bakhtiari, K; Vinciguerra, M; Ali Ahmad, H; Awala, H; Mintova, S; Daghighi, M; Bakhshandeh Rostami, F; de Vries, M; Motazacker, M M; Peppelenbosch, M P; Mahmoudi, M; Rezaee, F

    2015-11-30

    The affinity of zeolite nanoparticles (diameter of 8-12 nm) possessing high surface area and high pore volume towards human plasma proteins has been investigated. The protein composition (corona) of zeolite nanoparticles has been shown to be more dependent on the plasma protein concentrations and the type of zeolites than zeolite nanoparticles concentration. The number of proteins present in the corona of zeolite nanoparticles at 100% plasma (in vivo state) is less than with 10% plasma exposure. This could be due to a competition between the proteins to occupy the corona of the zeolite nanoparticles. Moreover, a high selective adsorption for apolipoprotein C-III (APOC-III) and fibrinogen on the zeolite nanoparticles at high plasma concentration (100%) was observed. While the zeolite nanoparticles exposed to low plasma concentration (10%) exhibited a high selective adsorption for immunoglobulin gamma (i.e. IGHG1, IGHG2 and IGHG4) proteins. The zeolite nanoparticles can potentially be used for selectively capture of APOC-III in order to reduce the activation of lipoprotein lipase inhibition during hypertriglyceridemia treatment. The zeolite nanoparticles can be adapted to hemophilic patients (hemophilia A (F-VIII deficient) and hemophilia B (F-IX deficient)) with a risk of bleeding, and thus might be potentially used in combination with the existing therapy.

  16. Zeolite Nanoparticles for Selective Sorption of Plasma Proteins

    PubMed Central

    Rahimi, M.; Ng, E.-P.; Bakhtiari, K.; Vinciguerra, M.; Ahmad, H. Ali; Awala, H.; Mintova, S.; Daghighi, M.; Bakhshandeh Rostami, F.; de Vries, M.; Motazacker, M. M.; Peppelenbosch, M. P.; Mahmoudi, M.; Rezaee, F.

    2015-01-01

    The affinity of zeolite nanoparticles (diameter of 8–12 nm) possessing high surface area and high pore volume towards human plasma proteins has been investigated. The protein composition (corona) of zeolite nanoparticles has been shown to be more dependent on the plasma protein concentrations and the type of zeolites than zeolite nanoparticles concentration. The number of proteins present in the corona of zeolite nanoparticles at 100% plasma (in vivo state) is less than with 10% plasma exposure. This could be due to a competition between the proteins to occupy the corona of the zeolite nanoparticles. Moreover, a high selective adsorption for apolipoprotein C-III (APOC-III) and fibrinogen on the zeolite nanoparticles at high plasma concentration (100%) was observed. While the zeolite nanoparticles exposed to low plasma concentration (10%) exhibited a high selective adsorption for immunoglobulin gamma (i.e. IGHG1, IGHG2 and IGHG4) proteins. The zeolite nanoparticles can potentially be used for selectively capture of APOC-III in order to reduce the activation of lipoprotein lipase inhibition during hypertriglyceridemia treatment. The zeolite nanoparticles can be adapted to hemophilic patients (hemophilia A (F-VIII deficient) and hemophilia B (F-IX deficient)) with a risk of bleeding, and thus might be potentially used in combination with the existing therapy. PMID:26616161

  17. To Investigate the Absorption, Dynamic Contact Angle and Printability Effects of Synthetic Zeolite Pigments in an Inkjet Receptive Coating

    NASA Astrophysics Data System (ADS)

    Jalindre, Swaraj Sunil

    Ink absorption performance in inkjet receptive coatings containing synthetic zeolite pigments was studied. Coating pigment pore and particle size distribution are the key parameters that influence in modifying media surface properties, thus affecting the rate of ink penetration and drying time (Scholkopf, et al. 2004). The primary objective of this study was: (1) to investigate the synthetic zeolite pigment effects on inkjet ink absorption, dynamic contact angle and printability, and (2) to evaluate these novel synthetic zeolite pigments in replacing the fumed silica pigments in conventional inkjet receptive coatings. In this research study, single pigment coating formulations (in equal P:B ratio) were prepared using microporous synthetic zeolite pigments (5A, Organophilic and 13X) and polyvinyl alcohol (PVOH) binder. The laboratory-coated samples were characterized for absorption, air permeance, roughness, drying time, wettability and print fidelity. Based on the rheological data, it was found that the synthetic zeolite formulated coatings depicted a Newtonian flow behavior at low shear; while the industry accepted fumed silica based coatings displayed a characteristically high pseudoplastic flow behavior. Our coated samples generated using microporous synthetic zeolite pigments produced low absorption, reduced wettability and accelerated ink drying characteristics. These characteristics were caused due to the synthetic zeolite pigments, which resulted in relatively closed surface structure coated samples. The research suggested that no single selected synthetic zeolite coating performed better than the conventional fumed silica based coatings. Experimental data also showed that there was no apparent relationship between synthetic zeolite pigment pore sizes and inkjet ink absorption. For future research, above coated samples should be evaluated for pore size distribution using Mercury Porosimeter, which quantifies surface porosity of coated samples. This presented

  18. 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.

  19. Magnetostriction and corrosion studies in single crystals of iron-gallium alloys

    NASA Astrophysics Data System (ADS)

    Jayaraman, Tanjore V.

    Iron-gallium alloys have an excellent combination of large low-field magnetostriction, good mechanical properties, low hysteresis, and relatively low cost. This dissertation focuses on the magneto striction and corrosion behaviors of single crystals of Fe-Ga alloys. In the first part, the variation of magnetostrictive coefficient: (3/2) lambda100, with composition and heat treatment conditions of Fe-Ga alloys, is examined. Single crystals with compositions Fe-15 at.% Ga, Fe-20 at.% Ga, and Fe-27.5 at.% Ga were obtained by (a) vertical Bridgman technique (DG) and (b) vertical Bridgman technique followed by long-term annealing (LTA) and quenching. Rapid quenching from a phase region improves the (3/2) lambda 100 value in these alloys. X-ray diffraction characterization showed for the first time the direct evidence of short-range ordering in these alloys. The second part reports the first study of alpha" ordering heat treatment on the elastic properties and magnetostriction of Fe-27.5 at.% Ga alloy single crystals. The elastic constants were measured using resonant ultrasound spectroscopy (RUS), and the elastic properties and magneto-elastic coupling constant were calculated. The (3/2) lambda100 and B1 values obtained for a phase were higher than alpha" phase. The third part examines the first study of corrosion behavior of as-cast FeGa and Fe-Ga-Al alloys in acidic, basic, and simulated seawater environments. Corrosion measurements were performed by Tafel scan and polarization resistance method and in general exhibited good corrosion resistance. The fourth part examines the first study of corrosion behavior of Fe-15 at.% Ga, Fe-20 at.% Ga, and Fe-27.5 at.% Ga DG and LTA alloy single crystals and the dependence of corrosion rates on the crystal orientations. The corrosion resistance was better in basic environments followed by simulated seawater and acidic environments. The fifth part examines the effect of magnetostriction on the corrosion behavior of [100]-oriented

  20. Mechanical and optical nanodevices in single-crystal quartz

    NASA Astrophysics Data System (ADS)

    Sohn, Young-Ik; Miller, Rachel; Venkataraman, Vivek; Lončar, Marko

    2017-12-01

    Single-crystal α-quartz, one of the most widely used piezoelectric materials, has enabled a wide range of timing applications. Owing to the fact that an integrated thin-film based quartz platform is not available, most of these applications rely on macroscopic, bulk crystal-based devices. Here, we show that the Faraday cage angled-etching technique can be used to realize nanoscale electromechanical and photonic devices in quartz. Using this approach, we demonstrate quartz nanomechanical cantilevers and ring resonators featuring Qs of 4900 and 8900, respectively.

