Sample records for vapor-phase materials synthesis

  1. Synthesis of TiO2 Nanoparticles from Ilmenite Through the Mechanism of Vapor-Phase Reaction Process by Thermal Plasma Technology (United States)

    Samal, Sneha


    Synthesis of nanoparticles of TiO2 was carried out by non-transferred arc thermal plasma reactor using ilmenite as the precursor material. The powder ilmenite was vaporized at high temperature in plasma flame and converted to a gaseous state of ions in the metastable phase. On cooling, chamber condensation process takes place on recombination of ions for the formation of nanoparticles. The top-to-bottom approach induces the disintegration of complex ilmenite phases into simpler compounds of iron oxide and titanium dioxide phases. The vapor-phase reaction mechanism was carried out in thermal plasma zone for the synthesis of nanoparticles from ilmenite compound in a plasma reactor. The easy separation of iron particles from TiO2 was taken place in the plasma chamber with deposition of light TiO2 particles at the top of the cooling chamber and iron particles at the bottom. The dissociation and combination process of mechanism and synthesis are studied briefly in this article. The product TiO2 nanoparticle shows the purity with a major phase of rutile content. TiO2 nanoparticles produced in vapor-phase reaction process shows more photo-induced capacity.

  2. Synthesis of polymer nanoparticles via vapor phase deposition onto liquid substrates. (United States)

    Haller, Patrick D; Gupta, Malancha


    In this article, the growth of polymer nanoparticles formed at the liquid-vapor interface via vapor phase polymerization is studied. The particles grow by polymer aggregation, which is driven by the surface tension interaction between the liquid and polymer. It is demonstrated that the mechanism of particle growth is determined by whether polymer particles remain at the liquid-vapor interface or submerge into the liquid. The position of the particles depends on the interaction between the polymer and the liquid. For example, the deposition of poly(n-butyl acrylate) onto poly(dimethyl siloxane) and Krytox liquids leads to the formation of nanoparticles that remain at the liquid-vapor interface. The size of these particles increases as a function of deposition time. The deposition of poly(4-vinylpyridine) onto poly(dimethyl siloxane) and Krytox leads to the formation of nanoparticles that submerge into the liquid. The size of these particles does not significantly change with deposition time. Our study offers a new rapid, one-step synthetic approach for fabricating functional polymer nanoparticles for applications in catalysis, photonics, and drug delivery. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Vapor-Phase Stoichiometry and Heat Treatment of CdTe Starting Material for Physical Vapor Transport (United States)

    Su, Ching-Hua; Sha, Yi-Gao; Lehoczky, S. L.; Liu, Hao-Chieh; Fang, Rei; Brebrick, R. F.


    Six batches of CdTe, having total amounts of material from 99 to 203 g and gross mole fraction of Te, X(sub Te), 0.499954-0.500138, were synthesized from pure Cd and Te elements. The vapor-phase stoichiometry of the assynthesized CdTe batches was determined from the partial pressure of Te2, P(sub Te2) using an optical absorption technique. The measured vapor compositions at 870 C were Te-rich for all of the batches with partial pressure ratios of Cd to Te2, P(sub Cd)/P(sub Te2), ranging from 0.00742 to 1.92. After the heat treatment of baking under dynamic vacuum at 870 C for 8 min, the vapor-phase compositions moved toward that of the congruent sublimation, i.e. P(sub Cd)/P(sub Te2) = 2.0, with the measured P(sub Cd)/P(sub Te2) varying from 1.84 to 3.47. The partial pressure measurements on one of the heat-treated samples also showed that the sample remained close to the congruent sublimation condition over the temperature range 800-880 C.

  4. Solution-free and catalyst-free synthesis of ZnO-based nanostructured TCOs by PED and vapor phase growth techniques (United States)

    Calestani, D.; Pattini, F.; Bissoli, F.; Gilioli, E.; Villani, M.; Zappettini, A.


    Zinc oxide (ZnO) is one of the most promising materials for realizing three-dimensional (3D) nanostructured transparent conducting oxides (TCOs) on large scale, because it is cheap, it can be modified with large concentrations of trivalent elements (such Al, Ga or In) and it is characterized by good electron mobility, wide bandgap and visible-range transparency. But, above all, it can be easily obtained in the form of different nanostructures with a large number of growth techniques. A solution-free and catalyst-free approach has been explored here by the vapor phase synthesis of vertically aligned ZnO nanorods on ZnO:Al (AZO) films grown by pulsed electron deposition (PED). The obtained nanostructured TCOs resulted to be homogeneous on large areas and easily patternable by means of mechanical masks. The morphology, crystalline structure, electrical and optical properties of the obtained samples have been characterized in depth. The possible use of such a nanostructured TCO in excitonic (e.g. DSSC) or low-reflectivity traditional solar cells is discussed.

  5. Metal-Organic Vapor Phase Epitaxial Reactor for the Deposition of Infrared Detector Materials (United States)


    researchers from First Solar in depositing single crystal solar cell materials . A research contract worth over $150K was awarded to RPI b First Solar based contact layers in solar cells . As part of another project funded by Arizona State University/DOE, subcontract from Bay Area Photovoltaic ...II-VI semiconductor layers to further improve the performance of Si solar cells with comparable thickness to HIT structures. We use the installed

  6. Vaporization behavior of non-stoichiometric refractory carbide materials and direct observations of the vapor phase using laser diagnostics

    Energy Technology Data Exchange (ETDEWEB)

    Butt, D.P.; Wantuck, P.J.; Rehse, S.J.; Wallace, T.C. Sr.


    Transition metal and actinide carbides, such as ZrC or NbC and UC or ThC, exhibit a wide range of stoichiometry, and therefore vaporize incongruently. At long times, steady state vaporization can be achieved where relative concentrations of atomic species on solid surface equals that in the gas phase. The surface composition under these steady state conditions is termed the congruently vaporizing composition, (CVC). Modeling the vaporization or corrosion behavior of this dynamic process is complex and requires an understanding of how the surface composition changes with time and a knowledge of CVC, which is both temperature and atmosphere dependent. This paper describes vaporization and corrosion behavior of non-stoichiometric refractory carbide materials and, as an example, describes a thermokinetic model that characterizes the vaporization behavior of the complex carbide U{sub x}Zr{sub 1-x}C{sub y} in hydrogen at 2500 to 3200 K. This model demonstrates that steady state corrosion of U{sub x}Zr{sub l-x}C{sub y} is rate limited by gaseous transport of Zr where partial pressure of Zr is determined by CVC. This paper also briefly describes efforts to image and characterize the vapor phase above the surface of ZrC in static and flowing gas environments using planar laser induced fluorescence. We have developed the method for monitoring and controlling the corrosion behavior of nuclear fuels in nuclear thermal rockets. However, the techniques described can be used, to image boundary layers, and could be used verifying corrosion models.

  7. Synthesis of highly dispersed platinum particles on carbon nanotubes by an in situ vapor-phase method

    Energy Technology Data Exchange (ETDEWEB)

    Mercado-Zúñiga, C. [Depto. Ing. Metalurgia y Materiales, Instituto Politecnico Nacional, Mexico 07300 D.F. (Mexico); Vargas-García, J.R., E-mail: [Depto. Ing. Metalurgia y Materiales, Instituto Politecnico Nacional, Mexico 07300 D.F. (Mexico); Hernández-Pérez, M.A. [Depto. Ing. Metalurgia y Materiales, Instituto Politecnico Nacional, Mexico 07300 D.F. (Mexico); Figueroa-Torres, M.Z. [Depto. Eco-Materiales y Energia, Univ. Autonoma de Nuevo Leon, Nuevo Leon 66450 (Mexico); Cervantes-Sodi, F. [Depto. Fisica y Matematicas, Univ. Iberoamericana, Mexico 01209 D.F. (Mexico); Torres-Martínez, L.M. [Depto. Eco-Materiales y Energia, Univ. Autonoma de Nuevo Leon, Nuevo Leon 66450 (Mexico)


    Highlights: • Highly dispersed Pt nanoparticles were prepared on functionalized carbon nanotubes. • A simple and competitive vapor-phase method was employed. • Carbonyl groups were assumed to be responsible for assisted decomposition of Pt-acac. • Pt particles were highly dispersed because carbonyl groups served as reaction sites. • Particles of 2.3 nm in size were highly dispersed even the high loading (27 wt%Pt). - Abstract: Highly dispersed Pt nanoparticles were prepared on functionalized multi-walled carbon nanotubes (f-MWCNTs) using a simple in situ vapor-phase method. The method consisted in two-step procedure in which an initial mixture of Pt precursor (Pt-acac) and f-MWCNTs was heated in a quartz tube reactor, first at 180 °C and then at 400 °C. Fourier transform infrared spectroscopy (FTIR–ATR), thermal gravimetric analysis (TGA) and X-ray diffraction (XRD) were used to follow the chemical and structural transformations of mixture components during heating steps. The functionalization of MWCNTs with HNO{sub 3}/H{sub 2}SO{sub 4} solution resulted in formation of surface carbonyl groups. The FTIR–ATR and XRD results indicated that individual Pt-acac withstood heating at 180 °C, whereas it was dissociated when heated in contact with f-MWCNTs at the same temperature. Thus, the functional carbonyl groups were found to be responsible for assisted decomposition of Pt-acac at 180 °C. Since carbonyl groups served as reaction sites for decomposition of Pt-acac, the resulting particles were highly and homogeneously dispersed on the surface of MWCNTs even the relatively high metallic loading of 27 wt%. TEM observations revealed that crystalline Pt particles exhibit narrow size distribution with a mean size of 2.3 nm.

  8. Synthesis of Fe3O4/C/TiO2 Magnetic Photocatalyst via Vapor Phase Hydrolysis

    Directory of Open Access Journals (Sweden)

    Fuzhi Shi


    Full Text Available A core/multi-shell-structured Fe3O4/C/TiO2 magnetic photocatalyst is prepared via vapor phase hydrolysis process. The as-synthesized core/multi-shell-structured composite is characterized by X-ray diffraction (XRD, field emission scanning electron microscopy (FE-SEM, transmission electron microscopy (TEM, high-resolution electron microscopy (HRTEM, N2 adsorption-desorption isotherm analyses, vibrating sample magnetometer (VSM, and ultraviolet-visible (UV-Vis absorption spectroscopy. TEM and HRTEM show that well-crystallized anatase TiO2 nanocrystals are immobilized on the surface of as-prepared Fe3O4/C microspheres with dimensions around 200 nm. N2 adsorption-desorption isotherm analysis shows that the obtained photocatalyst exists disorderedly mesoporous structure. The photocatalytic efficiency of the catalyst in degradation of methylene blue is evaluated, and the Fe3O4/C/TiO2 photocatalyst with low TiO2 content (37% has a relatively higher activity than commercial anatase TiO2. The intermediate carbon layer avoids the photodissolution of Fe3O4 effectively, and the recycling property is largely improved due to the existence of magnetic Fe3O4 core.

  9. In situ synthesis of silver nanoparticles on the cotton fabrics modified by plasma induced vapor phase graft polymerization of acrylic acid for durable multifunction

    Energy Technology Data Exchange (ETDEWEB)

    Wang, C.X., E-mail: [College of Textiles and Clothing, Yancheng Institute of Technology, Jiangsu, 224003 (China); Collaborative Innovation Center for Ecological Building, Materials and Environmental Protection Equipments, Jiangsu, 224051 (China); Laboratory for Advanced Technology in Environmental Protection, Jiangsu, 224051 (China); School of Textile and Clothing, Nantong University, Jiangsu, 226019 (China); Ren, Y. [School of Textile and Clothing, Nantong University, Jiangsu, 226019 (China); Lv, J.C.; Zhou, Q.Q.; Ma, Z.P.; Qi, Z.M.; Chen, J.Y.; Liu, G.L.; Gao, D.W. [College of Textiles and Clothing, Yancheng Institute of Technology, Jiangsu, 224003 (China); Lu, Z.Q. [College of Textiles and Clothing, Yancheng Institute of Technology, Jiangsu, 224003 (China); Collaborative Innovation Center for Ecological Building, Materials and Environmental Protection Equipments, Jiangsu, 224051 (China); Laboratory for Advanced Technology in Environmental Protection, Jiangsu, 224051 (China); Zhang, W. [College of Textiles and Clothing, Yancheng Institute of Technology, Jiangsu, 224003 (China); Jin, L.M. [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai, 201204 (China)


    Highlights: • A new means for multifunctional cotton fabrics by PIVPGP of AA and AgNPs synthesis. • Surface modification by PIVPGP of AA had a positive effect on AgNPs loading. • Antibacterial, self-cleaning and thermal stability were greatly improved. • AgNP loaded cotton fabric exhibited excellent laundering durability. • Mechanism of AgNPs in situ synthesis on cotton fabrics by PIVPGP of AA was proposed. - Abstract: A practical and ecological method for preparing the multifunctional cotton fabrics with excellent laundering durability was explored. Cotton fabrics were modified by plasma induced vapor phase graft polymerization (PIVPGP) of acrylic acid (AA) and subsequently silver nanoparticles (AgNPs) were in situ synthesized on the treated cotton fabrics. The AgNP loaded cotton fabrics were characterized by scanning electron microscope (SEM), energy dispersive X-ray (EDX), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), antibacterial activity, self-cleaning activity, thermal stability and laundering durability, respectively. SEM observation and EDX, XPS and XRD analysis demonstrated the much more AgNPs deposition on the cotton fabrics modified by PIVPGP of AA. The AgNP loaded cotton fabrics also exhibited better antibacterial activity, self-cleaning activity, thermal stability and laundering durability. It was concluded that the surface modification of the cotton fabrics by PIVPGP of AA could increase the loading efficiency and binding fastness of AgNPs on the treated cotton fabrics, which could fabricate the cotton fabrics with durable multifunction. In addition, the mechanism of in situ synthesis of AgNPs on the cotton fabrics modified by PIVPGP of AA was proposed.

  10. In situ synthesis of silver nanoparticles on the cotton fabrics modified by plasma induced vapor phase graft polymerization of acrylic acid for durable multifunction (United States)

    Wang, C. X.; Ren, Y.; Lv, J. C.; Zhou, Q. Q.; Ma, Z. P.; Qi, Z. M.; Chen, J. Y.; Liu, G. L.; Gao, D. W.; Lu, Z. Q.; Zhang, W.; Jin, L. M.


    A practical and ecological method for preparing the multifunctional cotton fabrics with excellent laundering durability was explored. Cotton fabrics were modified by plasma induced vapor phase graft polymerization (PIVPGP) of acrylic acid (AA) and subsequently silver nanoparticles (AgNPs) were in situ synthesized on the treated cotton fabrics. The AgNP loaded cotton fabrics were characterized by scanning electron microscope (SEM), energy dispersive X-ray (EDX), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), antibacterial activity, self-cleaning activity, thermal stability and laundering durability, respectively. SEM observation and EDX, XPS and XRD analysis demonstrated the much more AgNPs deposition on the cotton fabrics modified by PIVPGP of AA. The AgNP loaded cotton fabrics also exhibited better antibacterial activity, self-cleaning activity, thermal stability and laundering durability. It was concluded that the surface modification of the cotton fabrics by PIVPGP of AA could increase the loading efficiency and binding fastness of AgNPs on the treated cotton fabrics, which could fabricate the cotton fabrics with durable multifunction. In addition, the mechanism of in situ synthesis of AgNPs on the cotton fabrics modified by PIVPGP of AA was proposed.

  11. Lattice site location of optical centers in GaN:Eu light emitting diode material grown by organometallic vapor phase epitaxy

    KAUST Repository

    Lorenz, K.


    Eu-doped GaN was grown by organometallic vapor phase epitaxy at temperatures from 900 to 1100 °C. Eu incorporation is influenced by temperature with the highest concentration found for growth at 1000 °C. In all samples, Eu is incorporated entirely on substitutional Ga sites with a slight displacement which is highest (∼0.2 Å) in the sample grown at 900 °C and mainly directed along the c-axis. The major optical Eu3+ centers are identical for in situdoped and ion-implanted samples after high temperature and pressure annealing. The dominant Eu3+luminescence lines are attributed to isolated, substitutional Eu.

  12. Alternate methods of applying diffusants to silicon solar cells. [screen printing of thick-film paste materials and vapor phase transport from solid sources (United States)

    Brock, T. W.; Field, M. B.