  1. Multilevel organization in hybrid thin films for optoelectronic applications.

    PubMed

    Vohra, Varun; Bolognesi, Alberto; Calzaferri, Gion; Botta, Chiara

    2009-10-20

    In this work we report two simple approaches to prepare hybrid thin films displaying a high concentration of zeolite crystals that could be used as active layers in optoelectronic devices. In the first approach, in order to organize nanodimensional zeolite crystals of 40 nm diameter in an electroactive environment, we chemically modify their external surface and play on the hydrophilic/hydrophobic forces. We obtain inorganic nanocrystals that self-organize in honeycomb electroluminescent polymer structures obtained by breath figure formation. The different functionalizations of the zeolite surface result in different organizations inside the cavities of the polymeric structure. The second approach involving soft-litography techniques allows one to arrange single dye-loaded zeolite L crystals of 800 nm of length by mechanical loading into the nanocavities of a conjugated polymer. Both techniques result in the formation of thin hybrid films displaying three levels of organization: organization of the dye molecules inside the zeolite nanochannels, organization of the zeolite crystals inside the polymer cavities, and micro- or nanostructuration of the polymer.

  2. One-step model of photoemission from single-crystal surfaces

    DOE PAGES

    Karkare, Siddharth; Wan, Weishi; Feng, Jun; ...

    2017-02-28

    In our paper, we present a three-dimensional one-step photoemission model that can be used to calculate the quantum efficiency and momentum distributions of electrons photoemitted from ordered single-crystal surfaces close to the photoemission threshold. Using Ag(111) as an example, we also show that the model can not only calculate the quantum efficiency from the surface state accurately without using any ad hoc parameters, but also provides a theoretical quantitative explanation of the vectorial photoelectric effect. This model in conjunction with other band structure and wave function calculation techniques can be effectively used to screen single-crystal photoemitters for use as electronmore » sources for particle accelerator and ultrafast electron diffraction applications.« less

  3. 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.

  4. Increased thermal conductivity monolithic zeolite structures

    DOEpatents

    Klett, James; Klett, Lynn; Kaufman, Jonathan

    2008-11-25

    A monolith comprises a zeolite, a thermally conductive carbon, and a binder. The zeolite is included in the form of beads, pellets, powders and mixtures thereof. The thermally conductive carbon can be carbon nano-fibers, diamond or graphite which provide thermal conductivities in excess of about 100 W/mK to more than 1,000 W/mK. A method of preparing a zeolite monolith includes the steps of mixing a zeolite dispersion in an aqueous colloidal silica binder with a dispersion of carbon nano-fibers in water followed by dehydration and curing of the binder is given.

  5. Effect of grain boundary on the field-effect mobility of microrod single crystal organic transistors.

    PubMed

    Kim, Jaekyun; Kang, Jingu; Cho, Sangho; Yoo, Byungwook; Kim, Yong-Hoon; Park, Sung Kyu

    2014-11-01

    High-performance microrod single crystal organic transistors based on a p-type 2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene (C8-BTBT) semiconductor are fabricated and the effects of grain boundaries on the carrier transport have been investigated. The spin-coating of C8-BTBT and subsequent solvent vapor annealing process enabled the formation of organic single crystals with high aspect ratio in the range of 10 - 20. It was found that the organic field-effect transistors (OFETs) based on these single crystals yield a field-effect mobility and an on/off current ratio of 8.04 cm2/Vs and > 10(5), respectively. However, single crystal OFETs with a kink, in which two single crystals are fused together, exhibited a noticeable drop of field-effect mobility, and we claim that this phenomenon results from the carrier scattering at the grain boundary.

  6. Zeolites on Mars: Prospects for Remote Sensing

    NASA Technical Reports Server (NTRS)

    Gaffney, E. S.; Singer, R. B.; Kunkle, T. D.

    1985-01-01

    The Martian surface composition measured by Viking can be represented by several combinations of minerals incorporating major fractions of zeolites known to occur in altered mafic rocks and polar soils on Earth. The abundant occurrence of zeolites on Mars is consistent with what is known about both the physical and chemical environment of that planet. The laboratory reflectance spectra (0.65 to 2.55 microns) of a number of relatively pure zeolite minerals and some naturally occurring zeolite-clay soils were measured. All of the spectra measured are dominated by strong absorption near 1.4 and 1.9 microns and a steep reflectance drop longward of about 2.2 microns, all of which are due to abundant H2O. Weaker water overtone bands are also apparent, and in most cases there is spectral evidence for minor Fe(3+). In these features the zeolite spectra are similar to spectra of smectite clays which have abundant interlayer water. The most diagnostic difference between clay and zeolite spectra is the total absence in the zeolites of the weak structural OH absorption.

  7. Low Leakage Superconducting Tunnel Junctions with a Single Crystal Al2O3 Barrier

    DTIC Science & Technology

    2016-03-30

    have recently implemented Josephson junction superconducting devices into qubits [1-6]. Before a multi -qubit quantum computer is realized, however...Low-Leakage Superconducting Tunnel Junctions with a Single-Crystal Al2O3 Barrier* S Oh1,2, K Cicak1, R McDermott3, K B Cooper3, K D Osborn1, R W...growth scheme for single-crystal Al2O3 tunnel barriers. The barriers are epitaxially grown on single-crystal rhenium (Re) base electrodes that are

  8. Modeling Nonlinear Elastic-plastic Behavior of RDX Single Crystals During Indentation

    DTIC Science & Technology

    2012-01-01

    single crystals has also been probed using shock experiments (6, 12) and molecular dynamics simulations (12–14). RDX undergoes a polymorphic phase...Patterson, J.; Dreger, Z.; Gupta, Y. Shock-wave Induced Phase Transition in RDX Single Crystals. J. Phys. Chem. B 2007, 111, 10897–10904. 17. Bedrov, D...and Volume Compression of β - HMX and RDX . In Proc. Int. Symp. High Dynamic Pressures; Commissariat a l’Energie Atomique: Paris, 1978; pp 3–8. 24

  9. An Extra-Large-Pore Zeolite with 24×8×8-Ring Channels Using a Structure-Directing Agent Derived from Traditional Chinese Medicine.

    PubMed

    Zhang, Chuanqi; Kapaca, Elina; Li, Jiyang; Liu, Yunling; Yi, Xianfeng; Zheng, Anmin; Zou, Xiaodong; Jiang, Jiuxing; Yu, Jihong

    2018-03-12

    Extra-large-pore zeolites have attracted much interest because of their important applications because for processing larger molecules. Although great progress has been made in academic science and industry, it is challenging to synthesize these materials. A new extra-large-pore zeolite SYSU-3 (Sun Yat-sen University no. 3) has been synthesized by using a novel sophoridine derivative as an organic structure-directing agent (OSDA). The framework structure was solved and refined using continuous rotation electron diffraction (cRED) data from nanosized crystals. SYSU-3 exhibits a new zeolite framework topology, which has the first 24×8×8-ring extra-large-pore system and a framework density (FD) as low as 11.4 T/1000 Å 3 . The unique skeleton of the OSDA plays an essential role in the formation of the distinctive zeolite structure. This work provides a new perspective for developing new zeolitic materials by using alkaloids as cost-effective OSDAs. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. X-Ray diffraction on large single crystals using a powder diffractometer

    DOE PAGES

    Jesche, A.; Fix, M.; Kreyssig, A.; ...

    2016-06-16

    Information on the lattice parameter of single crystals with known crystallographic structure allows for estimations of sample quality and composition. In many cases it is sufficient to determine one lattice parameter or the lattice spacing along a certain, high- symmetry direction, e.g. in order to determine the composition in a substitution series by taking advantage of Vegard’s rule. Here we present a guide to accurate measurements of single crystals with dimensions ranging from 200 μm up to several millimeter using a standard powder diffractometer in Bragg-Brentano geometry. The correction of the error introduced by the sample height and the optimizationmore » of the alignment are discussed in detail. Finally, in particular for single crystals with a plate-like habit, the described procedure allows for measurement of the lattice spacings normal to the plates with high accuracy on a timescale of minutes.« less

  11. Magnetic properties of single crystal alpha-benzoin oxime: An EPR study

    NASA Astrophysics Data System (ADS)

    Sayin, Ulku; Dereli, Ömer; Türkkan, Ercan; Ozmen, Ayhan

    2012-02-01

    The electron paramagnetic resonance (EPR) spectra of gamma irradiated single crystals of alpha-benzoinoxime (ABO) have been examined between 120 and 440 K. Considering the dependence on temperature and the orientation of the spectra of single crystals in the magnetic field, we identified two different radicals formed in irradiated ABO single crystals. To theoretically determine the types of radicals, the most stable structure of ABO was obtained by molecular mechanic and B3LYP/6-31G(d,p) calculations. Four possible radicals were modeled and EPR parameters were calculated for the modeled radicals using the B3LYP method and the TZVP basis set. Calculated values of two modeled radicals were in strong agreement with experimental EPR parameters determined from the spectra. Additional simulated spectra of the modeled radicals, where calculated hyperfine coupling constants were used as starting points for simulations, were well matched with experimental spectra.

  12. Electrical resistivity measurements on fragile organic single crystals in the diamond anvil cell

    NASA Astrophysics Data System (ADS)

    Adachi, T.; Tanaka, H.; Kobayashi, H.; Miyazaki, T.

    2001-05-01

    A method of sample assembly for four-probe resistivity measurements on fragile organic single crystals using a diamond anvil cell is presented. A procedure to keep insulation between the metal gasket and four leads of thin gold wires bonded to the sample crystal by gold paint is described in detail. The resistivity measurements performed on a single crystal of an organic semiconductor and that of neutral molecules up to 15 GPa and down to 4.2 K showed that this new procedure of four-probe diamond anvil resistivity measurements enables us to obtain sufficiently accurate resistivity data of organic crystals.

  13. Orientation dependence of the stress rupture properties of Nickel-base superalloy single crystals

    NASA Technical Reports Server (NTRS)

    Mackay, R. A.

    1981-01-01

    The influence of orientation of the stress rupture behavior of Mar-M247 single crystals was studied. Stress rupture tests were performed at 724 MPa and 774 C where the effect of anisotropy is prominent. The mechanical behavior of the single crystals was rationalized on the basis of the Schmid factors for the operative slip systems and the lattice rotations which the crystals underwent during deformation. The stress rupture lives were found to be greatly influenced by the lattice rotations required to produce intersecting slip, because steady-state creep does not begin until after the onset of intersecting slip. Crystals which required large rotations to become oriented for intersecting slip exhibited a large primary creep strain, a large effective stress level at the onset of steady-state creep, and consequently a short stress rupture life. A unified analysis was attained for the stress rupture behavior of the Mar-M247 single crystals tested in this study at 774 C and that of the Mar-M200 single crystals tested in a prior study at 760 C. In this analysis, the standard 001-011-111 stereographic triangle was divided into several regions of crystallographic orientation which were rank ordered according to stress rupture life for this temperature regime. This plot indicates that those crystals having orientations within about 25 deg of the 001 exhibited significantly longer lives when their orientations were closer to the 001-011 boundary of the stereographic triangle than to the 001-111 boundary.

  14. Potassic zeolites from Brazilian coal ash for use as a fertilizer in agriculture.

    PubMed

    Flores, Camila Gomes; Schneider, Helena; Marcilio, Nilson Romeu; Ferret, Lizete; Oliveira, João Carlos Pinto

    2017-12-01

    Brazilian coal has an ash content ranging from 30 to 50% by weight. Consequently, its use in coal-fired thermoelectric for power production generates a lot of waste. The construction sector is the largest consumer of coal ash, but it cannot absorb the entire amount generated. Thus, other applications for coal ash should be studied in aim to optimize the use of this industrial waste. This research had as focus to synthesize potassic zeolite from of the coal ash into on potassium fertilizer for the grown wheat plant. In this work, it was used a subbituminous coal from Mina do Leão (RS, Brazil) presenting 48.7% ash content on a dry basis. Concerning the synthesis of potassic zeolite, it was adopted the conventional method of hydrothermal treatment with potassium hydroxide. A schedule of experiments was conducted in order to define the optimum condition of zeolite synthesis that was then used an alkaline solution of 5M KOH with a reaction time of 24h at 150°C. According to this procedure, it was obtained a zeolite with a single crystalline phase, identified through X-ray diffraction as Merlinoite. Subsequently, it was performed a set of tests using potassic zeolite asa fertilizer for plants in a greenhouse. The synthesized potassic zeolite showed a good potential for its use as fertilizer in agriculture. Copyright © 2017 Elsevier Ltd. All rights reserved.

  15. Anisotropic charge transport in large single crystals of π-conjugated organic molecules.

    PubMed

    Hourani, Wael; Rahimi, Khosrow; Botiz, Ioan; Koch, Felix Peter Vinzenz; Reiter, Günter; Lienerth, Peter; Heiser, Thomas; Bubendorff, Jean-Luc; Simon, Laurent

    2014-05-07

    The electronic properties of organic semiconductors depend strongly on the nature of the molecules, their conjugation and conformation, their mutual distance and the orientation between adjacent molecules. Variations of intramolecular distances and conformation disturb the conjugation and perturb the delocalization of charges. As a result, the mobility considerably decreases compared to that of a covalently well-organized crystal. Here, we present electrical characterization of large single crystals made of the regioregular octamer of 3-hexyl-thiophene (3HT)8 using a conductive-atomic force microscope (C-AFM) in air. We find a large anisotropy in the conduction with charge mobility values depending on the crystallographic orientation of the single crystal. The smaller conduction is in the direction of π-π stacking (along the long axis of the single crystal) with a mobility value in the order of 10(-3) cm(2) V(-1) s(-1), and the larger one is along the molecular axis (in the direction normal to the single crystal surface) with a mobility value in the order of 0.5 cm(2) V(-1) s(-1). The measured current-voltage (I-V) curves showed that along the molecular axis, the current followed an exponential dependence corresponding to an injection mode. In the π-π stacking direction, the current exhibits a space charge limited current (SCLC) behavior, which allows us to estimate the charge carrier mobility.

  16. Mutiple Czochralski growth of silicon crystals from a single crucible

    NASA Technical Reports Server (NTRS)

    Lane, R. L.; Kachare, A. H.

    1980-01-01

    An apparatus for the Czochralski growth of silicon crystals is presented which is capable of producing multiple ingots from a single crucible. The growth chamber features a refillable crucible with a water-cooled, vacuum-tight isolation valve located between the pull chamber and the growth furnace tank which allows the melt crucible to always be at vacuum or low argon pressure when retrieving crystal or introducing recharge polysilicon feed stock. The grower can thus be recharged to obtain 100 kg of silicon crystal ingots from one crucible, and may accommodate crucibles up to 35 cm in diameter. Evaluation of the impurity contents and I-V characteristics of solar cells fabricated from seven ingots grown from two crucibles reveals a small but consistent decrease in cell efficiency from 10.4% to 9.6% from the first to the fourth ingot made in a single run, which is explained by impurity build-up in the residual melt. The crystal grower thus may offer economic benefits through the extension of crucible lifetime and the reduction of furnace downtime.