    Low-melting phosphate and borate glasses were screen printed on silicon wafers and heated to form n and p junctions. Data on surface appearance, sheet resistance and junction depth are presented. Similar data are reported for vapor phase transport from sintered aluminum metaphosphate and boron-containing glass-ceramic solid sources. Simultaneous diffusion of an N(+) layer with screen-printed glass and a p(+) layer with screen-printed Al alloy paste was attempted. No p(+) back surface field formation was achieved. Some good cells were produced but the heating in an endless-belt furnace caused a large scatter in sheet resistance and junction depth for three separate lots of wafers.

  13. Thermodynamic analysis and synthesis of porous Mo{sub 2}C sponge by vapor-phase condensation and in situ carburization of MoO{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Cetinkaya, S. [Istanbul University, Engineering Faculty, Department of Materials and Metallurgical Engineering, Avcilar, Istanbul (Turkey); Eroglu, S., E-mail: [Istanbul University, Engineering Faculty, Department of Materials and Metallurgical Engineering, Avcilar, Istanbul (Turkey)


    Spongy porous MoO{sub 3} deposits were grown by vaporization, vapor-phase transportation and condensation of MoO{sub 3} in Ar flow. It was observed that increased source temperature ({>=}1200 K) and temperature gradient ({>=}100 K/cm) favor the formation of spongy deposit owing to high supersaturation of the oxide vapor at {approx}900 K. Spongy Mo{sub 2}C deposits consisting of intermingled platelet crystals with thin walls were synthesized by in situ carburization of the condensed MoO{sub 3} using 0.05-0.1 mol of CH{sub 4} and 1 mol of H{sub 2} at 900 K. Thermodynamic analysis in the Mo-O-C-H system was used as a guide to predict the conditions for the formation of Mo{sub 2}C from the MoO{sub 3}-CH{sub 4}-H{sub 2} reactants at 900 K. X-ray diffraction analysis showed that the carburized deposits consisted of single phase Mo{sub 2}C, in agreement with the thermodynamic prediction. The equilibrium analysis was also used to reveal possible reaction pathways to Mo{sub 2}C formation from MoO{sub 3}-CH{sub 4}-H{sub 2} reactants which yielded gaseous products of H{sub 2}O, CO{sub 2}, CO, C{sub 2}H{sub 6} and C{sub 2}H{sub 4}.

  14. Vapor phase transformer drying – Part II


    Steeves, Gregory R.


    Vapor phase drying is the most effective method for drying transformer insulation in a manufacturing setting. The process does not lend itself well to transformer drying in the field for a variety of reasons, including the difficulty of removing residual kerosene which can cause a potential change in transformer oil flash point. Several techniques are available for transformer insulation drying in both the field and in manufacturing. Vapor phase drying as part of transformer manufacturing is ...

  15. Vapor phase transformer drying – Part I


    Steeves, Gregory R.


    Vapor phase drying is the most effective method for drying transformer insulation in a manufacturing setting. The process does not lend itself well to transformer drying in the field for a variety of reasons, including the difficulty of removing residual kerosene which can cause a potential change in transformer oil flash point. Several techniques are available for transformer insulation drying in both the field and in manufacturing. Vapor phase drying as part of transformer manufacturing is ...

  16. Vapor phase lubrication of high temperature alloys

    Energy Technology Data Exchange (ETDEWEB)

    Hanyaloglu, B.F.; Graham, E.E.; Oreskovic, T.; Hajj, C.G. [Cleveland State Univ., OH (United States)


    In a previous study, it was found that when a nickel-based superalloy IN750 was heated to high temperatures, a passive layer of aluminum oxide formed on the surface, preventing vapor phase lubrication. In this study, two nickel-chrome-iron alloys and a nickel-copper alloy were studied for high temperature lubrication to see if these alloys, which contained small amounts of aluminum, would exhibit similar behavior. It was found that under static conditions, all three alloys formed a lubricious nodular coating when exposed to a vapor of aryl phosphate. Under dynamic sliding conditions at 500{degrees}C, these alloys were successfully lubricated with a coefficient of friction of 0.1 and no detectable wear. In order to explain these results, a direct correlation between successful vapor phase lubrication and the composition of the alloys containing aluminum has been proposed. If the ratio of copper/aluminum or iron/aluminum is greater that 100 vapor phase, lubrication will be successful. If the ratio is less than 10, a passive aluminum oxide layer will prevent vapor phase lubrication. By selecting alloys with a high iron or copper content, vapor phase lubrication can provide excellent lubrication at high temperatures. 14 refs., 11 figs., 1 tab.

  17. Organometallic vapor-phase epitaxy theory and practice

    CERN Document Server

    Stringfellow, Gerald B


    Here is one of the first single-author treatments of organometallic vapor-phase epitaxy (OMVPE)--a leading technique for the fabrication of semiconductor materials and devices. Also included are metal-organic molecular-beam epitaxy (MOMBE) and chemical-beam epitaxy (CBE) ultra-high-vacuum deposition techniques using organometallic source molecules. Of interest to researchers, students, and people in the semiconductor industry, this book provides a basic foundation for understanding the technique and the application of OMVPE for the growth of both III-V and II-VI semiconductor materials and the

  18. Synthesis and characterization of a liquid Eu precursor (EuCp{sup pm}{sub 2}) allowing for valence control of Eu ions doped into GaN by organometallic vapor phase epitaxy

    Energy Technology Data Exchange (ETDEWEB)

    Mitchell, Brandon, E-mail: [Department of Physics, West Chester University, West Chester, PA, 19383 (United States); Division of Materials and Manufacturing Science, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka, 565-0871 (Japan); Koizumi, Atsushi; Nunokawa, Takumi; Wakamatsu, Ryuta; Lee, Dong-gun; Saitoh, Yasuhisa; Timmerman, Dolf [Division of Materials and Manufacturing Science, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka, 565-0871 (Japan); Kuboshima, Yoshinori; Mogi, Takayuki; Higashi, Shintaro; Kikukawa, Kaoru [Kojundo Chemical Laboratory Co., Ltd., 5-1-28 Chiyoda, Sakado, Saitama, 350-0284 (Japan); Ofuchi, Hironori; Honma, Tetsuo [Japan Synchrotron Radiation Research Institute (JASRI/SPring-8), 1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo, 679-5198 (Japan); Fujiwara, Yasufumi, E-mail: [Division of Materials and Manufacturing Science, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka, 565-0871 (Japan)


    A liquid Eu precursor, bis(normal-propyl-tetramethylcyclopentadienyl)europium has been synthesized. This precursor exists as a liquid at temperatures higher than 49 °C, has a moderately high vapor pressure, contains no oxygen in its molecular structure, and can be distilled to high purity. These properties make it ideal for doping using a chemical vapor or atomic layer deposition method, and provide a degree of control previously unavailable. As a precursor the Eu exists in the divalent valance state, however, once doped into GaN by organometallic vapor phase epitaxy, the room-temperature photoluminescence of the Eu-doped GaN exhibited the typical red emission due to the intra-4f shell transition of trivalent Eu. After variation of the growth temperature, it was found that divalent Eu could be stabilized in the GaN matrix. By tuning the Fermi level through donor doping, the ratio of Eu{sup 2+} to Eu{sup 3+} could be controlled. The change in valence state of the Eu ions was confirmed using X-ray absorption near-edge structure. - Highlights: • A liquid Eu precursor was synthesized and its properties were characterized. • Precursor has a low melting point and a moderately high vapor pressure. • Does not contain oxygen in its molecular structure. • Eu can changed its valance state when incorporated into GaN. • Valence state of Eu in GaN can be controlled by donor doping.

  19. Development of vapor phase hydrogenation and of catalysts immune to poison (abstract)

    Energy Technology Data Exchange (ETDEWEB)


    The development of catalysts immune to poison and the development of vapor-phase hydrogenation were closely connected and they were considered together. Catalysts used at high thruputs and high partial pressures showed rapid deterioration of their activity caused by deposition and condensation of high-molecular-weight substances on the surface of the catalysts. This phenomenon made it necessary to divide hydrogenation into two phases: the liquid phase and the vapor phase. The first of the vapor-phase operating catalysts was catalyst 3510, which consisted of zinc--magnesium molybdate. Development of catalyst 5058, which consisted of pure tungsten disulfide and was produced by decomposing ammonium--sulfotungstate in H/sub 2/ atmosphere, largely terminated development of vapor-phase catalysts. Maximum activity had been obtained. Compared to 3510, two to three times as much gasoline was produced per hour with a fixed volume of catalyst, besides being able to work at a temperature about 100/sup 0/C lower, and gasification losses were considerably smaller. In order to use 5058 in mass production, the dry catalyst powder had to be compressed into cylindrical shapes 10 mm in diameter. The demands for higher antiknock gasolines in the processing of certain paraffinic raw material could not be met by 5058 because of its strong hydrogenation effect, and the dilute catalyst 6434, consisting of 90% Fullers earth treated with HF and 10% WS/sub 2/, was developed for this. 3 tables.

  20. Essentials of inorganic materials synthesis

    CERN Document Server

    Rao, C N R


    This compact handbook describes all the important methods of synthesis employed today for synthesizing inorganic materials. Some features: Focuses on modern inorganic materials with applications in nanotechnology, energy materials, and sustainability Synthesis is a crucial component of materials science and technology; this book provides a simple introduction as well as an updated description of methods Written in a very simple style, providing references to the literature to get details of the methods of preparation when required

  1. Tunnel Junction Development Using Hydride Vapor Phase Epitaxy

    Energy Technology Data Exchange (ETDEWEB)

    Ptak, Aaron J [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Simon, John D [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Schulte, Kevin L [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Jain, Nikhil [National Renewable Energy Laboratory (NREL), Golden, CO (United States)


    We demonstrate for the first time III-V tunnel junctions grown using hydride vapor phase epitaxy (HVPE) with peak tunneling currents >8 A/cm2, sufficient for operation of a multijunction device to several hundred suns of concentration. Multijunction solar cells rely on tunneling interconnects between subcells to enable series connection with minimal voltage loss, but tunnel junctions have never been shown using the HVPE growth method. HVPE has recently reemerged as a low-cost growth method for high-quality III-V materials and devices, including the growth of high-efficiency III-V solar cells. We previously showed single-junction GaAs solar cells with conversion efficiencies of ~24% with a path forward to equal or exceed the practical efficiency limits of crystalline Si. Moving to a multijunction device structure will allow for even higher efficiencies with minimal impact on cost, necessitating the development of tunnel interconnects. Here, we demonstrate the performance of both isolated HVPE-grown tunnel junctions, as well as single-junction GaAs solar cell structures with a tunnel junction incorporated into the contact region. We observe no degradation in device performance compared to a structure without the added junction.

  2. The liquid to vapor phase transition in excited nuclei

    Energy Technology Data Exchange (ETDEWEB)

    Elliott, J.B.; Moretto, L.G.; Phair, L.; Wozniak, G.J.; Beaulieu, L.; Breuer, H.; Korteling, R.G.; Kwiatkowski, K.; Lefort, T.; Pienkowski, L.; Ruangma, A.; Viola, V.E.; Yennello, S.J.


    For many years it has been speculated that excited nuclei would undergo a liquid to vapor phase transition. For even longer, it has been known that clusterization in a vapor carries direct information on the liquid-vapor equilibrium according to Fisher's droplet model. Now the thermal component of the 8 GeV/c pion + 197 Au multifragmentation data of the ISiS Collaboration is shown to follow the scaling predicted by Fisher's model, thus providing the strongest evidence yet of the liquid to vapor phase transition.

  3. Hybrid vapor phase-solution phase growth techniques for improved CZT(S,Se) photovoltaic device performance

    Energy Technology Data Exchange (ETDEWEB)

    Chang, Liang-Yi; Gershon, Talia S.; Haight, Richard A.; Lee, Yun Seog


    A hybrid vapor phase-solution phase CZT(S,Se) growth technique is provided. In one aspect, a method of forming a kesterite absorber material on a substrate includes the steps of: depositing a layer of a first kesterite material on the substrate using a vapor phase deposition process, wherein the first kesterite material includes Cu, Zn, Sn, and at least one of S and Se; annealing the first kesterite material to crystallize the first kesterite material; and depositing a layer of a second kesterite material on a side of the first kesterite material opposite the substrate using a solution phase deposition process, wherein the second kesterite material includes Cu, Zn, Sn, and at least one of S and Se, wherein the first kesterite material and the second kesterite material form a multi-layer stack of the absorber material on the substrate. A photovoltaic device and method of formation thereof are also provided.

  4. Vapor phase growth of functional pentacene films at atmospheric pressure

    NARCIS (Netherlands)

    Rolin, C.; Vasseur, K.; Niesen, B.; Willegems, M.; Müller, R.; Steudel, S.; Genoe, J.; Heremans, P.


    Compared to traditional vacuum evaporation techniques for small organic molecules, organic vapor phase deposition (OVPD) possesses a extra processing parameter: the pressure of process gas Pch. Here, the influence of large Pch variations (from 0.1 mbar to atmospheric pressure) on pentacene thin film

  5. Low temperature vapor phase digestion of graphite

    Energy Technology Data Exchange (ETDEWEB)

    Pierce, Robert A.


    A method for digestion and gasification of graphite for removal from an underlying surface is described. The method can be utilized to remove graphite remnants of a formation process from the formed metal piece in a cleaning process. The method can be particularly beneficial in cleaning castings formed with graphite molding materials. The method can utilize vaporous nitric acid (HNO.sub.3) or vaporous HNO.sub.3 with air/oxygen to digest the graphite at conditions that can avoid damage to the underlying surface.

  6. Ferroic materials synthesis and applications

    CERN Document Server

    Virk, Hardev Singh


    Ferroics is the generic name given to the study of ferromagnets, ferroelectrics, and ferroelastics. The basis of this study is to understand the large changes in physical characteristics that occur over a very narrow temperature range. In recent years, a new class of ferroic materials has been attracting increased interest. These multiferroics exhibit more than one ferroic property simultaneously in a single phase. The present volume: ""Ferroic Materials: Synthesis and Applications"" has ten Chapters, spread over areas as diverse as Magnetic Oxide Nanomaterials, Ferrites Synthesis, Hexaferrite

  7. Synthesis of Energetic Materials. (United States)


    of the diazabicyclooctanes 11 and 12. The starting materials in this work were gbtained by the reaction of c-anogen with sodio diethylmalonate to give...effortto find routes which would lead to 11 and 12. Catalytic hydrogenation of 27 gave the doy~le lactam 28. The sodio derivative 26 was methylated to

  8. Assessment of radionuclide vapor-phase transport in unsaturated tuff

    Energy Technology Data Exchange (ETDEWEB)

    Smith, D.M.; Updegraff, C.D.; Bonano, E.J.; Randall, J.D.


    This report describes bounding calculations performed to investigate the possibility of radionuclide migration in a vapor phase associated with the emplacement of high-level waste canister in unsaturated tuff formations. Two potential radionuclide transport mechanisms in the vapor phase were examined: aerosol migration and convection/diffusion of volatile species. The former may have significant impact on the release of radionuclides to the accessible environment as the concentration in the aerosols will be equal to that in the ground water. A conservative analysis of air diffusion in a stagnant liquid film indicated that for all expected repository conditions, aerosol formation is not possible. The migration of volatile species was examined both in the vicinity of a waste canister and outside the thermally disturbed zone. Two-dimensional (radial) and three-dimensional (radial-vertical) coupled heat transfer-gas flow-liquid flow simulations were performed using the TOUGH computer code. The gas flow rate relative to the liquid flow rate predicted from the simulations allowed calculations of mobility ratios due to convection which led to the conclusion that, except for the immediate region near the canister, transport in the liquid phase will be dominant for radionuclides heavier than radon. Near the waste canister, iodine transport may also be important in the vapor phase. Bounding calculations for vertical mobility ratios were carried out as a function of saturation. These calculations are conservative and agree well with the two-dimensional simulations. Based on this analysis, it is clear that vapor-phase transport will not be important for radionuclides such as cesium and heavier species. Vapor transport for iodine may play a role in the overall release scenario depending on the particular repository conditions.