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

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

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

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

  18. Transverse Mode Multi-Resonant Single Crystal Transducer

    NASA Technical Reports Server (NTRS)

    Snook, Kevin A. (Inventor); Liang, Yu (Inventor); Luo, Jun (Inventor); Hackenberger, Wesley S. (Inventor); Sahul, Raffi (Inventor)

    2015-01-01

    A transducer is disclosed that includes a multiply resonant composite, the composite having a resonator bar of a piezoelectric single crystal configured in a d(sub 32) transverse length-extensional resonance mode having a crystallographic orientation set such that the thickness axis is in the (110) family and resonance direction is the (001) family.

  19. Atomistic simulation of shocks in single crystal and polycrystalline Ta

    NASA Astrophysics Data System (ADS)

    Bringa, E. M.; Higginbotham, A.; Park, N.; Tang, Y.; Suggit, M.; Mogni, G.; Ruestes, C. J.; Hawreliak, J.; Erhart, P.; Meyers, M. A.; Wark, J. S.

    2011-06-01

    Non-equilibrium molecular dynamics (MD) simulations of shocks in Ta single crystals and polycrystals were carried out using up to 360 million atoms. Several EAM and FS type potentials were tested up to 150 GPa, with varying success reproducing the Hugoniot and the behavior of elastic constants under pressure. Phonon modes were studied to exclude possible plasticity nucleation by soft-phonon modes, as observed in MD simulations of Cu crystals. The effect of loading rise time in the resulting microstructure was studied for ramps up to 0.2 ns long. Dislocation activity was not observed in single crystals, unless there were defects acting as dislocation sources above a certain pressure. E.M.B. was funded by CONICET, Agencia Nacional de Ciencia y Tecnología (PICT2008-1325), and a Royal Society International Joint Project award.

  20. Ultrafast lattice dynamics of single crystal and polycrystalline gold nanofilms☆

    NASA Astrophysics Data System (ADS)

    Hu, Jianbo; Karam, Tony E.; Blake, Geoffrey A.; Zewail, Ahmed H.

    2017-09-01

    Ultrafast electron diffraction is employed to spatiotemporally visualize the lattice dynamics of 11 nm-thick single-crystal and 2 nm-thick polycrystalline gold nanofilms. Surprisingly, the electron-phonon coupling rates derived from two temperature simulations of the data reveal a faster interaction between electrons and the lattice in the case of the single-crystal sample. We interpret this unexpected behavior as arising from quantum confinement of the electrons in the 2 nm-thick gold nanofilm, as supported by absorption spectra, an effect that counteracts the expected increase in the electron scattering off surfaces and grain boundaries in the polycrystalline materials.

  1. Plastic strain arrangement in copper single crystals in sliding

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

    Chumaevskii, Andrey V., E-mail: tch7av@gmail.com; Lychagin, Dmitry V., E-mail: dvl-tomsk@mail.ru; Tarasov, Sergei Yu., E-mail: tsy@ispms.tsc.ru

    2014-11-14

    Deformation of tribologically loaded contact zone is one of the wear mechanisms in spite of the fact that no mass loss may occur during this process. Generation of optimal crystallographic orientations of the grains in a polycrystalline materials (texturing) may cause hardening and reducing the deformation wear. To reveal the orientation dependence of an individual gain and simplify the task we use copper single crystals with the orientations of the compression axis along [111] and [110]. The plastic deformation was investigated by means of optical, scanning electron microscopy and EBSD techniques. It was established that at least four different zonesmore » were generated in the course of sliding test, such as non-deformed base metal, plastic deformation layer sliding, crystalline lattice reorientation layer and subsurface grain structure layer. The maximum plastic strain penetration depth was observed on [110]-single crystals. The minimum stability of [111]-crystals with respect to rotation deformation mode as well as activation of shear in the sliding contact plane provide for rotation deformation localization below the worn surface. The high-rate accumulation of misorientations and less strain penetration depth was observed on [111]-crystals as compared to those of [110]-oriented ones.« less

  2. 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

  3. 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.

  4. 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.

  5. Zeolite-templated carbons - three-dimensional microporous graphene frameworks.

    PubMed

    Nishihara, H; Kyotani, T

    2018-05-31

    Zeolite-templated carbons (ZTCs) are ordered microporous carbons synthesized by using zeolite as a sacrificial template. Unlike well-known ordered mesoporous carbons obtained by using mesoporous silica templates, ZTCs consist of curved and single-layer graphene frameworks, thereby affording uniform micropore size (ca. 1.2 nm), developed microporosity (∼1.7 cm3 g-1), very high surface area (∼4000 m2 g-1), good compatibility with chemical modification, and remarkable softness/elasticity. Thus, ZTCs have been used in many applications such as hydrogen storage, methane storage, CO2 capture, liquid-phase adsorption, catalysts, electrochemical capacitors, batteries, and fuel cells. Herein, the relevant research studies are summarized, and the properties as well as the performances of ZTCs are compared with those of other materials including metal-organic frameworks, to elucidate the intrinsic advantages of ZTCs and their future development.

  6. Anisotropic constitutive modeling for nickel base single crystal superalloys using a crystallographic approach

    NASA Technical Reports Server (NTRS)

    Stouffer, D. C.; Sheh, M. Y.

    1988-01-01

    A micromechanical model based on crystallographic slip theory was formulated for nickel-base single crystal superalloys. The current equations include both drag stress and back stress state variables to model the local inelastic flow. Specially designed experiments have been conducted to evaluate the effect of back stress in single crystals. The results showed that (1) the back stress is orientation dependent; and (2) the back stress state variable in the inelastic flow equation is necessary for predicting anelastic behavior of the material. The model also demonstrated improved fatigue predictive capability. Model predictions and experimental data are presented for single crystal superalloy Rene N4 at 982 C.

  7. Single-crystal films of a combination of materials (co-crystal) involving DAST and IR-125 for electro-optic applications

    NASA Astrophysics Data System (ADS)

    Narayanan, A.; Titus, J.; Rajagopalan, H.; Vippa, P.; Thakur, M.

    2006-03-01

    Single-crystal film of DAST (4'-dimethylamino-N-methyl-4-stilbazolium tosylate) has been shown [1] to have exceptionally large electro-optic coefficients (r11 ˜ 770 pm/V at 633 nm). In this report, single crystal film of a combination of materials (co-crystal) involving DAST and a dye molecule IR-125 will be discussed. Modified shear method was used to prepare the co-crystal films. The film has been characterized using polarized optical microscopy, optical absorption spectroscopy and x-ray diffraction. The optical absorption spectrum has two major bands: one at about 350--600 nm corresponding to DAST and the other at about 600-900 nm corresponding to IR-125. The x-ray diffraction results show peaks involving the presence of DAST and IR-125 within the co-crystal film. Since the co-crystal has strong absorption at longer wavelengths it is expected to show higher electro-optic coefficients at longer wavelengths. Preliminary measurements at 1.55 μm indicate a high electro-optic coefficient of the co-crystal film. [1] Swamy, Kutty, Titus, Khatavkar, Thakur, Appl. Phys. Lett. 2004, 85, 4025; Kutty, Thakur, Appl. Phys. Lett. 2005, 87, 191111.

  8. 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.

  9. 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.

  10. Preparation of functionalized zeolitic frameworks

    DOEpatents

    Yaghi, Omar M; Hayashi, Hideki; Banerjee, Rahul; Park, Kyo Sung; Wang, Bo; Cote, Adrien P

    2012-11-20

    The disclosure provides zeolitic frameworks for gas separation, gas storage, catalysis and sensors. More particularly the disclosure provides zeolitic frameworks (ZIFs). The ZIF of the disclosure comprises any number of transition metals or a homogenous transition metal composition.

  11. Preparation of functionalized zeolitic frameworks

    DOEpatents

    Yaghi, Omar M.; Hayashi, Hideki; Banerjee, Rahul; Park, Kyo Sung; Wang, Bo; Cote, Adrien P.