  9. Synthesis of chiral polyaniline films via chemical vapor phase polymerization

    DEFF Research Database (Denmark)

    Chen, J.; Winther-Jensen, B.; Pornputtkul, Y.


    methods, such as cyclic voltammetry (CV), UV- vis spectroscopy, four- point probe conductivity measurement, Raman spectroscopy, circular dichroism spectroscopy, and scanning electron microscopy. The polyaniline films grown by this method not only showed high electrochemical activity, supported by CV...

  10. Synthesis of new nanocrystal materials (United States)

    Hassan, Yasser Hassan Abd El-Fattah

    Colloidal semiconductor nanocrystals (NCs) have sparked great excitement in the scientific community in last two decades. NCs are useful for both fundamental research and technical applications in various fields owing to their size and shape-dependent properties and their potentially inexpensive and excellent chemical processability. These NCs are versatile fluorescence probes with unique optical properties, including tunable luminescence, high extinction coefficient, broad absorption with narrow photoluminescence, and photobleaching resistance. In the past few years, a lot of attention has been given to nanotechnology based on using these materials as building blocks to design light harvesting assemblies. For instant, the pioneering applications of NCs are light-emitting diodes, lasers, and photovoltaic devices. Synthesis of the colloidal stable semiconductor NCs using the wet method of the pyrolysis of organometallic and chalcogenide precursors, known as hot-injection approach, is the chart-topping preparation method in term of high quality and monodisperse sized NCs. The advancement in the synthesis of these artificial materials is the core step toward their applications in a broad range of technologies. This dissertation focuses on exploring various innovative and novel synthetic methods of different types of colloidal nanocrystals, both inorganic semiconductors NCs, also known as quantum dots (QDs), and organic-inorganic metal halide-perovskite materials, known as perovskites. The work presented in this thesis focuses on pursuing fundamental understanding of the synthesis, material properties, photophysics, and spectroscopy of these nanostructured semiconductor materials. This thesis contains 6 chapters and conclusions. Chapters 1?3 focus on introducing theories and background of the materials being synthesized in the thesis. Chapter 4 demonstrates our synthesis of colloidal linker--free TiO2/CdSe NRs heterostructures with CdSe QDs grown in the presence of Ti

  11. Modeling of Gallium Nitride Hydride Vapor Phase Epitaxy (United States)

    Meyyappan, Meyya; Arnold, James O. (Technical Monitor)


    A reactor model for the hydride vapor phase epitaxy of GaN is presented. The governing flow, energy, and species conservation equations are solved in two dimensions to examine the growth characteristics as a function of process variables and reactor geometry. The growth rate varies with GaCl composition but independent of NH3 and H2 flow rates. A change in carrier gas for Ga source from H2 to N2 affects the growth rate and uniformity for a fixed reactor configuration. The model predictions are in general agreement with observed experimental behavior.

  12. A Kinetic Model for GaAs Growth by Hydride Vapor Phase Epitaxy

    Energy Technology Data Exchange (ETDEWEB)

    Schulte, Kevin L.; Simon, John; Jain, Nikhil; Young, David L.; Ptak, Aaron J.


    Precise control of the growth of III-V materials by hydride vapor phase epitaxy (HVPE) is complicated by the fact that the growth rate depends on the concentrations of nearly all inputs to the reactor and also the reaction temperature. This behavior is in contrast to metalorganic vapor phase epitaxy (MOVPE), which in common practice operates in a mass transport limited regime where growth rate and alloy composition are controlled almost exclusively by flow of the Group III precursor. In HVPE, the growth rate and alloy compositions are very sensitive to temperature and reactant concentrations, which are strong functions of the reactor geometry. HVPE growth, particularly the growth of large area materials and devices, will benefit from the development of a growth model that can eventually be coupled with a computational fluid dynamics (CFD) model of a specific reactor geometry. In this work, we develop a growth rate law using a Langmuir-Hinshelwood (L-H) analysis, fitting unknown parameters to growth rate data from the literature that captures the relevant kinetic and thermodynamic phenomena of the HVPE process. We compare the L-H rate law to growth rate data from our custom HVPE reactor, and develop quantitative insight into reactor performance, demonstrating the utility of the growth model.

  13. MEMS Lubrication by In-Situ Tribochemical Reactions From the Vapor Phase.

    Energy Technology Data Exchange (ETDEWEB)

    Dugger, Michael Thomas; Asay, David B.; Kim, Seong H.


    Vapor Phase Lubrication (VPL) of silicon surfaces with pentanol has been demonstrated. Two potential show stoppers with respect to application of this approach to real MEMS devices have been investigated. Water vapor was found to reduce the effectiveness of VPL with alcohol for a given alcohol concentration, but the basic reaction mechanism observed in water-free environments is still active, and devices operated much longer in mixed alcohol and water vapor environments than with chemisorbed monolayer lubricants alone. Complex MEMS gear trains were successfully lubricated with alcohol vapors, resulting in a factor of 104 improvement in operating life without failure. Complex devices could be made to fail if operated at much higher frequencies than previously used, and there is some evidence that the observed failure is due to accumulation of reaction products at deeply buried interfaces. However, if hypothetical reaction mechanisms involving heated surfaces are valid, then the failures observed at high frequency may not be relevant to operation at normal frequencies. Therefore, this work demonstrates that VPL is a viable approach for complex MEMS devices in conventional packages. Further study of the VPL reaction mechanisms are recommended so that the vapor composition may be optimized for low friction and for different substrate materials with potential application to conventionally fabricated, metal alloy parts in weapons systems. Reaction kinetics should be studied to define effective lubrication regimes as a function of the partial pressure of the vapor phase constituent, interfacial shear rate, substrate composition, and temperature.

  14. Mechanistic investigation of non-ideal sorption behavior in natural organic matter. 1. Vapor phase equilibrium. (United States)

    Bell, Katherine Young; Leboeuf, Eugene J


    Results from an experimental and modeling investigation of the influence of thermodynamic properties of highly purified natural organic matter (NOM) on observed equilibrium sorption/desorption behaviors of vapor phase trichloroethylene (TCE) is presented. Identification of glass transition (T(g)) behavior in Leonardite humic acid and Organosolv lignin enabled evaluation of equilibrium and nonequilibrium sorption behavior in glassy and rubbery NOM. Specific differences in vapor phase equilibrium behavior in NOM above and below their T(g) were identified. In the glassy state (below T(g)), sorption of TCE is well-described by micropore models, with enthalpies of sorption characteristic of microporous, glassy macromolecules. Above T(g), sorptive behavior was well-described by Flory-Huggins theory, indicating that the mobility and structural configuration of rubbery NOM materials may be analogous to the characteristic sorption behavior observed in more mobile, rubbery macromolecules, including strong entropic changes during sorption. Results from this work provide further support that, at least for the samples employed in this study, NOM possesses macromolecular characteristics which display sorption behavior similar to synthetic macromolecules-an important assumption in conceptual sorption equilibrium models used in the analysis of the fate and transport of VOCs in the environment.

  15. Vapor phase deposition of functional polymers onto paper-based microfluidic devices for advanced unit operations. (United States)

    Kwong, Philip; Gupta, Malancha


    Paper-based microfluidic devices have recently received significant attention as a potential platform for low-cost diagnostic assays. However, the number of advanced unit operations, such as separation of analytes and fluid manipulation, that can be applied to these devices has been limited. Here, we use a vapor phase polymerization process to sequentially deposit functional polymer coatings onto paper-based microfluidic devices to integrate multiple advanced unit operations while retaining the fibrous morphology necessary to generate capillary-driven flow. A hybrid grafting process was used to apply hydrophilic polymer coatings with a high surface concentration of ionizable groups onto the surface of the paper fibers in order to passively separate analytes, which allowed a multicomponent mixture to be separated into its anionic and cationic components. Additionally, a UV-responsive polymer was sequentially deposited to act as a responsive switch to control the path of fluid within the devices. This work extends the advanced unit operations available for paper-based microfluidics and allows for more complex diagnostics. In addition, the vapor phase polymerization process is substrate independent, and therefore, these functional coatings can be applied to other textured materials such as membranes, filters, and fabrics.

  16. Vapor-phase fabrication and properties of continuous-filament ceramic composites. (United States)

    Besmann, T M; Sheldon, B W; Lowden, R A; Stinton, D P


    The continuous-filament ceramic composite is becoming recognized as necessary for new, high-temperature structural applications. Yet because of the susceptibility of the filaments to damage from traditional methods for the preparation of ceramics, vapor-phase infiltration has become the fabrication method of choice. The chemical vapor infiltration methods for producing these composites are now being studied in earnest, with the complexity of filament weaves and deposition chemistry being merged with standard heat and mass-transport relationships. Two of the most influential effects on the mechanical properties of these materials are the adhesion and frictional force between the fibers and the matrix, which can be controlled by a tailored interface coating. A variety of materials are available for producing these composites including carbide, nitride, boride, and oxide filaments and matrices. Silicon carbide-based materials are by far the most advanced and are already being used in aerospace applications.

  17. Field demonstration of vapor phase TCE bioreactor. Final report

    Energy Technology Data Exchange (ETDEWEB)



    The objective of this Cooperative Research and Development Agreement (CRADA), was to demonstrate the effectiveness of a vapor-phase bioreactor system for the destruction of trichloroethylene (TCE) from contaminated groundwater. A field demonstration was per-formed using groundwater at the Oak Ridge K-25 Site contaminated with a complex mixture of organic chemicals. This site is managed and operated by Martin Marietta Energy Systems, Inc. for the Department of Energy (DOE). Analysis of the data generated during the test can be summarized in three major observations. First, TCE was degraded in the presence of all the organics found in the steam strip condensate. This was observed during treatment of both the steam strip condensate and condensate amended with TCE to increase its concentration relative to the other components. The conclusion that TCE was being biodegraded was supported by performing mass balance control experiments with the reactor and by tracking recalcitrant chemicals also present in the steam stripper condensate. Second, there appeared to be an initial lag period of up to 24 hours before onset of TCE degradation in the reactor. The source of this lag was not determined but could be related to either an acclimation of the microorganisms to other chemicals found in the condensate or reversible inhibitory effects on TCE degradation. The duration of TCE degradative activity was relatively short for only 2 to 5 days. compared to previous demonstrations where TCE was the sole contaminant. However, several of the runs were interrupted due to mechanical and not biological issues. Third, other chemical contaminants were also degraded. by the bacteria used in the vapor phase reactor which is consistent with previous work performed both at ENVIROGEN and elsewhere.

  18. Halogen-free vapor phase epitaxy for high-rate growth of GaN bulk crystals (United States)

    Nakamura, Daisuke; Kimura, Taishi; Horibuchi, Kayo


    Here, we propose a halogen-free vapor phase epitaxy (HF-VPE) technique to grow bulk GaN single crystals. This technique employs the simplest reaction for GaN synthesis (reaction of Ga vapor with NH3) and can potentially achieve a high growth rate, a prolonged growth duration, a high crystal quality, and a low cost. The analyses of thick HF-VPE-GaN layers grown under optimized growth conditions revealed that high-quality crystals, both in terms of dislocation density and impurity concentration, are obtained at high growth rates of over 100 µm/h.

  19. Vapor phase elemental sulfur amendment for sequestering mercury in contaminated soil (United States)

    Looney, Brian B.; Denham, Miles E.; Jackson, Dennis G.


    The process of treating elemental mercury within the soil is provided by introducing into the soil a heated vapor phase of elemental sulfur. As the vapor phase of elemental sulfur cools, sulfur is precipitated within the soil and then reacts with any elemental mercury thereby producing a reaction product that is less hazardous than elemental mercury.

  20. Genetic Synthesis of Periodic Protein Materials


    Fournier, M J; Creel, H. S.; Krejchi, M. T.; Mason, T L; Tirrell, D.A.; McGrath, K. P.; Atkins, E. D. T.


    Genetic engineering offers a novel approach to the development of advanced polymeric materials, in particular protein-based materials. Biological synthesis provides levels of control of polymer chain architecture that cannot yet be attained by current methods of chemical synthesis. In addition to employing naturally occurring genetic templates artificial genes can be designed to encode completely new materials with customized properties. In the present paper we: 1) review th...

  1. Protein purification with vapor-phase carbon dioxide. (United States)

    Winters, M A; Frankel, D Z; Debenedetti, P G; Carey, J; Devaney, M; Przybycien, T M


    Gaseous CO2 was used as an antisolvent to induce the fractional precipitation of alkaline phosphatase, insulin, lysozyme, ribonuclease, trypsin, and their mixtures from dimethylsulfoxide (DMSO). Compressed CO2 was added continuously and isothermally to stationary DMSO solutions (gaseous antisolvent, GAS). Dissolution of CO2 was accompanied by a pronounced, pressure-dependent volumetric expansion of DMSO and a consequent reduction in solvent strength of DMSO towards dissolved proteins. View cell experiments were conducted to determine the pressures at which various proteins precipitate from DMSO. The solubility of each protein in CO2-expanded DMSO was different, illustrating the potential to separate and purify proteins using gaseous antisolvents. Polyacrylamide gel electrophoresis in sodium dodecyl sulfate (SDS-PAGE) was used to quantify the separation of lysozyme from ribonuclease, alkaline phosphatase from insulin, and trypsin from catalase. Lysozyme biological activity assays were also performed to determine the composition of precipitates from DMSO initially containing lysozyme and ribonuclease. SDS-PAGE characterizations suggest that the composition and purity of solid-phase precipitated from a solution containing multiple proteins may be accurately controlled through the antisolvent's pressure. Insulin, lysozyme, ribonuclease, and trypsin precipitates recovered substantial amounts of biological activity upon redissolution in aqueous media. Alkaline phosphatase, however, was irreversibly denaturated. Vapor-phase antisolvents, which are easily separated and recovered from proteins and liquid solvents upon depressurization, appear to be a reliable and effective means of selectively precipitating proteins. Copyright 1999 John Wiley & Sons, Inc.

  2. Quantum materials discovery from a synthesis perspective (United States)

    Samarth, Nitin


    The synthesis of bulk crystals, thin films and nanostructures plays a seminal role in expanding the frontiers of quantum materials. Crystal growers accomplish this by creating materials aimed at harnessing the complex interplay between quantum wavefunctions and various factors such as dimensionality, topology, Coulomb interactions and symmetry. This Review provides a synthesis perspective on how this discovery of quantum materials takes place. After introducing the general paradigms that arise in this context, we provide a few examples to illustrate how thin-film growers in particular exploit quantum confinement, topology, disorder and interfacial heterogeneity to realize new quantum materials.

  3. Vapor-Phase Free Radical Polymerization in the Presence of Ionic Liquids (United States)

    Gupta, Malancha


    Ionic liquids (ILs) have recently attracted significant interest as an environmentally-friendly alternative to traditional volatile organic solvents because ILs are non-volatile, non-flammable, and can be easily recycled. ILs can be exploited in many ways to improve the selectivity and kinetics of chemical reactions, including polymer synthesis. Ionic liquids have negligible vapor pressure and are therefore stable under vacuum. A few studies have investigated ILs as substrates in inorganic vacuum deposition processes, but to our knowledge ILs have not been used in vapor phase polymerization systems. We have recently introduced ionic liquids into the initiated chemical vapor deposition (iCVD) process for the first time. The iCVD polymerization process occurs via a free-radical mechanism, and the deposited polymeric films are compositionally analogous to solution-phase polymers. Despite the wide range of polymers that have been synthesized using iCVD, it has proven difficult to polymerize monomers with low surface concentrations such as styrene and low propagation rates such as methyl methacrylate and it is difficult to produce block copolymers. In this talk, we will show that our novel ILiCVD system can address some of these shortcomings. We will explain the effects of deposition time, temperature, and monomer solubility on the morphology of the polymer and the molecular weight of the polymer chains.

  4. Hydroxylation of phenol over MeAPO molecular sieves synthesized by vapor phase transport (United States)

    Shao, Hui; Chen, Jingjing; Chen, Xia; Leng, Yixin; Zhong, Jing


    In this study, MeAPO-25 (Me = Fe, Cu, Mn) molecular sieves were first synthesized by a vapor phase transport method using tetramethyl guanidine as the template and applied to hydroxylation of phenol. The zeolites were characterized by XRD, SEM, FT-IR, and DR UV-Vis. As a result, MeAPO-21 and MeAPO-15 were synthesized by changing the Me/Al ratio. UV-Visible diffuse reflectance study suggested incorporation of heteroatoms into the framework and FT-IR study also supported these data. Effects of heteroatoms, contents of Me in MeAPO-25, reaction temperature, phenol/H2O2 mole ratios, reaction time and concentration of catalyst on the conversion of phenol, as well as on the selectivity were studied. FeAPO-25 exhibited a high catalytic activity at the mole ratio of FeO and Al2O3 equal to 0.1 in the synthesis gel, giving the phenol conversion of 88.75% and diphenols selectivity of 66.23% at 60°C within 3 h [ n(phenol)/ n(H2O2) = 0.75, m(FeAPO-25)/ m(phenol) = 7.5%]. Experimental results indicated that the FeAPO-25 molecular sieve was a fairly promising candidate for the application in hydroxylation of phenol.