    2014-08-19

    The disclosure provides zeolitic frameworks for gas separation, gas storage, catalysis and sensors. More particularly the disclosure provides zeolitic frameworks (ZIFs). The ZIF of the disclosure comprises any number of transition metals or a homogenous transition metal composition.

  12. Preparation of functionalized zeolitic frameworks

    DOEpatents

    Yaghi, Omar M; Furukawa, Hiroyasu; Wang, Bo

    2013-07-09

    The disclosure provides zeolitic frameworks for gas separation, gas storage, catalysis and sensors. More particularly the disclosure provides zeolitic frameworks (ZIFs). The ZIF of the disclosure comprises any number of transition metals or a homogenous transition metal composition.

  13. High Pressure Single Crystal Diffraction at PX 2

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

    Zhang, Dongzhou; Dera, Przemyslaw K.; Eng, Peter J.

    2017-01-01

    In this report, we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell at the GSECARS 13-BM-C beamline at the Advanced Photon Source. ATREX and RSV programs are used to analyze the data.

  14. Ammonothermal Growth of Chalcogenide Single Crystal Materials

    DTIC Science & Technology

    1997-11-05

    chalcogenide with an acidic mineraiizer 15 in presence of liquid ammonia solvent at high pressures and at temperatures in the range of about 300 to 550°C...demonstrates growth of binary CaS single crystals in a medium consisting of CaS powder and NH4I acid mineraiizer in ammonia solvent in a fused quartz

  15. Activated zeolite--suitable carriers for microorganisms in anaerobic digestion processes?

    PubMed

    Weiß, S; Lebuhn, M; Andrade, D; Zankel, A; Cardinale, M; Birner-Gruenberger, R; Somitsch, W; Ueberbacher, B J; Guebitz, G M

    2013-04-01

    Plant cell wall structures represent a barrier in the biodegradation process to produce biogas for combustion and energy production. Consequently, approaches concerning a more efficient de-polymerisation of cellulose and hemicellulose to monomeric sugars are required. Here, we show that natural activated zeolites (i.e. trace metal activated zeolites) represent eminently suitable mineral microhabitats and potential carriers for immobilisation of microorganisms responsible for anaerobic hydrolysis of biopolymers stabilising related bacterial and methanogenic communities. A strategy for comprehensive analysis of immobilised anaerobic populations was developed that includes the visualisation of biofilm formation via scanning electron microscopy and confocal laser scanning microscopy, community and fingerprint analysis as well as enzyme activity and identification analyses. Using SDS polyacrylamide gel electrophoresis, hydrolytical active protein bands were traced by congo red staining. Liquid chromatography/mass spectroscopy revealed cellulolytical endo- and exoglucanase (exocellobiohydrolase) as well as hemicellulolytical xylanase/mannase after proteolytic digestion. Relations to hydrolytic/fermentative zeolite colonisers were obtained by using single-strand conformation polymorphism analysis (SSCP) based on amplification of bacterial and archaeal 16S rRNA fragments. Thereby, dominant colonisers were affiliated to the genera Clostridium, Pseudomonas and Methanoculleus. The specific immobilisation on natural zeolites with functional microbes already colonising naturally during the fermentation offers a strategy to systematically supply the biogas formation process responsive to population dynamics and process requirements.

  16. 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.

  17. Natural zeolites in diet or litter of broilers.

    PubMed

    Schneider, A F; Almeida, D S De; Yuri, F M; Zimmermann, O F; Gerber, M W; Gewehr, C E

    2016-04-01

    This study aims to analyse the influence of adding natural zeolites (clinoptilolite) to the diet or litter of broilers and their effects on growth performance, carcass yield and litter quality. Three consecutive flocks of broilers were raised on the same sawdust litter, from d 1 to d 42 of age, and distributed in three treatments (control with no added zeolites, addition of 5 g/kg zeolite to diet and addition of 100 g/kg zeolites to litter). The addition of zeolites to the diet or litter did not affect growth performance or carcass yield. The addition of zeolites to the diet did not influence moisture content of the litter, ammonia volatilisation was reduced only in the first flock and pH of litter was reduced in the second and third flock. However, the addition of zeolites to the litter reduced moisture content, litter pH and ammonia volatilisation in all flocks analysed. The addition of 5 g/kg zeolite to the diet in three consecutive flocks was not effective in maintaining litter quality, whereas the addition of 100 g/kg natural zeolites to sawdust litter reduced litter moisture and ammonia volatilisation in three consecutive flocks raised on the same litter.

  18. Single crystal growth, magnetic and thermal properties of perovskite YFe0.6Mn0.4O3 single crystal

    NASA Astrophysics Data System (ADS)

    Xie, Tao; Shen, Hui; Zhao, Xiangyang; Man, Peiwen; Wu, Anhua; Su, Liangbi; Xu, Jiayue

    2016-11-01

    High quality YFe0.6Mn0.4O3 single crystal was grown by floating zone technique using a four-mirror-image-furnace under flowing air. Powder X-ray diffraction gives well evidence that the specimen has an orthorhombic structure, with space group Pbnm. Temperature dependence of the magnetizations of YFe0.6Mn0.4O3 single crystal were studied under ZFC and FC modes in the temperature range from 5 K to 400 K. A clear spin reorientation transition behavior (Γ4→Γ1) is observed in the temperature range of 322-316 K, due to the substitution of Mn at the Fe site of YFeO3. Its Néel temperature is around 385 K. Moreover, the spin reorientation is verified by the change of magnetic hysteresis loops of the sample along [001] axis in the temperature range of 50-385 K. The thermal properties of the sample were measured by the differential scanning calorimeter (DSC) from 300 K to 500 K, which also clearly appear anomaly in the spin reorientation region.

  19. Self-assembled single-crystal silicon circuits on plastic

    PubMed Central

    Stauth, Sean A.; Parviz, Babak A.

    2006-01-01

    We demonstrate the use of self-assembly for the integration of freestanding micrometer-scale components, including single-crystal, silicon field-effect transistors (FETs) and diffusion resistors, onto flexible plastic substrates. Preferential self-assembly of multiple microcomponent types onto a common platform is achieved through complementary shape recognition and aided by capillary, fluidic, and gravitational forces. We outline a microfabrication process that yields single-crystal, silicon FETs in a freestanding, powder-like collection for use with self-assembly. Demonstrations of self-assembled FETs on plastic include logic inverters and measured electron mobility of 592 cm2/V-s. Finally, we extend the self-assembly process to substrates each containing 10,000 binding sites and realize 97% self-assembly yield within 25 min for 100-μm-sized elements. High-yield self-assembly of micrometer-scale functional devices as outlined here provides a powerful approach for production of macroelectronic systems. PMID:16968780

  20. Zeolites: Can they be synthesized by design

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

    Davis, M.E.

    1994-09-01

    Zeolites and zeolite-like molecular sieves are crystalline oxides that have high surface-to-volume ratios and are able to recognize, discriminate, and organize molecules with differences of < 1 [angstrom]. The close connection between the atomic structure and macroscopic properties of these materials has led to uses in molecular recognition. For example, zeolites and zeolite-like molecular sieves can reveal marvelous molecular recognition specificity and sensitivity that can be applied to catalysis, separations technology, and chemical sensing. Additionally, they can serve as hosts to organize guest atoms and molecules that endow composite materials with optoelectric and electrochemical properties. Because of the high levelmore » of structural control necessary to create high-performance materials with zeolites or zeolite-like molecular sieves, the design and synthesis of these solids with specific architectures and properties are highly desired. Although this lofty goal is still elusive, advances have been made to allow the serious consideration of designing molecular sieves. Here, the author covers two aspects of this ongoing effort. First, he discusses the feasibility of designing pore architectures through the use of organic structure-directing agents. Second, he explores the possibility of creating zeolites through ''Lego chemistry.''« less

  1. Crystallinity of the epitaxial heterojunction of C60 on single crystal pentacene

    NASA Astrophysics Data System (ADS)

    Tsuruta, Ryohei; Mizuno, Yuta; Hosokai, Takuya; Koganezawa, Tomoyuki; Ishii, Hisao; Nakayama, Yasuo

    2017-06-01

    The structure of pn heterojunctions is an important subject in the field of organic semiconductor devices. In this work, the crystallinity of an epitaxial pn heterojunction of C60 on single crystal pentacene is investigated by non-contact mode atomic force microscopy and high-resolution grazing incidence x-ray diffraction. Analysis shows that the C60 molecules assemble into grains consisting of single crystallites on the pentacene single crystal surface. The in-plane mean crystallite size exceeds 0.1 μm, which is at least five time larger than the size of crystallites deposited onto polycrystalline pentacene thin films grown on SiO2. The results indicate that improvement in the crystal quality of the underlying molecular substrate leads to drastic promotion of the crystallinity at the organic semiconductor heterojunction.