  5. Melt-vapor phase transition in the lead-selenium system at atmospheric and low pressure (United States)

    Volodin, V. N.; Burabaeva, N. M.; Trebukhov, S. A.


    The boiling temperature and the corresponding vapor phase composition in the existence domain of liquid solutions were calculated from the partial pressures of saturated vapor of the components and lead selenide over liquid melts in the lead-selenium system. The phase diagram was complemented with the liquid-vapor phase transition at atmospheric pressure and in vacuum of 100 Pa, which allowed us to judge the behavior of the components during the distillation separation.

  6. Radiation synthesis of materials and compounds

    CERN Document Server

    Kharisov, Boris Ildusovich; Ortiz Méndez, Ubaldo


    Researchers and engineers working in nuclear laboratories, nuclear electric plants, and elsewhere in the radiochemical industries need a comprehensive handbook describing all possible radiation-chemistry interactions between irradiation and materials, the preparation of materials under distinct radiation types, the possibility of damage of materials under irradiation, and more. Radiation nanotechnology is still practically an undeveloped field, except for some achievements in the fabrication of metallic nanoparticles under ionizing flows. Radiation Synthesis of Materials and Compounds presents the state of the art of the synthesis of materials, composites, and chemical compounds, and describes methods based on the use of ionizing radiation. It is devoted to the preparation of various types of materials (including nanomaterials) and chemical compounds using ionizing radiation (alpha particles, beta particles, gamma rays, x-rays, and neutron, proton, and ion beams). The book presents contributions from leaders ...

  7. Inorganic materials synthesis in ionic liquids

    Directory of Open Access Journals (Sweden)

    Christoph Janiak


    Full Text Available The field of "inorganic materials from ionic liquids" (ILs is a young and dynamically growing research area for less than 10 years. The ionothermal synthesis in ILs is often connected with the preparation of nanomaterials, the use of microwave heating and in part also ultrasound. Inorganic material synthesis in ILs allows obtaining phases which are not accessible in conventional organic or aqueous solvents or with standard methods of solid-state chemistry or under such mild conditions. Cases at hand include "ligand-free" metal nanoparticles without added stabilizing capping ligands, inorganic or inorganic-organic hybrid solid-state compounds, large polyhedral clusters and exfoliated graphene from low-temperature synthesis. There are great expectations that ILs open routes towards new, possibly unknown, inorganic materials with advantageous properties that cannot (or only with great difficulty be made via conventional processes.

  8. Combinatorial synthesis of inorganic or composite materials (United States)

    Goldwasser, Isy; Ross, Debra A.; Schultz, Peter G.; Xiang, Xiao-Dong; Briceno, Gabriel; Sun, Xian-Dong; Wang, Kai-An


    Methods and apparatus for the preparation and use of a substrate having an array of diverse materials in predefined regions thereon. A substrate having an array of diverse materials thereon is generally prepared by delivering components of materials to predefined regions on a substrate, and simultaneously reacting the components to form at least two materials or, alternatively, allowing the components to interact to form at least two different materials. Materials which can be prepared using the methods and apparatus of the present invention include, for example, covalent network solids, ionic solids and molecular solids. More particularly, materials which can be prepared using the methods and apparatus of the present invention include, for example, inorganic materials, intermetallic materials, metal alloys, ceramic materials, organic materials, organometallic materials, nonbiological organic polymers, composite materials (e.g., inorganic composites, organic composites, or combinations thereof), etc. Once prepared, these materials can be screened for useful properties including, for example, electrical, thermal, mechanical, morphological, optical, magnetic, chemical, or other properties. Thus, the present invention provides methods for the parallel synthesis and analysis of novel materials having useful properties.

  9. High Growth Rate Hydride Vapor Phase Epitaxy at Low Temperature through Use of Uncracked Hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Schulte, Kevin L [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Simon, John D [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Ptak, Aaron J [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Braun, Anna [Rose-Hulman Institute of Technology


    We demonstrate hydride vapor phase epitaxy (HVPE) of GaAs with unusually high growth rates (RG) at low temperature and atmospheric pressure by employing a hydride-enhanced growth mechanism. Under traditional HVPE growth conditions that involve growth from Asx species, RG exhibits a strong temperature dependence due to slow kinetics at the surface, and growth temperatures >750 degrees C are required to obtain RG > 60 um/h. We demonstrate that when the group V element reaches the surface in a hydride, the kinetic barrier is dramatically reduced and surface kinetics no longer limit RG. In this regime, RG is dependent on mass transport of uncracked AsH3 to the surface. By controlling the AsH3 velocity and temperature profile of the reactor, which both affect the degree of AsH3 decomposition, we demonstrate tuning of RG. We achieve RG above 60 um/h at temperatures as low as 560 degrees C and up to 110 um/h at 650 degrees C. We incorporate high-RG GaAs into solar cell devices to verify that the electronic quality does not deteriorate as RG is increased. The open circuit voltage (VOC), which is a strong function of non-radiative recombination in the bulk material, exhibits negligible variance in a series of devices grown at 650 degrees C with RG = 55-110 um/h. The implications of low temperature growth for the formation of complex heterostructure devices by HVPE are discussed.

  10. Radiation-induced defects in GaN bulk grown by halide vapor phase epitaxy

    Energy Technology Data Exchange (ETDEWEB)

    Duc, Tran Thien; Pozina, Galia; Son, Nguyen Tien; Janzén, Erik; Hemmingsson, Carl [Department of Physics, Chemistry and Biology (IFM), Linköping University, S-581 83 Linköping (Sweden); Ohshima, Takeshi [Japan Atomic Energy Agency (JAEA), Takasaki, Gunma 370-1292 (Japan)


    Defects induced by electron irradiation in thick free-standing GaN layers grown by halide vapor phase epitaxy were studied by deep level transient spectroscopy. In as-grown materials, six electron traps, labeled D2 (E{sub C}–0.24 eV), D3 (E{sub C}–0.60 eV), D4 (E{sub C}–0.69 eV), D5 (E{sub C}–0.96 eV), D7 (E{sub C}–1.19 eV), and D8, were observed. After 2 MeV electron irradiation at a fluence of 1 × 10{sup 14 }cm{sup −2}, three deep electron traps, labeled D1 (E{sub C}–0.12 eV), D5I (E{sub C}–0.89 eV), and D6 (E{sub C}–1.14 eV), were detected. The trap D1 has previously been reported and considered as being related to the nitrogen vacancy. From the annealing behavior and a high introduction rate, the D5I and D6 centers are suggested to be related to primary intrinsic defects.

  11. Sulfidic vapor phase catalysts, especially tungsten sulfide, in industrial coal hydrogenation

    Energy Technology Data Exchange (ETDEWEB)

    Pier, M.


    The historical development of high-pressure processes of the I. G. Farbenindustrie, from ammonia through methanol and gasoline, and the special case of gasoline production with a fixed-bed catalyst (tungsten sulfide) were discussed. The preparation, properties, and uses of this versatile catalyst were discussed, but it was emphasized that with the sotrmy development of the process, a condition which still existed at the time of this report, and with a great number of practical problems to solve, no extensive study of basic facts had ben possible. This tungsten sulfide catalyst was an especially active vapor-phase catalyst which operated at lower temperatures than the molybdenum catalysts formerly used. It also permitted higher thruputs, even with the oils from bituminous coal that were difficult to split. For certain uses, such as the improvement of the antiknock properties or the saving in tungsten, it was strongly diluted. Studies on using up sulfur in the tungsten sulfide catalyst were in progress at this time and showed there was practically no reduction of it under the conditions of hydrogenation under pressure as long as the raw material contained sulfur.

  12. A semi-empirical model for the complete orientation dependence of the growth rate for vapor phase epitaxy - Chloride VPE of GaAs (United States)

    Seidel-Salinas, L. K.; Jones, S. H.; Duva, J. M.


    A semi-empirical model has been developed to determine the complete crystallographic orientation dependence of the growth rate for vapor phase epitaxy (VPE). Previous researchers have been able to determine this dependence for a limited range of orientations; however, our model yields relative growth rate information for any orientation. This model for diamond and zincblende structure materials is based on experimental growth rate data, gas phase diffusion, and surface reactions. Data for GaAs chloride VPE is used to illustrate the model. The resulting growth rate polar diagrams are used in conjunction with Wulff constructions to simulate epitaxial layer shapes as grown on patterned substrates. In general, this model can be applied to a variety of materials and vapor phase epitaxy systems.

  13. Synthesis and characterization of innovative insulation materials

    Directory of Open Access Journals (Sweden)

    Skaropoulou Aggeliki


    Full Text Available Insulation elements are distinguished in inorganic fibrous and organic foamed materials. Foamed insulation materials are of great acceptance and use, but their major disadvantage is their flammability. In case of fire, they tend to transmit the flame producing toxic gases. In this paper, the synthesis and characterization of innovative inorganic insulation materials with properties competitive to commercial is presented. Their synthesis involves the mixing of inorganic raw material and water with reinforcing agent or/and foaming agent leading to the formation of a gel. Depending on raw materials nature, the insulation material is produced by freeze drying or ambient drying techniques of the gel. The raw material used are chemically benign and abundantly available materials, or industrial by-products and the final products are non-toxic and, in some cases, non-flammable. Their density and thermal conductivity was measured and found 0.02-0.06 g/cm3 and 0.03-0.04 W/mK, respectively.

  14. Combustion Synthesis of Energy Storage Materials (United States)

    Eagle, W. Ethan; Wooldridge, Margaret


    Advancement in the understanding of state of charge and efficiency requires better coupling of battery level properties with the micro-structure of the constituents. The composition of the target synthesis material, lithium manganese oxide (Li Mn2O4, or LMO for short) is known to impact lithium ion battery properties. Following this motivation, our aim is to demonstrate control over the microstructure and compositional properties of LMO using parameters of the combustion synthesis environment. In this experiment, one or both solid phase precursors, lithium acetate-hydrate and manganse acetate-hydrate, were aerosolized and delivered to a hydrogen-oxygen Henken burner at atmospheric pressure. The characteristic time scales for reaction and flow control the synthesis process. Controlling reactant concentrations targets changes in nanoparticle composition and flow rate controls residence times and synthesis temperatures. To explore the effects of composition, first lithium oxide (Li2O) and manganese oxide (Mn2O2) powders are generated independently from the corresponding acetate precursors. Following that, several mixtures of lithium and manganese acetate precursor trials were conducted and the resulting material properties were investigated using TEM and XRD.

  15. Aluminum Nitride Micro-Channels Grown via Metal Organic Vapor Phase Epitaxy for MEMs Applications

    Energy Technology Data Exchange (ETDEWEB)

    Rodak, L.E.; Kuchibhatla, S.; Famouri, P.; Ting, L.; Korakakis, D.


    Aluminum nitride (AlN) is a promising material for a number of applications due to its temperature and chemical stability. Furthermore, AlN maintains its piezoelectric properties at higher temperatures than more commonly used materials, such as Lead Zirconate Titanate (PZT) [1, 2], making AlN attractive for high temperature micro and nanoelectromechanical (MEMs and NEMs) applications including, but not limited to, high temperature sensors and actuators, micro-channels for fuel cell applications, and micromechanical resonators. This work presents a novel AlN micro-channel fabrication technique using Metal Organic Vapor Phase Epitaxy (MOVPE). AlN easily nucleates on dielectric surfaces due to the large sticking coefficient and short diffusion length of the aluminum species resulting in a high quality polycrystalline growth on typical mask materials, such as silicon dioxide and silicon nitride [3,4]. The fabrication process introduced involves partially masking a substrate with a silicon dioxide striped pattern and then growing AlN via MOVPE simultaneously on the dielectric mask and exposed substrate. A buffered oxide etch is then used to remove the underlying silicon dioxide and leave a free standing AlN micro-channel. The width of the channel has been varied from 5 ìm to 110 ìm and the height of the air gap from 130 nm to 800 nm indicating the stability of the structure. Furthermore, this versatile process has been performed on (111) silicon, c-plane sapphire, and gallium nitride epilayers on sapphire substrates. Reflection High Energy Electron Diffraction (RHEED), Atomic Force Microscopy (AFM), and Raman measurements have been taken on channels grown on each substrate and indicate that the substrate is influencing the growth of the AlN micro-channels on the SiO2 sacrificial layer.

  16. Simplified efficient phosphorescent organic light-emitting diodes by organic vapor phase deposition (United States)

    Pfeiffer, P.; Beckmann, C.; Stümmler, D.; Sanders, S.; Simkus, G.; Heuken, M.; Vescan, A.; Kalisch, H.


    The most efficient phosphorescent organic light-emitting diodes (OLEDs) are comprised of complex stacks with numerous organic layers. State-of-the-art phosphorescent OLEDs make use of blocking layers to confine charge carriers and excitons. On the other hand, simplified OLEDs consisting of only three organic materials have shown unexpectedly high efficiency when first introduced. This was attributed to superior energy level matching and suppressed external quantum efficiency (EQE) roll-off. In this work, we study simplified OLED stacks, manufactured by organic vapor phase deposition, with a focus on charge balance, turn-on voltage (Von), and efficiency. To prevent electrons from leaking through the device, we implemented a compositionally graded emission layer. By grading the emitter with the hole transport material, charge confinement is enabled without additional blocking layers. Our best performing organic stack is composed of only three organic materials in two layers including the emitter Ir(ppy)3 and yields a Von of 2.5 V (>1 cd/m2) and an EQE of 13% at 3000 cd/m2 without the use of any additional light extraction techniques. Changes in the charge balance, due to barrier tuning or adjustments in the grading parameters and layer thicknesses, are clearly visible in the current density-voltage-luminance (J-V-L) measurements. As charge injection at the electrodes and organic interfaces is of great interest but difficult to investigate in complex device structures, we believe that our simplified organic stack is not only a potent alternative to complex state-of-the-art OLEDs but also a well suited test vehicle for experimental studies focusing on the modification of the electrode-organic semiconductor interface.

  17. Organometallic Vapor-Phase Epitaxy theory and practice

    CERN Document Server

    Stringfellow, Gerald B


    This book describes the operation of a particular technique for the production of compound semiconductor materials. It describes how the technique works, how it can be used for the growth of particular materials and structures, and the application of these materials for specific devices. It contains not only a fundamental description of the operation of the technique but also contains lists of data useful for the everyday operation of OMVPE reactors. It also offers specific recipes that can be used to produce a wide range of specific materials, structures, and devices.Key Features* Updated wit

  18. Desalination of water by vapor-phase transport through hydrophobic nanopores (United States)

    Lee, Jongho; Karnik, Rohit


    We propose a new approach to desalination of water whereby a pressure difference across a vapor-trapping nanopore induces selective transport of water by isothermal evaporation and condensation across the pore. Transport of water through a nanopore with saline water on one side and pure water on the other side under a pressure difference was theoretically analyzed under the rarefied gas assumption using a probabilistic framework that accounts for diffuse scattering from the pore walls as well as reflection from the menisci. The analysis revealed that in addition to salinity, temperature, and pressure difference, the nanopore aspect ratio and the probability of condensation of a water molecule incident on a meniscus from the vapor phase, known as the condensation coefficient, are key determinants of flux. The effect of condensation coefficient on mass flux becomes critical when the aspect ratio is small. However, the mass flux becomes independent of the condensation coefficient as the pore aspect ratio increases, converging to the Knudsen flux for long nanopores. For design of a nanopore membrane that can trap vapor, a minimum aspect ratio is derived for which coalescence of the two interfaces on either side of the nanopore remains energetically unfavorable. Based on this design criterion, the analysis suggests that mass flux in the range of 20-70 g/m2 s may be feasible if the system is operated at temperatures in the range of 30-50 °C. The proposed approach further decouples transport properties from material properties of the membrane, which opens the possibility of engineering membranes with appropriate materials that may lead to reverse osmosis membranes with improved flux, better selectivity, and high chlorine resistance.

  19. Epitaxial Integration of Nanowires in Microsystems by Local Micrometer Scale Vapor Phase Epitaxy

    DEFF Research Database (Denmark)

    Mølhave, Kristian; Wacaser, Brent A.; Petersen, Dirch Hjorth


    Free-standing epitaxially grown nanowires provide a controlled growth system and an optimal interface to the underlying substrate for advanced optical, electrical, and mechanical nanowire device connections. Nanowires can be grown by vapor-phase epitaxy (VPE) methods such as chemical vapor...


    Results of an experiment in which grass was grown in a greenhouse and outdoors, and in soils of different concentration levels of dioxins and furans, were used in a modeling exercise to derive an air-to-leaf vapor phase transfer factor. The purpose of the experiment was to under...

  1. Inhibition effects of vapor phase thymol and modified atmosphere against Salmonella spp. on raw shrimp (United States)

    Salmonella contamination of shrimp is a food safety concern in the U.S. and other countries. Natural antimicrobial compounds (e.g. essential oils) in vapor phase and modified atmosphere (MA) technology can inhibit the growth potential of Salmonella spp. However, each strategy has its limitations, wh...

  2. Improved thermal lattice Boltzmann model for simulation of liquid-vapor phase change (United States)

    Li, Qing; Zhou, P.; Yan, H. J.


    In this paper, an improved thermal lattice Boltzmann (LB) model is proposed for simulating liquid-vapor phase change, which is aimed at improving an existing thermal LB model for liquid-vapor phase change [S. Gong and P. Cheng, Int. J. Heat Mass Transfer 55, 4923 (2012), 10.1016/j.ijheatmasstransfer.2012.04.037]. First, we emphasize that the replacement of ∇ .(λ ∇ T ) /∇.(λ ∇ T ) ρ cV ρ cV with ∇ .(χ ∇ T ) is an inappropriate treatment for diffuse interface modeling of liquid-vapor phase change. Furthermore, the error terms ∂t 0(T v ) +∇ .(T vv ) , which exist in the macroscopic temperature equation recovered from the previous model, are eliminated in the present model through a way that is consistent with the philosophy of the LB method. Moreover, the discrete effect of the source term is also eliminated in the present model. Numerical simulations are performed for droplet evaporation and bubble nucleation to validate the capability of the model for simulating liquid-vapor phase change. It is shown that the numerical results of the improved model agree well with those of a finite-difference scheme. Meanwhile, it is found that the replacement of ∇ .(λ ∇ T ) /∇ .(λ ∇ T ) ρ cV ρ cV with ∇ .(χ ∇ T ) leads to significant numerical errors and the error terms in the recovered macroscopic temperature equation also result in considerable errors.

  3. Recent Advances in Atmospheric Vapor-Phase Deposition of Transparent and Conductive Zinc Oxide

    NARCIS (Netherlands)

    Illiberi, A.; Poodt, P.; Roozeboom, F.


    The industrial need for high-throughput and low-cost ZnO deposition processes has triggered the development of atmospheric vapor-phase deposition techniques which can be easily applied to continuous, in-line manufacturing. While atmospheric CVD is a mature technology, new processes for the growth of

  4. Polycrystalline indium phosphide on silicon by indium assisted growth in hydride vapor phase epitaxy

    Energy Technology Data Exchange (ETDEWEB)

    Metaferia, Wondwosen; Sun, Yan-Ting, E-mail:; Lourdudoss, Sebastian [Laboratory of Semiconductor Materials, Department of Materials and Nano Physics, KTH—Royal Institute of Technology, Electrum 229, 164 40 Kista (Sweden); Pietralunga, Silvia M. [CNR-Institute for Photonics and Nanotechnologies, P. Leonardo da Vinci, 32 20133 Milano (Italy); Zani, Maurizio; Tagliaferri, Alberto [Department of Physics Politecnico di Milano, P. Leonardo da Vinci, 32 20133 Milano (Italy)


    Polycrystalline InP was grown on Si(001) and Si(111) substrates by using indium (In) metal as a starting material in hydride vapor phase epitaxy (HVPE) reactor. In metal was deposited on silicon substrates by thermal evaporation technique. The deposited In resulted in islands of different size and was found to be polycrystalline in nature. Different growth experiments of growing InP were performed, and the growth mechanism was investigated. Atomic force microscopy and scanning electron microscopy for morphological investigation, Scanning Auger microscopy for surface and compositional analyses, powder X-ray diffraction for crystallinity, and micro photoluminescence for optical quality assessment were conducted. It is shown that the growth starts first by phosphidisation of the In islands to InP followed by subsequent selective deposition of InP in HVPE regardless of the Si substrate orientation. Polycrystalline InP of large grain size is achieved and the growth rate as high as 21 μm/h is obtained on both substrates. Sulfur doping of the polycrystalline InP was investigated by growing alternating layers of sulfur doped and unintentionally doped InP for equal interval of time. These layers could be delineated by stain etching showing that enough amount of sulfur can be incorporated. Grains of large lateral dimension up to 3 μm polycrystalline InP on Si with good morphological and optical quality is obtained. The process is generic and it can also be applied for the growth of other polycrystalline III–V semiconductor layers on low cost and flexible substrates for solar cell applications.

  5. Synthesis, characterization and application of electrode materials

    Energy Technology Data Exchange (ETDEWEB)

    He, Lin [Iowa State Univ., Ames, IA (United States)


    It has been known that significant advances in electrochemistry really depend on improvements in the sensitivity, selectivity, convenience, and/or economy of working electrodes, especially through the development of new working electrode materials. The advancement of solid state chemistry and materials science makes it possible to provide the materials which may be required as satisfactory electrode materials. The combination of solid state techniques with electrochemistry expands the applications of solid state materials and leads to the improvement of electrocatalysis. The study of Ru-Ti4O7 and Pt-Ti4O7 microelectrode arrays as introduced in paper 1 and paper 4, respectively, focuses on their synthesis and characterization. The synthesis is described by high temperature techniques for Ru or Pt microelectrode arrays within a conductive Ti4O7ceramic matrix. The characterization is based on the data obtained by x-ray diffractometry, scanning electron microscopy, voltammetry and amperometry. These microelectrode arrays show significant enhancement in current densities in comparison to solid Ru and Pt electrodes. Electrocatalysis at pyrochlore oxide Bi2Ru2O7.3 and Bi2Ir2O7 electrodes are described in paper 2 and paper 3, respectively. Details are reported for the synthesis and characterization of composite Bi2Ru2O7.3 electrodes. Voltammetric data are examined for evidence that oxidation can occur with transfer of oxygen to the oxidation products in the potential region corresponding to anodic discharge of H2O with simultaneous evolution of O2. Paper 3 includes electrocatalytic activities of composite Bi2Ir2O7 disk electrodes for the oxidation of I- and the reduction of IO3-.

  6. Polydopamine Based Colloidal Materials: Synthesis and Applications. (United States)

    Deng, Ziwei; Shang, Bin; Peng, Bo


    Polydopamine is a synthetic analogue of natural melanin (eumelanin) produced from oxidative polymerization of dopamine. Owing to its strong adhesion ability, versatile chemical reactivity, biocompatibility and biodegradation, polydopamine is commonly applied as a versatile linker to synthesize colloidal materials with diverse structures, unique physicochemical properties and tunable functions, which allow for a broad scope of applications including biomedicine, sensing, catalysis, environment and energy. In this personal account, we discuss first about the different synthetic approaches of polydopamine, as well as its polymerization mechanism, and then with a comprehensive overview of recent progress in the synthesis and applications of polydopamine-based colloidal materials. Finally, we summarize this personal account with future perspectives. © 2017 The Chemical Society of Japan & Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Synthesis and Characterization of 2-D Materials (United States)

    Pazos, S.; Sahoo, P.; Afaneh, T.; Rodriguez Gutierrez, H.

    Atomically thin transition-metal dichacogenides (TMD), graphene, and boron nitride (BN) are two-dimensional materials where the charge carriers (electrons and holes) are confined to move in a plane. They exhibit distinctive optoelectronic properties compared to their bulk layered counterparts. When combined into heterostructures, these materials open more possibilities in terms of new properties and device functionality. In this work, WSe2 and graphene were grown using Chemical Vapor Deposition (CVD) and Physical Vapor Deposition (PVD) techniques. The quality and morphology of each material was checked using Raman, Photoluminescence Spectroscopy, and Scanning Electron Microscopy. Graphene had been successfully grown homogenously, characterized, and transferred from copper to silicon dioxide substrates; these films will be used in future studies to build 2-D devices. Different morphologies of WSe2 2-D islands were successfully grown on SiO2 substrates. Depending on the synthesis conditions, the material on each sample had single layer, double layer, and multi-layer areas. A variety of 2-D morphologies were also observed in the 2-D islands. This project is supported by the NSF REU Grant #1560090 and NSF Grant #DMR-1557434.

  8. Compact Raman Lidar Measurement of Liquid and Vapor Phase Water Under the Influence of Ionizing Radiation

    Directory of Open Access Journals (Sweden)

    Shiina Tatsuo


    Full Text Available A compact Raman lidar has been developed for studying phase changes of water in the atmosphere under the influence of ionization radiation. The Raman lidar is operated at the wavelength of 349 nm and backscattered Raman signals of liquid and vapor phase water are detected at 396 and 400 nm, respectively. Alpha particles emitted from 241Am of 9 MBq ionize air molecules in a scattering chamber, and the resulting ions lead to the formation of liquid water droplets. From the analysis of Raman signal intensities, it has been found that the increase in the liquid water Raman channel is approximately 3 times as much as the decrease in the vapor phase water Raman channel, which is consistent with the theoretical prediction based on the Raman cross-sections. In addition, the radius of the water droplet is estimated to be 0.2 μm.

  9. In situ, subsurface monitoring of vapor-phase TCE using fiber optics

    Energy Technology Data Exchange (ETDEWEB)

    Rossabi, J. [Westinghouse Savannah River Co., Aiken, SC (United States); Colston, B. Jr.; Brown, S.; Milanovich, F. [Lawrence Livermore National Lab., CA (United States); Lee, L.T. Jr. [Army Engineer Waterways Experiment Station, Vicksburg, MS (United States). Geotechnical Lab.


    A vapor-phase, reagent-based, fiber optic trichloroethylene (TCE) sensor developed by Lawrence Livermore National Laboratory (LLNL) was demonstrated at the Savannah River Site (SRS) in two configurations. The first incorporated the sensor into a down-well instrument bounded by two inflatable packers capable of sealing an area for discrete depth analysis. The second involved an integration of the sensor into the probe tip of the Army Corps of Engineers Waterways Experiment Station (WES) cone penetrometry system. Discrete depth measurements of vapor-phase concentrations of TCE in the vadose zone were successfully made using both configurations. These measurements demonstrate the first successful in situ sensing (as opposed to sampling) of TCE at a field site.

  10. Vapor phase epitaxial liftoff of GaAs and silicon single crystal films

    Energy Technology Data Exchange (ETDEWEB)

    Chang, W.; Kao, C.P.; Pike, G.A.; Slone, J.A.; Yablonovitch, E. [Electrical Engineering Department, University of California, Los Angeles, CA 90095-1594 (United States)


    Among the technologies for integrating GaAs devices with Si VLSI chips, epitaxial liftoff (ELO) is conspicuous for maintaining the quality of the single crystal epitaxial GaAs films. Traditionally, ELO is implemented in aqueous HF solution. It would be cleaner and simpler if ELO could be implemented in a vapor process. In this article, we will present the potential improvements in the ELO process by using a vapor phase etch to undercut thin films

  11. Manufacturing Demonstration Facility: Low Temperature Materials Synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Graham, David E. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Moon, Ji-Won [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Armstrong, Beth L. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Datskos, Panos G. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Duty, Chad E. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Gresback, Ryan [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Ivanov, Ilia N. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jacobs, Christopher B. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jellison, Gerald Earle [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jang, Gyoung Gug [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Joshi, Pooran C. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jung, Hyunsung [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Meyer, III, Harry M. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Phelps, Tommy [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)


    The Manufacturing Demonstration Facility (MDF) low temperature materials synthesis project was established to demonstrate a scalable and sustainable process to produce nanoparticles (NPs) for advanced manufacturing. Previous methods to chemically synthesize NPs typically required expensive, high-purity inorganic chemical reagents, organic solvents and high temperatures. These processes were typically applied at small laboratory scales at yields sufficient for NP characterization, but insufficient to support roll-to-roll processing efforts or device fabrication. The new NanoFermentation processes described here operated at a low temperature (~60 C) in low-cost, aqueous media using bacteria that produce extracellular NPs with controlled size and elemental stoichiometry. Up-scaling activities successfully demonstrated high NP yields and quality in a 900-L pilot-scale reactor, establishing this NanoFermentation process as a competitive biomanufacturing strategy to produce NPs for advanced manufacturing of power electronics, solid-state lighting and sensors.

  12. Synthesis of functional materials in combustion reactions

    Energy Technology Data Exchange (ETDEWEB)

    Zhuravlev, V. D., E-mail:; Bamburov, V. G.; Ermakova, L. V.; Lobachevskaya, N. I. [Russian Academy of Sciences, Institute of Solid State Chemistry, Ural Branch (Russian Federation)


    The conditions for obtaining oxide compounds in combustion reactions of nitrates of metals with organic chelating–reducing agents such as amino acids, urea, and polyvinyl alcohol are reviewed. Changing the nature of internal fuels and the reducing agent-to-oxidizing agent ratio makes possible to modify the thermal regime of the process, fractal dimensionality, morphology, and dispersion of synthesized functional materials. This method can be used to synthesize simple and complex oxides, composites, and metal powders, as well as ceramics and coatings. The possibilities of synthesis in combustion reactions are illustrated by examples of αand γ-Al{sub 2}O{sub 3}, YSZ composites, uranium oxides, nickel powder, NiO and NiO: YSZ composite, TiO{sub 2}, and manganites, cobaltites, and aluminates of rare earth elements.

  13. Synthesis of functional materials in combustion reactions (United States)

    Zhuravlev, V. D.; Bamburov, V. G.; Ermakova, L. V.; Lobachevskaya, N. I.


    The conditions for obtaining oxide compounds in combustion reactions of nitrates of metals with organic chelating-reducing agents such as amino acids, urea, and polyvinyl alcohol are reviewed. Changing the nature of internal fuels and the reducing agent-to-oxidizing agent ratio makes possible to modify the thermal regime of the process, fractal dimensionality, morphology, and dispersion of synthesized functional materials. This method can be used to synthesize simple and complex oxides, composites, and metal powders, as well as ceramics and coatings. The possibilities of synthesis in combustion reactions are illustrated by examples of αand γ-Al2O3, YSZ composites, uranium oxides, nickel powder, NiO and NiO: YSZ composite, TiO2, and manganites, cobaltites, and aluminates of rare earth elements.

  14. Machine-learned and codified synthesis parameters of oxide materials (United States)

    Kim, Edward; Huang, Kevin; Tomala, Alex; Matthews, Sara; Strubell, Emma; Saunders, Adam; McCallum, Andrew; Olivetti, Elsa


    Predictive materials design has rapidly accelerated in recent years with the advent of large-scale resources, such as materials structure and property databases generated by ab initio computations. In the absence of analogous ab initio frameworks for materials synthesis, high-throughput and machine learning techniques have recently been harnessed to generate synthesis strategies for select materials of interest. Still, a community-accessible, autonomously-compiled synthesis planning resource which spans across materials systems has not yet been developed. In this work, we present a collection of aggregated synthesis parameters computed using the text contained within over 640,000 journal articles using state-of-the-art natural language processing and machine learning techniques. We provide a dataset of synthesis parameters, compiled autonomously across 30 different oxide systems, in a format optimized for planning novel syntheses of materials.