  2. Ambipolar light-emitting organic single-crystal transistors with a grating resonator

    PubMed Central

    Maruyama, Kenichi; Sawabe, Kosuke; Sakanoue, Tomo; Li, Jinpeng; Takahashi, Wataru; Hotta, Shu; Iwasa, Yoshihiro; Takenobu, Taishi

    2015-01-01

    Electrically driven organic lasers are among the best lasing devices due to their rich variety of emission colors as well as other advantages, including printability, flexibility, and stretchability. However, electrically driven lasing in organic materials has not yet been demonstrated because of serious luminescent efficiency roll-off under high current density. Recently, we found that the organic ambipolar single-crystal transistor is an excellent candidate for lasing devices because it exhibits less efficient roll-off, high current density, and high luminescent efficiency. Although a single-mode resonator combined with light-emitting transistors (LETs) is necessary for electrically driven lasing devices, the fragility of organic crystals has strictly limited the fabrication of resonators, and LETs with optical cavities have never been fabricated until now. To achieve this goal, we improved the soft ultraviolet-nanoimprint lithography method and demonstrated electroluminescence from a single-crystal LET with a grating resonator, which is a crucial milestone for future organic lasers. PMID:25959455

  3. Reversible adapting layer produces robust single-crystal electrocatalyst for oxygen evolution.

    PubMed

    Tung, Ching-Wei; Hsu, Ying-Ya; Shen, Yen-Ping; Zheng, Yixin; Chan, Ting-Shan; Sheu, Hwo-Shuenn; Cheng, Yuan-Chung; Chen, Hao Ming

    2015-08-28

    Electrochemically converting water into oxygen/hydrogen gas is ideal for high-density renewable energy storage in which robust electrocatalysts for efficient oxygen evolution play crucial roles. To date, however, electrocatalysts with long-term stability have remained elusive. Here we report that single-crystal Co3O4 nanocube underlay with a thin CoO layer results in a high-performance and high-stability electrocatalyst in oxygen evolution reaction. An in situ X-ray diffraction method is developed to observe a strong correlation between the initialization of the oxygen evolution and the formation of active metal oxyhydroxide phase. The lattice of skin layer adapts to the structure of the active phase, which enables a reversible facile structural change that facilitates the chemical reactions without breaking the scaffold of the electrocatalysts. The single-crystal nanocube electrode exhibits stable, continuous oxygen evolution for >1,000 h. This robust stability is attributed to the complementary nature of defect-free single-crystal electrocatalyst and the reversible adapting layer.

  4. Deformation relief evolution during sliding friction of Hadfield steel single crystal

    NASA Astrophysics Data System (ADS)

    Lychagin, D. V.; Filippov, A. V.; Novitskaya, O. S.; Kolubaev, A. V.; Sizova, O. V.

    2017-12-01

    The paper deals with the evolution of the deformation relief formed on lateral faces of single crystals of Hadfield steel during dry sliding friction. The use of single crystals with the predetermined orientation enables to analyze the development of shear systems subject to the duration of tribological tests. As the test duration increases, slip bands are curved and thicken in the near-surface region. After 24 hours of friction, single crystals of Hadfield steel demonstrate the maximum hardening. Afterwards, the wear process begins, which is followed by the repeated strain hardening of the specimens. After 48 hours of friction, the height of the deformation relief nearly halves on all of the three faces, as compared to that observed after 24 hours of friction. Differences in the propagation height of slip bands on the faces occur due to the uneven running-in as well as the complex involvement pattern of shear systems into the deformation process.

  5. 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.

  6. Magnetostriction of Hexagonal HoMnO3 and YMnO3 Single Crystals

    NASA Astrophysics Data System (ADS)

    Pavlovskii, N. S.; Dubrovskii, A. A.; Nikitin, S. E.; Semenov, S. V.; Terent'ev, K. Yu.; Shaikhutdinov, K. A.

    2018-03-01

    We report on the magnetostriction of hexagonal HoMnO3 and YMnO3 single crystals in a wide range of applied magnetic fields (up to H = 14 T) at all possible combinations of the mutual orientations of magnetic field H and magnetostriction Δ L/L. The measured Δ L/L( H, T) data agree well with the magnetic phase diagram of the HoMnO3 single crystal reported previously by other authors. It is shown that the nonmonotonic behavior of magnetostriction of the HoMnO3 crystal is caused by the Ho3+ ion; the magnetic moment of the Mn3+ ion parallel to the hexagonal crystal axis. The anomalies established from the magnetostriction measurements of HoMnO3 are consistent with the phase diagram of these compounds. For the isostructural YMnO3 single crystal with a nonmagnetic rare-earth ion, the Δ L/L( H, T) dependences are described well by a conventional quadratic law in a wide temperature range (4-100 K). In addition, the magnetostriction effect is qualitatively estimated with regard to the effect of the crystal electric field on the holmium ion.

  7. Electrically-pumped, broad-area, single-mode photonic crystal lasers.

    PubMed

    Zhu, Lin; Chak, Philip; Poon, Joyce K S; DeRose, Guy A; Yariv, Amnon; Scherer, Axel

    2007-05-14

    Planar broad-area single-mode lasers, with modal widths of the order of tens of microns, are technologically important for high-power applications and improved coupling efficiency into optical fibers. They may also find new areas of applications in on-chip integration with devices that are of similar size scales, such as for spectroscopy in microfluidic chambers or optical signal processing with micro-electromechanical systems. An outstanding challenge is that broad-area lasers often require external means of control, such as injection-locking or a frequency/spatial filter to obtain single-mode operation. In this paper, we propose and demonstrate effective index-guided, large-area, edge-emitting photonic crystal lasers driven by pulsed electrical current injection at the optical telecommunication wavelength of 1550 nm. By suitable design of the photonic crystal lattice, our lasers operate in a single mode with a 1/e(2) modal width of 25 microm and a length of 600 microm.