  15. Physical basis for materials synthesis using biomineralization

    Energy Technology Data Exchange (ETDEWEB)

    De Yoreo, J; Orme, C; Dove, P; Teng, H


    Since the dawn of life on earth, organisms have directed the crystallization of inorganic ions from solution to form minerals that meet specific biological needs. The resulting materials often exhibit remarkable properties, making the processes involved in biomineralization of interest to a wide array of scientific disciplines. From a geochemical standpoint, perhaps the most important consequence is that CaCO{sub 3} biomineral formation occurs in the Oceans on such a large scale that it influences many aspects of seawater chemistry and results in sequestration of carbon in the form of carbonate sediments. In this manner, the products of biomineralization are preserved in the rock record and serve as an extensive chronicle of the interplay between biota and the earth system environment. From the point of view of materials synthesis, biological control over epitaxy is an elegant example of self-organization in complex molecular systems. Through selective introduction of peptides and proteins, living organisms deterministically modify nucleation, step kinetics, surface morphologies, and facet stabilities to produce nanophase materials, topologically complex single-crystals, and multi-layer composite. The resulting materials have biological functions as diverse as structural supports, porous filtration media, grinding and cutting tools, lenses, gravity sensors and magnetic guidance systems. As Table I shows, calcium carbonate minerals are ubiquitous amongst these biomineral structures. In addition , calcium carbonate is a well studied material that is easily crystallized and has known solution chemistry. Consequently, the calcium carbonate system provides an excellent model for investigating biomineralization processes. Surprisingly, in spite of the identification of carbonate biogenesis as a critical contributor to the carbon reservoir mediating climate change, and the enormous potential of biomimetic synthesis for production of tailored, crystalline nano- and micro

  16. Vapor Phase Self-assembled Monolayers for Anti-stiction Applications in MEMS

    DEFF Research Database (Denmark)

    Zhuang, Yanxin; Hansen, Ole; Knieling, Thomas


    We have investigated the anti-stiction performance of self-assembled monolayers (SAMs) that were grown in vapor phase from six different organosilane precursors: CF3(CF2)5(CH2)2SiCl3 (FOTS), CF3(CF2)5(CH2)2Si(OC2H5)3 (FOTES), CF3(CF2)5(CH2)2Si(CH3)Cl2 (FOMDS), CF3(CF2)5(CH2)2Si(CH3)2Cl (FOMMS), CF3...

  17. High flux diode packaging using passive microscale liquid-vapor phase change (United States)

    Bandhauer, Todd; Deri, Robert J.; Elmer, John W.; Kotovsky, Jack; Patra, Susant


    A laser diode package includes a heat pipe having a fluid chamber enclosed in part by a heat exchange wall for containing a fluid. Wicking channels in the fluid chamber is adapted to wick a liquid phase of the fluid from a condensing section of the heat pipe to an evaporating section of the heat exchanger, and a laser diode is connected to the heat exchange wall at the evaporating section of the heat exchanger so that heat produced by the laser diode is removed isothermally from the evaporating section to the condensing section by a liquid-to-vapor phase change of the fluid.

  18. Thermodynamics of acetone sorption from vapor phase by Keplerate and toroid polyoxomolybdate nanoclusters (United States)

    Ostroushko, A. A.; Adamova, L. V.; Eremina, E. V.; Grzhegorzhevskii, K. V.; Velichko, E. V.; Bogdanov, S. G.; Pirogov, A. N.


    The sorption of acetone from the vapor phase by Keplerate polyoxomolybdate (POM) nanoclusters, Mo132 and Mo72Fe30, and Mo138, a POM with a toroid structure, is studied via equilibrium interval sorption (a modification of vapor sorption gravimetry). The highest sorption capacity is registered for Mo132, while the other two show performance an order of magnitude lower. The specific Gibbs energy of the interaction between the POMs and acetone is reported. Small-angle X-ray and neutron scattering analysis indicates a considerable difference between the natures of Mo132 and Mo138 surfaces.

  19. Calculation of Liquid Water-Hydrate-Methane Vapor Phase Equilibria from Molecular Simulations

    DEFF Research Database (Denmark)

    Jensen, Lars; Thomsen, Kaj; von Solms, Nicolas


    Monte Carlo simulation methods for determining fluid- and crystal-phase chemical potentials are used for the first time to calculate liquid water-methane hydrate-methane vapor phase equilibria from knowledge of atomistic interaction potentials alone. The water and methane molecules are modeled...... potential of the zero-occupancy hydrate system using thermodynamic integration from an Einstein crystal reference state, and (iii) thermodynamic integration to obtain the water and guest molecules' chemical potentials as a function of the hydrate occupancy. The three-phase equilibrium curve is calculated...... value at corresponding conditions. While computationally intensive, simulations such as these are essential to map the thermodynamically stable conditions for hydrate systems....

  20. Vapor Phase Sensing Using Metal Nanorod Thin Films Grown by Cryogenic Oblique Angle Deposition

    Directory of Open Access Journals (Sweden)

    Piyush Shah


    Full Text Available We demonstrate the chemical sensing capability of silver nanostructured films grown by cryogenic oblique angle deposition (OAD. For comparison, the films are grown side by side at cryogenic (~100 K and at room temperature (~300 K by e-beam evaporation. Based on the observed structural differences, it was hypothesized that the cryogenic OAD silver films should show an increased surface enhanced Raman scattering (SERS sensitivity. COMSOL simulation results are presented to validate this hypothesis. Experimental SERS results of 4-aminobenzenethiol (4-ABT Raman test probe molecules in vapor phase show good agreement with the simulation and indicate promising SERS applications for these nanostructured thin films.

  1. Structural, electrical and luminescent characteristics of ultraviolet light emitting structures grown by hydride vapor phase epitaxy

    Directory of Open Access Journals (Sweden)

    A.Y. Polyakov


    Full Text Available Electrical and luminescent properties of near-UV light emitting diode structures (LEDs prepared by hydride vapor phase epitaxy (HVPE were studied. Variations in photoluminescence and electroluminescence efficiency observed for LEDs grown under nominally similar conditions could be attributed to the difference in the structural quality (dislocation density, density of dislocations agglomerates of the GaN active layers, to the difference in strain relaxation achieved by growth of AlGaN/AlGaN superlattice and to the presence of current leakage channels in current confining AlGaN layers of the double heterostructure.

  2. A model for arsenic anti-site incorporation in GaAs grown by hydride vapor phase epitaxy

    Energy Technology Data Exchange (ETDEWEB)

    Schulte, K. L.; Kuech, T. F. [Department of Chemical and Biological Engineering, University of Wisconsin-Madison, Madison, Wisconsin 53706 (United States)


    GaAs growth by hydride vapor phase epitaxy (HVPE) has regained interest as a potential route to low cost, high efficiency thin film photovoltaics. In order to attain the highest efficiencies, deep level defect incorporation in these materials must be understood and controlled. The arsenic anti-site defect, As{sub Ga} or EL2, is the predominant deep level defect in HVPE-grown GaAs. In the present study, the relationships between HVPE growth conditions and incorporation of EL2 in GaAs epilayers were determined. Epitaxial n-GaAs layers were grown under a wide range of deposition temperatures (T{sub D}) and gallium chloride partial pressures (P{sub GaCl}), and the EL2 concentration, [EL2], was determined by deep level transient spectroscopy. [EL2] agreed with equilibrium thermodynamic predictions in layers grown under conditions in which the growth rate, R{sub G}, was controlled by conditions near thermodynamic equilibrium. [EL2] fell below equilibrium levels when R{sub G} was controlled by surface kinetic processes, with the disparity increasing as R{sub G} decreased. The surface chemical composition during growth was determined to have a strong influence on EL2 incorporation. Under thermodynamically limited growth conditions, e.g., high T{sub D} and/or low P{sub GaCl}, the surface vacancy concentration was high and the bulk crystal was close to equilibrium with the vapor phase. Under kinetically limited growth conditions, e.g., low T{sub D} and/or high P{sub GaCl}, the surface attained a high GaCl coverage, blocking As adsorption. This competitive adsorption process reduced the growth rate and also limited the amount of arsenic that incorporated as As{sub Ga}. A defect incorporation model which accounted for the surface concentration of arsenic as a function of the growth conditions, was developed. This model was used to identify optimal growth parameters for the growth of thin films for photovoltaics, conditions in which a high growth rate and low [EL2] could be

  3. Observation of atomic carbon during photodissociation of nitrotoluenes in the vapor phase (United States)

    Eilers, Hergen; Diez-y-Riega, Helena


    We perform laser-induced photodissociation fluorescence spectroscopy on mononitrotoluenes (MNTs) and dinitrotoluenes (DNTs) in the vapor phase and observe the spectrally overlapping fluorescence from nitric oxide (NO) and carbon (C). Energy-dispersive x-ray spectroscopy (EDS) and Raman spectroscopy of deposits found in the sample chamber confirm the presence of carbon. By comparing the observed fluorescence intensities with the Franck-Condon factors for NO, we are able to identify the presence or absence of fluorescence from carbon. 2-nitrotoluene and 4- nitrotoluene show carbon fluorescence for gate delays of up to 500 ns, while 2,4-dinitrotolune, 3,4-dinitrotolune, and 2,6-dinitrotolune show carbon fluorescence for gate delays of at least up to 1500 ns. The spectroscopic signal from atomic carbon in the vapor phase is observed at concentrations as low as 10 ppt. Based upon the observed S/N, detection at even lower concentrations appears feasible. Several non-nitrotoluene molecules including nitrobenzene, benzene, toluene, and CO2, are tested under identical conditions, but do not show any carbon emission. The presence of extra NO (simulation of NO pollutants) in the samples improves the S/N ratio for the detection of carbon. Energy transfer from laser-excited molecular nitrogen to NO, multiple decomposition channels in the electronic excited state of the nitrotoluene molecules, and interaction of NO with the excited-state decomposition process of the nitrotoluene molecules may all play a role.

  4. Enhanced Vapor-Phase Diffusion in Porous Media - LDRD Final Report

    Energy Technology Data Exchange (ETDEWEB)

    Ho, C.K.; Webb, S.W.


    As part of the Laboratory-Directed Research and Development (LDRD) Program at Sandia National Laboratories, an investigation into the existence of enhanced vapor-phase diffusion (EVD) in porous media has been conducted. A thorough literature review was initially performed across multiple disciplines (soil science and engineering), and based on this review, the existence of EVD was found to be questionable. As a result, modeling and experiments were initiated to investigate the existence of EVD. In this LDRD, the first mechanistic model of EVD was developed which demonstrated the mechanisms responsible for EVD. The first direct measurements of EVD have also been conducted at multiple scales. Measurements have been made at the pore scale, in a two- dimensional network as represented by a fracture aperture, and in a porous medium. Significant enhancement of vapor-phase transport relative to Fickian diffusion was measured in all cases. The modeling and experimental results provide additional mechanisms for EVD beyond those presented by the generally accepted model of Philip and deVries (1957), which required a thermal gradient for EVD to exist. Modeling and experimental results show significant enhancement under isothermal conditions. Application of EVD to vapor transport in the near-surface vadose zone show a significant variation between no enhancement, the model of Philip and deVries, and the present results. Based on this information, the model of Philip and deVries may need to be modified, and additional studies are recommended.

  5. Metalorganic vapor phase epitaxy of AlN on sapphire with low etch pit density (United States)

    Koleske, D. D.; Figiel, J. J.; Alliman, D. L.; Gunning, B. P.; Kempisty, J. M.; Creighton, J. R.; Mishima, A.; Ikenaga, K.


    Using metalorganic vapor phase epitaxy, methods were developed to achieve AlN films on sapphire with low etch pit density (EPD). Key to this achievement was using the same AlN growth recipe and only varying the pre-growth conditioning of the quartz-ware. After AlN growth, the quartz-ware was removed from the growth chamber and either exposed to room air or moved into the N2 purged glove box and exposed to H2O vapor. After the quartz-ware was exposed to room air or H2O, the AlN film growth was found to be more reproducible, resulting in films with (0002) and (10-12) x-ray diffraction (XRD) rocking curve linewidths of 200 and 500 arc sec, respectively, and EPDs NH3 on the quartz-ware surfaces generated AlN films with higher EPDs. The presence of these residual TMAl/NH3-derived coatings in metalorganic vapor phase epitaxy (MOVPE) systems and their impact on the sapphire surface during heating might explain why reproducible growth of AlN on sapphire is difficult.

  6. Comparative Study of Solution Phase and Vapor Phase Deposition of Aminosilanes on Silicon Dioxide Surfaces (United States)

    Yadav, Amrita R.; Sriram, Rashmi; Carter, Jared A.; Miller, Benjamin L.


    The uniformity of aminosilane layers typically used for the modification of hydroxyl bearing surfaces such as silicon dioxide is critical for a wide variety of applications, including biosensors. However, in spite of many studies that have been undertaken on surface silanization, there remains a paucity of easy-to-implement deposition methods reproducibly yielding smooth aminosilane monolayers. In this study, solution- and vapor-phase deposition methods for three aminoalkoxysilanes differing in the number of reactive groups (3-aminopropyl triethoxysilane (APTES), 3-aminopropyl methyl diethoxysilane (APMDES) and 3-aminopropyl dimethyl ethoxysilane (APDMES)) were assessed with the aim of identifying methods that yield highly uniform and reproducible silane layers that are resistant to minor procedural variations. Silane film quality was characterized based on measured thickness, hydrophilicity and surface roughness. Additionally, hydrolytic stability of the films was assessed via these thickness and contact angle values following desorption in water. We found that two simple solution-phase methods, an aqueous deposition of APTES and a toluene based deposition of APDMES, yielded high quality silane layers that exhibit comparable characteristics to those deposited via vapor-phase methods. PMID:24411379

  7. System Model of Heat and Mass Transfer Process for Mobile Solvent Vapor Phase Drying Equipment

    Directory of Open Access Journals (Sweden)

    Shiwei Zhang


    Full Text Available The solvent vapor phase drying process is one of the most important processes during the production and maintenance for large oil-immersed power transformer. In this paper, the working principle, system composition, and technological process of mobile solvent vapor phase drying (MVPD equipment for transformer are introduced in detail. On the basis of necessary simplification and assumption for MVPD equipment and process, a heat and mass transfer mathematical model including 40 mathematical equations is established, which represents completely thermodynamics laws of phase change and transport process of solvent, water, and air in MVPD technological processes and describes in detail the quantitative relationship among important physical quantities such as temperature, pressure, and flux in key equipment units and process. Taking a practical field drying process of 500 KV/750 MVA power transformer as an example, the simulation calculation of a complete technological process is carried out by programming with MATLAB software and some relation curves of key process parameters changing with time are obtained such as body temperature, tank pressure, and water yield. The change trend of theoretical simulation results is very consistent with the actual production record data which verifies the correctness of mathematical model established.

  8. Self-Catalyzed Growth of Vertically Aligned InN Nanorods by Metal-Organic Vapor Phase Epitaxy. (United States)

    Tessarek, C; Fladischer, S; Dieker, C; Sarau, G; Hoffmann, B; Bashouti, M; Göbelt, M; Heilmann, M; Latzel, M; Butzen, E; Figge, S; Gust, A; Höflich, K; Feichtner, T; Büchele, M; Schwarzburg, K; Spiecker, E; Christiansen, S


    Vertically aligned hexagonal InN nanorods were grown mask-free by conventional metal-organic vapor phase epitaxy without any foreign catalyst. The In droplets on top of the nanorods indicate a self-catalytic vapor-liquid-solid growth mode. A systematic study on important growth parameters has been carried out for the optimization of nanorod morphology. The nanorod N-polarity, induced by high temperature nitridation of the sapphire substrate, is necessary to achieve vertical growth. Hydrogen, usually inapplicable during InN growth due to formation of metallic indium, and silane are needed to enhance the aspect ratio and to reduce parasitic deposition beside the nanorods on the sapphire surface. The results reveal many similarities between InN and GaN nanorod growth showing that the process despite the large difference in growth temperature is similar. Transmission electron microscopy, spatially resolved energy-dispersive X-ray spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and Raman spectroscopy have been performed to analyze the structural properties. Spatially resolved cathodoluminescence investigations are carried out to verify the optical activity of the InN nanorods. The InN nanorods are expected to be the material of choice for high-efficiency hot carrier solar cells.

  9. Synthesis and catalytic applications of combined zeolitic/mesoporous materials

    Directory of Open Access Journals (Sweden)

    Jarian Vernimmen


    Full Text Available In the last decade, research concerning nanoporous siliceous materials has been focused on mesoporous materials with intrinsic zeolitic features. These materials are thought to be superior, because they are able to combine (i the enhanced diffusion and accessibility for larger molecules and viscous fluids typical of mesoporous materials with (ii the remarkable stability, catalytic activity and selectivity of zeolites. This review gives an overview of the state of the art concerning combined zeolitic/mesoporous materials. Focus is put on the synthesis and the applications of the combined zeolitic/mesoporous materials. The different synthesis approaches and formation mechanisms leading to these materials are comprehensively discussed and compared. Moreover, Ti-containing nanoporous materials as redox catalysts are discussed to illustrate a potential implementation of combined zeolitic/mesoporous materials.

  10. Virtual screening of inorganic materials synthesis parameters with deep learning (United States)

    Kim, Edward; Huang, Kevin; Jegelka, Stefanie; Olivetti, Elsa


    Virtual materials screening approaches have proliferated in the past decade, driven by rapid advances in first-principles computational techniques, and machine-learning algorithms. By comparison, computationally driven materials synthesis screening is still in its infancy, and is mired by the challenges of data sparsity and data scarcity: Synthesis routes exist in a sparse, high-dimensional parameter space that is difficult to optimize over directly, and, for some materials of interest, only scarce volumes of literature-reported syntheses are available. In this article, we present a framework for suggesting quantitative synthesis parameters and potential driving factors for synthesis outcomes. We use a variational autoencoder to compress sparse synthesis representations into a lower dimensional space, which is found to improve the performance of machine-learning tasks. To realize this screening framework even in cases where there are few literature data, we devise a novel data augmentation methodology that incorporates literature synthesis data from related materials systems. We apply this variational autoencoder framework to generate potential SrTiO3 synthesis parameter sets, propose driving factors for brookite TiO2 formation, and identify correlations between alkali-ion intercalation and MnO2 polymorph selection.

  11. Microgravity Production of Nanoparticles of Novel Materials Using Plasma Synthesis (United States)

    Frenklach, Michael; Fernandez-Pello, Carlos


    The research goal is to study the formation in reduced gravity of high quality nanoparticulate of novel materials using plasma synthesis. Particular emphasis will be placed on the production of powders of non-oxide materials like diamond, SiC, SiN, c-BN, etc. The objective of the study is to investigate the effect of gravity on plasma synthesis of these materials, and to determine how the microgravity synthesis can improve the quality and yield of the nanoparticles. It is expected that the reduced gravity will aid in the understanding of the controlling mechanisms of plasma synthesis, and will increase the yield, and quality of the synthesized powder. These materials have properties of interest in several industrial applications, such as high temperature load bearings or high speed metal machining. Furthermore, because of the nano-meter size of the particulate produced in this process, they have specific application in the fabrication of MEMS based combustion systems, and in the development and growth of nano-systems and nano-structures of these materials. These are rapidly advancing research areas, and there is a great need for high quality nanoparticles of different materials. One of the primary systems of interest in the project will be gas-phase synthesis of nanopowder of non-oxide materials.

  12. Materials informatics: a journey towards material design and synthesis. (United States)

    Takahashi, Keisuke; Tanaka, Yuzuru


    Materials informatics has been gaining popularity with the rapid development of computational materials science. However, collaborations between information science and materials science have not yet reached the success. There are several issues which need to be overcome in order to establish the field of materials informatics. Construction of material big data, implementation of machine learning, and platform design for materials discovery are discussed with potential solutions.

  13. Hierarchically porous materials: synthesis strategies and structure design. (United States)

    Yang, Xiao-Yu; Chen, Li-Hua; Li, Yu; Rooke, Joanna Claire; Sanchez, Clément; Su, Bao-Lian


    Owing to their immense potential in energy conversion and storage, catalysis, photocatalysis, adsorption, separation and life science applications, significant interest has been devoted to the design and synthesis of hierarchically porous materials. The hierarchy of materials on porosity, structural, morphological, and component levels is key for high performance in all kinds of applications. Synthesis and applications of hierarchically structured porous materials have become a rapidly evolving field of current interest. A large series of synthesis methods have been developed. This review addresses recent advances made in studies of this topic. After identifying the advantages and problems of natural hierarchically porous materials, synthetic hierarchically porous materials are presented. The synthesis strategies used to prepare hierarchically porous materials are first introduced and the features of synthesis and the resulting structures are presented using a series of examples. These involve templating methods (surfactant templating, nanocasting, macroporous polymer templating, colloidal crystal templating and bioinspired process, i.e. biotemplating), conventional techniques (supercritical fluids, emulsion, freeze-drying, breath figures, selective leaching, phase separation, zeolitization process, and replication) and basic methods (sol-gel controlling and post-treatment), as well as self-formation phenomenon of porous hierarchy. A series of detailed examples are given to show methods for the synthesis of hierarchically porous structures with various chemical compositions (dual porosities: micro-micropores, micro-mesopores, micro-macropores, meso-mesopores, meso-macropores, multiple porosities: micro-meso-macropores and meso-meso-macropores). We hope that this review will be helpful for those entering the field and also for those in the field who want quick access to helpful reference information about the synthesis of new hierarchically porous materials and

  14. Aluminum Gallium Nitride Alloys Grown via Metalorganic Vapor-Phase Epitaxy Using a Digital Growth Technique (United States)

    Rodak, L. E.; Korakakis, D.


    This work investigates the use of a digital growth technique as a viable method for achieving high-quality aluminum gallium nitride (Al x Ga1- x N) films via metalorganic vapor-phase epitaxy. Digital alloys are superlattice structures with period thicknesses of a few monolayers. Alloys with an AlN mole fraction ranging from 0.1 to 0.9 were grown by adjusting the thickness of the AlN layer in the superlattice. High-resolution x-ray diffraction was used to determine the superlattice period and c-lattice parameter of the structure, while reciprocal-space mapping was used to determine the a-lattice parameter and evaluate growth coherency. A comparison of the measured lattice parameter with both the nominal value and also the underlying buffer layer is discussed.

  15. Vapor phase polymerization of PEDOT on silicone rubber as flexible large strain sensor

    Directory of Open Access Journals (Sweden)

    Timothy Giffney


    Full Text Available This paper presents a flexible large strain sensor made from ethylenedioxythiophene deposited on silicone rubber (Ecoflex® 00-30 via vacuum assisted vapor phase polymerization (VPP process. EDOT was used due to its stability when exposed to the atmosphere. VPP is a very simple process requiring only a vacuum bell jar and a vacuum pump. Ferrite chloride (FeCl3 dissolved in tethrahydrofuran was used as the oxidant to make the resulting poly(3,4-ethylenedioxythiophene (PEDOT conductive. THF was used because it swells Ecoflex® for better infusion of oxidant and PEDOT adherence. The sensor performs reliably up to 80% strain with a gauge factor of ~2.4 and small hysteresis.

  16. Vapor-Phase Raman Spectra and the Barrier to Planarity of Cyclohexane. (United States)

    Chun, Hye Jin; Ocola, Esther J; Laane, Jaan


    The vapor-phase Raman spectra of an atmosphere of cyclohexane vapor heated to 90 and 110 °C collected over a large period of time and utilizing a high laser power of 4 W show hot band series starting at 380.8 cm-1 and corresponding to the v6(A1g) ring-inversion vibration. Fitting this data with a one-dimensional potential energy function allows the barrier to planarity of 8600 cm-1 (24.6 kcal/mol) to be calculated. Ab initio calculations (MP2/cc-pVTZ) predict a value of 10 377 cm-1 (29.7 kcal/mol), while DFT (B3LYP/cc-pVTZ) calculations predict 8804 cm-1 (25.2 kcal/mol).

  17. Procedure 5 Quality Assurance Requirements For Vapor Phase Mercury Continuous Emissions Monitoring Systems And Sorbent Trap Monitoring Systems Used For Compliance Determination At Stationary Sources (United States)

    Promulgated quality assurance Procedure 5 Quality Assurance Requirements For Vapor Phase Mercury Continuous Emissions Monitoring Systems And Sorbent Trap Monitoring Systems Used For Compliance Determination At Stationary Sources

  18. Vapor Phase Growth of ZnO Single Crystals/Thin Films and Attempts for p-type Doping


    Zhang, Xi


    The growth of ZnO single crystals and ZnO thin films on Si substrates by an open-system vapor phase method was studied in this thesis. The as-grown ZnO single crystals were investigated by means of photoluminescence (PL). Two unique emissions were observed in virgin and hydrogenated crystals. The up-to-now attempts for the p-type doping of ZnO were summarized and our doping studies were performed using nitrogen and antimony. The seed-free and open-system vapor phase method is a simple and...

  19. Study of the degradation of the external quantum efficiency of UV LEDs based on AlGaN/GaN heterostructures grown by chloride-hydride vapor-phase epitaxy (United States)

    Shmidt, N. M.; Usikov, A. S.; Shabunina, E. I.; Chernyakov, A. E.; Sakharov, A. V.; Kurin, S. Yu.; Antipov, A. A.; Barash, I. S.; Roenkov, A. D.; Makarov, Yu. N.; Helava, H.


    Final stage of the degradation of the external quantum efficiency of AlGaN/GaN UV light-emitting diodes (LEDs), grown by chloride-hydride vapor-phase epitaxy, and high-power InGaN/GaN blue LEDs, produced by metal-organic vapor-phase epitaxy, has been comparatively studied. It is shown that one of these processes leading to a decrease in the quantum efficiency for both types of LEDs is the local defect formation involving the Gold-Weisberg mechanism in a system of extended defects. To prolong the service life of AlGaN/GaN UV LEDs to more than 2000 h, it is necessary to improve the nanostructural arrangement of the material of light-emitting structures and determine the contribution from the AlGaN composition disorder to the degradation of the external quantum efficiency.

  20. Glass fibers and vapor phase components of cigarette smoke as cofactors in experimental respiratory tract carcinogenesis

    Energy Technology Data Exchange (ETDEWEB)

    Feron, V.J.; Kuper, C.F.; Spit, B.J.; Reuzel, P.G.; Woutersen, R.A.


    Syrian golden hamsters were given intratracheal instillations of glass fibers with or without BP suspended in saline, once a fortnight for 52 weeks; the experiment was terminated at week 85. No tumors of the respiratory tract were observed in hamsters treated with glass fibers alone. There was no indication that glass fibers enhanced the development of respiratory tract tumors induced by BP. In another study Syrian golden hamsters were exposed to fresh air or to a mixture of 4 major vapor phase components of cigarette smoke, viz. isoprene (800----700 ppm), methyl chloride (1000----900 ppm), methyl nitrite (200----190 ppm) and acetaldehyde (1400----1200 ppm) for a period of at most 23 months. Some of the animals were also given repeated intratracheal instillations of BP or norharman in saline. Laryngeal tumors were found in 7/31 male and 6/32 female hamsters exposed only to the vapor mixture, whereas no laryngeal tumors occurred in controls. The tumor response of the larynx most probably has to be ascribed entirely to the action of acetaldehyde. Simultaneous treatment with norharman or BP did not affect the tumor response of the larynx. Acetaldehyde may occur in the vapor phase of cigarette smoke at levels up to 2000 ppm. Chronic inhalation exposure of rats to acetaldehyde at levels of 0 (controls), 750, 1500 or 3000----1000 ppm resulted in a high incidence of nasal carcinomas, both squamous cell carcinomas of the respiratory epithelium and adenocarcinomas of the olfactory epithelium. It was discussed that acetaldehyde may significantly contribute to the induction of bronchogenic cancer by cigarette smoke in man.

  1. Treatment of Produced Waters Using a Surfactant Modified Zeolite/Vapor Phase Bioreactor System

    Energy Technology Data Exchange (ETDEWEB)

    Lynn E. Katz; Kerry A. Kinney; R. S. Bowman; E. J. Sullivan


    This report summarizes work of this project from October 2003 through March 2004. The major focus of the research was to further investigate BTEX removal from produced water, to quantify metal ion removal from produced water, and to evaluate a lab-scale vapor phase bioreactor (VPB) for BTEX destruction in off-gases produced during SMZ regeneration. Batch equilibrium sorption studies were conducted to evaluate the effect of semi-volatile organic compounds commonly found in produced water on the sorption of benzene, toluene, ethylbenzene, and xylene (BTEX) onto surfactant-modified zeolite (SMZ) and to examine selected metal ion sorption onto SMZ. The sorption of polar semi-volatile organic compounds and metals commonly found in produced water onto SMZ was also investigated. Batch experiments were performed in a synthetic saline solution that mimicked water from a produced water collection facility in Wyoming. Results indicated that increasing concentrations of semi-volatile organic compounds increased BTEX sorption. The sorption of phenol compounds could be described by linear isotherms, but the linear partitioning coefficients decreased with increasing pH, especially above the pKa's of the compounds. Linear correlations relating partitioning coefficients of phenol compounds with their respective solubilities and octanol-water partitioning coefficients were developed for data collected at pH 7.2. The sorption of chromate, selenate, and barium in synthetic produced water were also described by Langmuir isotherms. Experiments conducted with a lab-scale vapor phase bioreactor (VPB) packed with foam indicated that this system could achieve high BTEX removal efficiencies once the nutrient delivery system was optimized. The xylene isomers and benzene were found to require the greatest biofilter bed depth for removal. This result suggested that these VOCs would ultimately control the size of the biofilter required for the produced water application. The biofilter

  2. Recent Advances in the Synthesis of High Explosive Materials

    Directory of Open Access Journals (Sweden)

    Jesse J. Sabatini


    Full Text Available This review discusses the recent advances in the syntheses of high explosive energetic materials. Syntheses of some relevant modern primary explosives and secondary high explosives, and the sensitivities and properties of these molecules are provided. In addition to the synthesis of such materials, processing improvement and formulating aspects using these ingredients, where applicable, are discussed in detail.

  3. Flexible, Low-Power Thin-Film Transistors Made of Vapor-Phase Synthesized High-k, Ultrathin Polymer Gate Dielectrics. (United States)

    Choi, Junhwan; Joo, Munkyu; Seong, Hyejeong; Pak, Kwanyong; Park, Hongkeun; Park, Chan Woo; Im, Sung Gap


    A series of high-k, ultrathin copolymer gate dielectrics were synthesized from 2-cyanoethyl acrylate (CEA) and di(ethylene glycol) divinyl ether (DEGDVE) monomers by a free radical polymerization via a one-step, vapor-phase, initiated chemical vapor deposition (iCVD) method. The chemical composition of the copolymers was systematically optimized by tuning the input ratio of the vaporized CEA and DEGDVE monomers to achieve a high dielectric constant (k) as well as excellent dielectric strength. Interestingly, DEGDVE was nonhomopolymerizable but it was able to form a copolymer with other kinds of monomers. Utilizing this interesting property of the DEGDVE cross-linker, the dielectric constant of the copolymer film could be maximized with minimum incorporation of the cross-linker moiety. To our knowledge, this is the first report on the synthesis of a cyanide-containing polymer in the vapor phase, where a high-purity polymer film with a maximized dielectric constant was achieved. The dielectric film with the optimized composition showed a dielectric constant greater than 6 and extremely low leakage current densities (thin-film transistors (OTFTs) and oxide TFTs were fabricated, which showed hysteresis-free transfer characteristics with an operating voltage of less than 3 V. Furthermore, the flexible OTFTs retained their low gate leakage current and ideal TFT characteristics even under 2% applied tensile strain, which makes them some of the most flexible OTFTs reported to date. We believe that these ultrathin, high-k organic dielectric films with excellent mechanical flexibility will play a crucial role in future soft electronics.

  4. Nonthermal Plasma Synthesis of Nanocrystals: Fundamental Principles, Materials, and Applications. (United States)

    Kortshagen, Uwe R; Sankaran, R Mohan; Pereira, Rui N; Girshick, Steven L; Wu, Jeslin J; Aydil, Eray S


    Nonthermal plasmas have emerged as a viable synthesis technique for nanocrystal materials. Inherently solvent and ligand-free, nonthermal plasmas offer the ability to synthesize high purity nanocrystals of materials that require high synthesis temperatures. The nonequilibrium environment in nonthermal plasmas has a number of attractive attributes: energetic surface reactions selectively heat the nanoparticles to temperatures that can strongly exceed the gas temperature; charging of nanoparticles through plasma electrons reduces or eliminates nanoparticle agglomeration; and the large difference between the chemical potentials of the gaseous growth species and the species bound to the nanoparticle surfaces facilitates nanocrystal doping. This paper reviews the state of the art in nonthermal plasma synthesis of nanocrystals. It discusses the fundamentals of nanocrystal formation in plasmas, reviews practical implementations of plasma reactors, surveys the materials that have been produced with nonthermal plasmas and surface chemistries that have been developed, and provides an overview of applications of plasma-synthesized nanocrystals.