  8. Benzothiazolium Single Crystals: A New Class of Nonlinear Optical Crystals with Efficient THz Wave Generation.

    PubMed

    Lee, Seung-Heon; Lu, Jian; Lee, Seung-Jun; Han, Jae-Hyun; Jeong, Chan-Uk; Lee, Seung-Chul; Li, Xian; Jazbinšek, Mojca; Yoon, Woojin; Yun, Hoseop; Kang, Bong Joo; Rotermund, Fabian; Nelson, Keith A; Kwon, O-Pil

    2017-08-01

    Highly efficient nonlinear optical organic crystals are very attractive for various photonic applications including terahertz (THz) wave generation. Up to now, only two classes of ionic crystals based on either pyridinium or quinolinium with extremely large macroscopic optical nonlinearity have been developed. This study reports on a new class of organic nonlinear optical crystals introducing electron-accepting benzothiazolium, which exhibit higher electron-withdrawing strength than pyridinium and quinolinium in benchmark crystals. The benzothiazolium crystals consisting of new acentric core HMB (2-(4-hydroxy-3-methoxystyryl)-3-methylbenzo[d]thiazol-3-ium) exhibit extremely large macroscopic optical nonlinearity with optimal molecular ordering for maximizing the diagonal second-order nonlinearity. HMB-based single crystals prepared by simple cleaving method satisfy all required crystal characteristics for intense THz wave generation such as large crystal size with parallel surfaces, moderate thickness and high optical quality with large optical transparency range (580-1620 nm). Optical rectification of 35 fs pulses at the technologically very important wavelength of 800 nm in 0.26 mm thick HMB crystal leads to one order of magnitude higher THz wave generation efficiency with remarkably broader bandwidth compared to standard inorganic 0.5 mm thick ZnTe crystal. Therefore, newly developed HMB crystals introducing benzothiazolium with extremely large macroscopic optical nonlinearity are very promising materials for intense broadband THz wave generation and other nonlinear optical applications. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Free-standing nanomechanical and nanophotonic structures in single-crystal diamond

    NASA Astrophysics Data System (ADS)

    Burek, Michael John

    Realizing complex three-dimensional structures in a range of material systems is critical to a variety of emerging nanotechnologies. This is particularly true of nanomechanical and nanophotonic systems, both relying on free-standing small-scale components. In the case of nanomechanics, necessary mechanical degrees of freedom require physically isolated structures, such as suspended beams, cantilevers, and membranes. For nanophotonics, elements like waveguides and photonic crystal cavities rely on light confinement provided by total internal reflection or distributed Bragg reflection, both of which require refractive index contrast between the device and surrounding medium (often air). Such suspended nanostructures are typically fabricated in a heterolayer structure, comprising of device (top) and sacrificial (middle) layers supported by a substrate (bottom), using standard surface nanomachining techniques. A selective, isotropic etch is then used to remove the sacrificial layer, resulting in free-standing devices. While high-quality, crystalline, thin film heterolayer structures are readily available for silicon (as silicon-on-insulator (SOI)) or III-V semiconductors (i.e. GaAs/AlGaAs), there remains an extensive list of materials with attractive electro-optic, piezoelectric, quantum optical, and other properties for which high quality single-crystal thin film heterolayer structures are not available. These include complex metal oxides like lithium niobate (LiNbO3), silicon-based compounds such as silicon carbide (SiC), III-V nitrides including gallium nitride (GaN), and inert single-crystals such as diamond. Diamond is especially attractive for a variety of nanoscale technologies due to its exceptional physical and chemical properties, including high mechanical hardness, stiffness, and thermal conductivity. Optically, it is transparent over a wide wavelength range (from 220 nm to the far infrared), has a high refractive index (n ~ 2.4), and is host to a vast

  10. 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.

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

    DOE PAGES

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

    2016-12-03

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

  12. Growth of rare-earth doped single crystal yttrium aluminum garnet fibers

    NASA Astrophysics Data System (ADS)

    Bera, Subhabrata; Nie, Craig D.; Harrington, James A.; Cheng, Long; Rand, Stephen C.; Li, Yuan; Johnson, Eric G.

    2018-02-01

    Rare-earth doped single crystal (SC) yttrium aluminum garnet (YAG) fibers have great potential as high-power laser gain media. SC fibers combine the superior material properties of crystals with the advantages of a fiber geometry. Improving processing techniques, growth of low-loss YAG SC fibers have been reported. A low-cost technique that allows for the growth of optical quality Ho:YAG single crystal (SC) fibers with different dopant concentrations have been developed and discussed. This technique is a low-cost sol-gel based method which offers greater flexibility in terms of dopant concentration. Self-segregation of Nd ions in YAG SC fibers have been observed. Such a phenomenon can be utilized to fabricate monolithic SC fibers with graded index.

  13. [In vitro study of vitamins B1, B2 and B6 adsorption on zeolite].

    PubMed

    Basić, Zorica; Kilibarda, Vesna; Dobrić, Silva; Resanović, Radmila

    2011-01-01

    Zeolites are the hydratised alumosilicates of alcali and earthalcali cations, which have a long three-dimensional crystal structure. Preparations on the basis of zeolites are used for adsorption of organic and nonorganic toxic substances and they, also, find more and more use in veterinary and human medicine and pharmacy. The aim of this study was to evaluate the possibilities of zeolite to adsorb vitamins B1, B2 and B6 in acid and neutral solutions, as well as the characteristics of the process (saturability, reversibility and competitiveness). The specific and sensitive HPLC method with fluorescent detector was used for determination of vitamins B1, B2 and B6. Analyte separation and detection were carried out by applying the reverse-phase method on column C18. An in vitro experiment was done by testing the influence of pH value (2 and 7), concentration of vitamin solution (1, 2 and 5 mg/L), the length of contact with zeolite (10-180 min) and cation competitiveness on the exchange capacity, which is achieved by media and zeolite contact, as well as a possible vitamins desorption through changing pH value of the solution at 37 degrees C. Jon competitiveness was examined by adding commercial feed mixture (grower) with a defined content of the examined vitamins in zeolite solutions the pH = 2 and pH = 7. Vitamins B1, B2 and B6 were stable in both pH=2 and pH = 7 solutions at 37 degrees C, in the defined time intervals. In acid solution concentrations of vitamins significantly declined in the first 10 min, with no significant decline in further 30 min for all the three concentrations tests. In neutral solution, after the addition of 1% zeolite, decrease in vitamins concentrations was slightly lower than in acid solution, but also significant in the first 10 min of the contact with zeolite. It was found that zeolite, which adsorbed vitamins in acid solution, transferred in the neutral one released a significant quantity of adsorbed vitamins after 30 min of extraction

  14. Efficiency of basalt zeolite and Cuban zeolite to adsorb ammonia released from poultry litter.

    PubMed

    Nuernberg, Giselle B; Moreira, Marcelo A; Ernani, Paulo R; Almeida, Jaime A; Maciel, Tais M

    2016-12-01

    Confined poultry production is an important livestock activity, which generates large amounts of waste associated with the potential for environmental pollution and ammonia (NH 3 ) emissions. The release of ammonia negatively affects poultry production and decreases the N content of wastes that could be used as soil fertilizers. The objective of this study was to evaluate a low-cost, simple and rapid method to simulate ammonia emissions from poultry litter as well as to quantify the reduction in the ammonia emissions to the environment employing two adsorbent zeolites, a commercial Cuban zeolite (CZ) and a ground basalt Brazilian rock containing zeolite (BZ). The experiments were conducted in a laboratory, in 2012-2013. The zeolites were characterized by X-ray diffraction (XRD), X-ray fluorescence spectrometry (XRF), physical adsorption of N 2 (BET) and scanning electron microscopy (SEM). Ammonia released from poultry litter and its simulation from NH 4 OH solution presented similar capture rates of 7.99 × 10 -5 and 7.35 × 10 -5  mg/h, respectively. Both zeolites contain SiO 2 and Al 2 O 3 as major constituents, with contents of 84% and 12% in the CZ, and 51% and 12% in the BZ, respectively, besides heulandite groups. Their BET surface areas were 89.4 and 11.3 m 2  g -1 , respectively, and the two zeolites had similar surface morphologies. The zeolites successfully adsorbed the ammonia released, but CZ was more efficient than BZ, since to capture all of the ammonia 5 g of CZ and 20 g of BZ were required. This difference is due to higher values for the superficial area, porosity, CEC and acid site strength of CZ relatively to BZ. The proposed methodology was shown to be an efficient method to simulate and quantify the ammonia released from poultry litter. Copyright © 2016 Elsevier Ltd. All rights reserved.

  15. Host-guest interaction between Acridine orange molecules and AFI or CHA zeolite crystals

    NASA Astrophysics Data System (ADS)

    Chen, Yanping; Fu, Ling; Xu, Xintong; Li, Irene Ling; Ruan, Shuangchen; Jian, Dunliang; Zhai, Jianpang

    2017-02-01

    Acridine orange (AO) molecules were incorporated in AlPO4-5, SAPO-5 and SAPO-47 single crystals by vapor-phase diffusion method. Polarized absorption spectra show that AO molecules are well aligned by the one-dimensional channel systems of AlPO4-5 and SAPO-5 matrices. While the orientation of AO molecules in SAPO-47 crystals is diverse owing to the three-dimensional cage structure of chabazite (structure code CHA). The absorption peak and emission peak of AO/SAPO-5 blue shift compared with that of AO/AlPO4-5 because the channel environment changes from non-polar medium to polar medium when Si substituted in the framework of AlPO4-5. The greater blue shift in absorption band and emission band of AO/SAPO-47 are expected to originate from the polar channel medium and smaller channel size of SAPO-47.

  16. An improved implementable process for the synthesis of zeolite 4A from bauxite tailings and its Cr3+ removal capacity

    NASA Astrophysics Data System (ADS)

    Lei, Peng-cheng; Shen, Xian-jiang; Li, Yang; Guo, Min; Zhang, Mei

    2016-07-01

    A simple and practical method for the synthesis of zeolite 4A from bauxite tailings is presented in this paper. Systematic investigations were carried out regarding the capacity of zeolite 4A to remove Cr(III) from aqueous solutions with relatively low initial concentrations of Cr(III) (5-100 mg·L-1). It is found that the new method is extremely cost-effective and can significantly contribute in decreasing environmental pollution caused by the dumping of bauxite tailings. The Cr(III) removal capacity highly depends on the initial pH value and concentration of Cr(III) in the solution. The maximum removal capacity of Cr(III) was evaluated to be 85.1 mg·g-1 for zeolite 4A, measured at an initial pH value of 4 and an initial Cr(III) concentration of 5 mg·L-1. This approach enables a higher removal capacity at lower concentrations of Cr(III), which is a clear advantage over the chemical precipitation method. The removal mechanism of Cr(III) by zeolite 4A was examined. The results suggest that both ion exchange and the surface adsorption-crystallization reaction are critical steps. These two steps collectively resulted in the high removal capacity of zeolite 4A to remove Cr(III).

  17. Observation of Spectral Diffusion in Crystals Using Single Impurity Molecules

    DTIC Science & Technology

    1990-10-31

    from 12pentacene photophysical parameters including intersystem crossing . Apparently (and not surprisingly), the local pentacene environment this... pentacene molecules inp-terphenyl, both stable as well as spectrally diffusing single molecules can be observed. 20 DISTRIBUTION/AVAILABILITY OF ABSTRACT 121...with ultrathin sublimed crystals have removed this obstacle. For the case of pentacene impurities in crystals of p-terphenyl, we observe two radically

  18. Biochemical evolution. I. Polymerization On internal, organophilic silica surfaces of dealuminated zeolites and feldspars.

    PubMed

    Smith, J V

    1998-03-31

    Catalysis at mineral surfaces might generate replicating biopolymers from simple chemicals supplied by meteorites, volcanic gases, and photochemical gas reactions. Many ideas are implausible in detail because the proposed mineral surfaces strongly prefer water and other ionic species to organic ones. The molecular sieve silicalite (Union Carbide; = Al-free Mobil ZSM-5 zeolite) has a three-dimensional, 10-ring channel system whose electrically neutral Si-O surface strongly adsorbs organic species over water. Three -O-Si tetrahedral bonds lie in the surface, and the fourth Si-O points inwards. In contrast, the outward Si-OH of simple quartz and feldspar crystals generates their ionic organophobicity. The ZSM-5-type zeolite mutinaite occurs in Antarctica with boggsite and tschernichite (Al-analog of Mobil Beta). Archean mutinaite might have become de-aluminated toward silicalite during hot/cold/wet/dry cycles. Catalytic activity of silicalite increases linearly with Al-OH substitution for Si, and Al atoms tend to avoid each other. Adjacent organophilic and catalytic Al-OH regions in nanometer channels might have scavenged organic species for catalytic assembly into specific polymers protected from prompt photochemical destruction. Polymer migration along weathered silicic surfaces of micrometer-wide channels of feldspars might have led to assembly of replicating catalytic biomolecules and perhaps primitive cellular organisms. Silica-rich volcanic glasses should have been abundant on the early Earth, ready for crystallization into zeolites and feldspars, as in present continental basins. Abundant chert from weakly metamorphosed Archaean rocks might retain microscopic clues to the proposed mineral adsorbent/catalysts. Other framework silicas are possible, including ones with laevo/dextro one-dimensional channels. Organic molecules, transition-metal ions, and P occur inside modern feldspars.

  19. Biochemical evolution. I. Polymerization on internal, organophilic silica surfaces of dealuminated zeolites and feldspars

    PubMed Central

    Smith, Joseph V.

    1998-01-01

    Catalysis at mineral surfaces might generate replicating biopolymers from simple chemicals supplied by meteorites, volcanic gases, and photochemical gas reactions. Many ideas are implausible in detail because the proposed mineral surfaces strongly prefer water and other ionic species to organic ones. The molecular sieve silicalite (Union Carbide; = Al-free Mobil ZSM-5 zeolite) has a three-dimensional, 10-ring channel system whose electrically neutral Si-O surface strongly adsorbs organic species over water. Three -O-Si tetrahedral bonds lie in the surface, and the fourth Si-O points inwards. In contrast, the outward Si-OH of simple quartz and feldspar crystals generates their ionic organophobicity. The ZSM-5-type zeolite mutinaite occurs in Antarctica with boggsite and tschernichite (Al-analog of Mobil Beta). Archean mutinaite might have become de-aluminated toward silicalite during hot/cold/wet/dry cycles. Catalytic activity of silicalite increases linearly with Al-OH substitution for Si, and Al atoms tend to avoid each other. Adjacent organophilic and catalytic Al-OH regions in nanometer channels might have scavenged organic species for catalytic assembly into specific polymers protected from prompt photochemical destruction. Polymer migration along weathered silicic surfaces of micrometer-wide channels of feldspars might have led to assembly of replicating catalytic biomolecules and perhaps primitive cellular organisms. Silica-rich volcanic glasses should have been abundant on the early Earth, ready for crystallization into zeolites and feldspars, as in present continental basins. Abundant chert from weakly metamorphosed Archaean rocks might retain microscopic clues to the proposed mineral adsorbent/catalysts. Other framework silicas are possible, including ones with laevo/dextro one-dimensional channels. Organic molecules, transition-metal ions, and P occur inside modern feldspars. PMID:9520372

  20. The preparation of BP single crystals by high pressure flux method

    NASA Technical Reports Server (NTRS)

    Kumashiro, Y.; Misawa, S.; Gonda, S.

    1984-01-01

    Single crystals of BP, a III-V compound semiconductor, were obtained by the high pressure flux method. Cu3P and Ni12P5 powders were used as the flux, and mixed with BP powder. Two kinds of mixtures were prepared: (1) 1.8g (BP) + 35 G (Cu3P) and (2) 1.7 g (BP) + 25 g (Ni12P5). They were compressed into pellets, heated at 1300 C for 24 h in an induction furnace under a pressure of 1 MPa using Ar-P2 gas, and slowly cooled to room temperature. In case (1), BP single crystals grew along the (III) plane, and in case (2) they grew as an aggregate of crystallites. The cathodoluminescence spectra of the synthetic BP crystals showed peaks near 680 nm (1.82 eV) for case (1), and 500 nm (2.47 eV) for case (2). By using the high pressure flux method conventional sized crystals were obtained in a relatively short time.