  5. Hydride vapor phase epitaxy growth of GaN, InGaN, ScN, and ScAIN

    NARCIS (Netherlands)

    Bohnen, T.


    Chemical vapor deposition (CVD); hydride vapor phase epitaxy (HVPE); gallium nitride (GaN); indium gallium nitride (InGaN); scandium nitride (ScN); scandium aluminum nitride (ScAlN); semiconductors; thin films; nanowires; III nitrides; crystal growth - We studied the HVPE growth of different III

  6. Antimicrobial effects of vapor phase thymol, modified atmosphere and their combination against Salmonella spp. on raw shrimp (United States)

    Salmonella contamination of raw shrimp is a food safety concern in the U.S. and other countries. This research evaluated the effects of vapor phase thymol, modified atmosphere (MA) and their combination against Salmonella spp. on raw shrimp. Growth profiles of a Salmonella spp. cocktail (6 strains),...


    African Journals Online (AJOL)


    1Department of Chemistry, University of Agriculture, P.O. Box 28, UNAAB Post Office. Abeokuta, Nigeria. 2Department ... materials is an attractive and challenging area of research for materials chemists. For example, ..... Advances in Chemistry 218; American Chemical Society: Washington, DC; 1988; p 109. 16. Main, P. in ...

  8. Evaluation of the Antibacterial Potential of Liquid and Vapor Phase Phenolic Essential Oil Compounds against Oral Microorganisms. (United States)

    Wang, Tong-Hong; Hsia, Shih-Min; Wu, Chi-Hao; Ko, Shun-Yao; Chen, Michael Yuanchien; Shih, Yin-Hua; Shieh, Tzong-Ming; Chuang, Li-Chuan; Wu, Ching-Yi

    The aim of the present study was to determine the antibacterial activities of the phenolic essential oil (EO) compounds hinokitiol, carvacrol, thymol, and menthol against oral pathogens. Aggregatibacter actinomycetemcomitans, Streptococcus mutans, Methicillin-resistant Staphylococcus aureus (MRSA), and Escherichia. coli were used in this study. The minimum inhibitory concentrations (MICs), minimum bactericidal concentrations (MBCs), bacterial growth curves, temperature and pH stabilities, and synergistic effects of the liquid and vapor EO compounds were tested. The MIC/MBC of the EO compounds, ranging from the strongest to weakest, were hinokitiol (40-60 μg/mL/40-100 μg/mL), thymol (100-200 μg/mL/200-400 μg/mL), carvacrol (200-400 μg/mL/200-600 μg/mL), and menthol (500-more than 2500 μg/mL/1000-more than 2500 μg/mL). The antibacterial activities of the four EO phenolic compound based on the agar diffusion test and bacterial growth curves showed that the four EO phenolic compounds were stable under different temperatures for 24 h, but the thymol activity decreased when the temperature was higher than 80°C. The combination of liquid carvacrol with thymol did not show any synergistic effects. The activities of the vaporous carvacrol and thymol were inhibited by the presence of water. Continual violent shaking during culture enhanced the activity of menthol. Both liquid and vaporous hinokitiol were stable at different temperatures and pH conditions. The combination of vaporous hinokitiol with zinc oxide did not show synergistic effects. These results showed that the liquid and vapor phases of hinokitiol have strong anti-oral bacteria abilities. Hinokitiol has the potential to be applied in oral health care products, dental materials, and infection controls to exert antimicrobial activity.

  9. Ion Implantation and Synthesis of Materials

    CERN Document Server

    Nastasi, Michael


    Ion implantation is one of the key processing steps in silicon integrated circuit technology. Some integrated circuits require up to 17 implantation steps and circuits are seldom processed with less than 10 implantation steps. Controlled doping at controlled depths is an essential feature of implantation. Ion beam processing can also be used to improve corrosion resistance, to harden surfaces, to reduce wear and, in general, to improve materials properties. This book presents the physics and materials science of ion implantation and ion beam modification of materials. It covers ion-solid interactions used to predict ion ranges, ion straggling and lattice disorder. Also treated are shallow-junction formation and slicing silicon with hydrogen ion beams. Topics important for materials modification, such as ion-beam mixing, stresses, and sputtering, are also described.

  10. Synthesis and design of silicide intermetallic materials

    Energy Technology Data Exchange (ETDEWEB)

    Petrovic, J.J.; Castro, R.G.; Butt, D.P. [Los Alamos National Lab., NM (United States)] [and others


    The overall objective of this program is to develop structural silicide-based materials with optimum combinations of elevated temperature strength/creep resistance, low temperature fracture toughness, and high temperature oxidation and corrosion resistance for applications of importance to the U.S. processing industry. A further objective is to develop silicide-based prototype industrial components. The ultimate aim of the program is to work with industry to transfer the structural silicide materials technology to the private sector in order to promote international competitiveness in the area of advanced high temperature materials and important applications in major energy-intensive U.S. processing industries. The program presently has a number of developing industrial connections, including a CRADA with Schuller International Inc. targeted at the area of MoSi{sub 2}-based high temperature materials and components for fiberglass melting and processing applications. The authors are also developing an interaction with the Institute of Gas Technology (IGT) to develop silicides for high temperature radiant gas burner applications, for the glass and other industries. Current experimental emphasis is on the development and characterization of MoSi{sub 2}-Si{sub 3}N{sub 4} and MoSi{sub 2}-SiC composites, the plasma spraying of MoSi{sub 2}-based materials, and the joining of MoSi{sub 2} materials to metals.

  11. Vapor phase toxicity of marjoram oil compounds and their related monoterpenoids to Blattella germanica (Orthoptera: Blattellidae). (United States)

    Jang, Young-Su; Yang, Young-Cheol; Choi, Dal-Soon; Ahn, Young-Joon


    The toxicity of marjoram, Origanum majorana L., oil, 41 monoterpenoids, and 2 sesquiterpenoids against adult females of the German cockroach, Blattella germanica L., was examined using direct contact and vapor phase toxicity bioassays and compared with those of deltamethrin, dichlorvos, permethrin, and propoxur, four commonly used insecticides. In a filter-paper contact toxicity bioassay, the adulticidal activities of pulegone (0.06 mg/cm2), (+/-)-camphor (0.07 mg/cm2), and verbenone (0.07 mg/cm2) were comparable to that of permethrin (0.05 mg/cm2) but more pronounced than that of propoxur (0.18 mg/cm2), as judged by the 24-h LC50 values. These compounds were less effective than either deltamethrin (0.013 mg/cm2) or dichlorvos (0.007 mg/cm2). The toxicity of marjoram oil, thymol, alpha-terpineol, (-)-alpha-thujone, linalool, 1,8-cineole, (-)-camphor, and (+)-carvone, ranging from 0.08 to 0.18 mg/cm2, was higher than that of propoxur. In vapor phase toxicity tests, verbenone (11.48 mg/L air) was the most toxic compound followed by (-)-alpha-thujone (18.43 mg/L of air), thymol (18.76 mg/L of air), alpha-terpineol (21.89 mg/L of air), (+/-)-camphor (24.59 mg/L of air), linalool (26.20 mg/L of air), and marjoram oil (38.28 mg/L of air) on the basis of the 24-h LC50 values. Dichlorvos (0.07 mg/L of air) was the most potent fumigant. Structure-activity relationships indicate that structural characteristics, such as degrees of saturation and types of functional groups rather than types of carbon skeleton, and hydrophobicity and vapor pressure parameters appear to play a role in determining the monoterpenoid toxicities to adult B. germanica. Marjoram oil and the monoterpenoids described merit further study as potential fumigants or leads for the control of B. germanica.

  12. Soft vesicles in the synthesis of hard materials. (United States)

    Dong, Renhao; Liu, Weimin; Hao, Jingcheng


    Vesicles of surfactants in aqueous solution have received considerable attention because of their use as simple model systems for biological membranes and their applications in various fields including colloids, pharmaceuticals, and materials. Because of their architecture, vesicles could prove useful as "soft" templates for the synthesis of "hard materials". The vesicle phase, however, has been challenging and difficult to work with in the construction of hard materials. In the solution-phase synthesis of various inorganic or macromolecular materials, templating methods provide a powerful strategy to control the size, morphology, and composition of the resulting micro- and nanostructures. In comparison with hard templates, soft templates are generally constructed using amphiphilic molecules, especially surfactants and amphiphilic polymers. These types of compounds offer advantages including the wide variety of available templates, simple fabrication processes under mild conditions, and easy removal of the templates with less damage to the final structures. Researchers have used many ordered molecular aggregates such as vesicles, micelles, liquid crystals, emulsion droplets, and lipid nanotubes as templates or structure-directing agents to control the synthesis or assembly hard micro- and nanomaterials composed from inorganic compounds or polymers. In addition to their range of sizes and morphologies, vesicles present unique structures that can simultaneously supply different microenvironments for the growth and assembly of hard materials: the inner chamber of vesicles, the outer surface of the vesicles, and the space between bilayers. Two main approaches for applying vesicles in the field of hard materials have been explored: (i) in situ synthesis of micro- or nanomaterials within a specific microenvironment by vesicle templating and (ii) the assembly or incorporation of guest materials during the formation of vesicles. This Account provides an in-depth look at

  13. Synthesis and chemistry of elemental 2D materials

    Energy Technology Data Exchange (ETDEWEB)

    Mannix, Andrew J.; Kiraly, Brian; Hersam, Mark C.; Guisinger, Nathan P.


    2D materials have attracted considerable attention in the past decade for their superlative physical properties. These materials consist of atomically thin sheets exhibiting covalent in-plane bonding and weak interlayer and layer-substrate bonding. Following the example of graphene, most emerging 2D materials are derived from structures that can be isolated from bulk phases of layered materials, which form a limited library for new materials discovery. Entirely synthetic 2D materials provide access to a greater range of properties through the choice of constituent elements and substrates. Of particular interest are elemental 2D materials, because they provide the most chemically tractable case for synthetic exploration. In this Review, we explore the progress made in the synthesis and chemistry of synthetic elemental 2D materials, and offer perspectives and challenges for the future of this emerging field.

  14. Combustion and Plasma Synthesis of High-Temperature Materials (United States)

    Munir, Z. A.; Holt, J. B.


    KEYNOTE ADDRESS. Self-Propagating High-Temperature Synthesis: Twenty Years of Search and Findings (A. Merzhanov). SOLID-STATE COMBUSTION SYNTHESIS. Recent Progress in Combustion Synthesis of High-Performance Materials in Japan (M. Koizumi & Y. Miyamoto). Modeling and Numerical Computation of a Nonsteady SHS Process (A. Bayliss & B. Matkowsky). New Models of Quasiperiodic Burning in Combustion Synthesis (S. Margolis, et al.). Modeling of SHS Operations (V. Hlavacek, et al.). Combustion Theory for Sandwiches of Alloyable Materials (R. Armstrong & M. Koszykowski). Observations on the Combustion Reaction Between Thin Foils of Ni and Al (U. Anselmi-Tamburini & Z. Munir). Combustion Synthesis of Intermetallic Compounds (Y. Kaieda, et al.). Combustion Synthesis of Nickel Aluminides (B. Rabin, et al.). Self-Propagating High-Temperature Synthesis of NiTi Intermetallics (H. Yi & J. Moore). Shock-Induced Chemical Synthesis of Intermetallic Compounds (S. Work, et al.). Advanced Ceramics Via SHS (T. DeAngelis & D. Weiss). In-Situ Formation of SiC and SiC-C Blocked Solids by Self-Combustion Synthesis (S. Ikeda, et al.). Powder Purity and Morphology Effects in Combustion-Synthesis Reactions (L. Kecskes, et al.). Simultaneous Synthesis and Densification of Ceramic Components Under Gas Pressure by SHS (Y. Miyamoto & M. Koizumi). The Use of Self-Propagating High-Temperature Synthesis of High-Density Titanium Diboride (P. Zavitsanos, et al.). Metal--Ceramic Composite Pipes Produced by a Centrifugal-Thermit Process (O. Odawara). Simultaneous Combustion Synthesis and Densification of AIN (S. Dunmead, et al.). Fabrication of a Functionally Gradient Material by Using a Self-Propagating Reaction Process (N. Sata, et al.). Combustion Synthesis of Oxide-Carbide Composites (L. Wang, et al.). Heterogeneous Reaction Mechanisms in the Si-C System Under Conditions of Solid Combustion (R. Pampuch, et al.). Experimental Modeling of Particle-Particle Interactions During SHS of TiB2 -Al2O3 (K. Logan

  15. Synthesis of nanocrystalline materials through reverse micelles: A ...

    Indian Academy of Sciences (India)


    A versatile methodology for synthesis of complex metal oxides. ASHOK K GANGULI*, SONALIKA VAIDYA and ... sitions using the reverse micellar method. Here we describe our methodology to obtain important metal oxides ... Nanomaterials have fascinated the scientific community in the recent past. These materials exhibit ...

  16. Synthesis and characterization of super-microporous material with ...

    Indian Academy of Sciences (India)


    Synthesis and characterization of super-microporous material with enhanced hydrothermal stability. SHUJIE WU, KE SONG, JINGQI GUAN and QIUBIN KAN*. College of Chemistry, Jilin University, Changchun 130023, P.R. China. MS received 9 July 2009; revised 18 November 2009. Abstract. Super-microporouos silicon ...

  17. Synthesis of thin films and materials utilizing a gaseous catalyst (United States)

    Morse, Daniel E; Schwenzer, Birgit; Gomm, John R; Roth, Kristian M; Heiken, Brandon; Brutchey, Richard


    A method for the fabrication of nanostructured semiconducting, photoconductive, photovoltaic, optoelectronic and electrical battery thin films and materials at low temperature, with no molecular template and no organic contaminants. High-quality metal oxide semiconductor, photovoltaic and optoelectronic materials can be fabricated with nanometer-scale dimensions and high dopant densities through the use of low-temperature biologically inspired synthesis routes, without the use of any biological or biochemical templates.

  18. Carbon-supported bimetallic Pd–Fe catalysts for vapor-phase hydrodeoxygenation of guaiacol

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Junming; Karim, Ayman M.; Zhang, He; Kovarik, Libor; Li, Xiaohong Shari; Hensley, Alyssa J.; McEwen, Jean-Sabin; Wang, Yong


    Abstract Carbon supported metal catalysts (Cu/C, Fe/C, Pd/C, Pt/C, PdFe/C and Ru/C) have been prepared, characterized and tested for vapor-phase hydrodeoxygenation (HDO) of guaiacol (GUA) at atmospheric pressure. Phenol was the major intermediate on all catalysts. Over the noble metal catalysts saturation of the aromatic ring was the major pathway observed at low temperature (250 °C), forming predominantly cyclohexanone and cyclohexanol. Substantial ring opening reaction was observed on Pt/C and Ru/C at higher reaction temperatures (e.g., 350 °C). Base metal catalysts, especially Fe/C, were found to exhibit high HDO activity without ring-saturation or ring-opening with the main products being benzene, phenol along with small amounts of cresol, toluene and trimethylbenzene (TMB). A substantial enhancement in HDO activity was observed on the PdFe/C catalysts. Compared with Fe/C, the yield to oxygen-free aromatic products (i.e., benzene/toluene/TMB) on PdFe/C increased by a factor of four at 350 °C, and by approximately a factor of two (83.2% versus 43.3%) at 450 °C. The enhanced activity of PdFe/C is attributed to the formation of PdFe alloy as evidenced by STEM, EDS and TPR.

  19. ZnO Nanowires Synthesized by Vapor Phase Transport Deposition on Transparent Oxide Substrates

    Directory of Open Access Journals (Sweden)

    Taylor Curtis


    Full Text Available Abstract Zinc oxide nanowires have been synthesized without using metal catalyst seed layers on fluorine-doped tin oxide (FTO substrates by a modified vapor phase transport deposition process using a double-tube reactor. The unique reactor configuration creates a Zn-rich vapor environment that facilitates formation and growth of zinc oxide nanoparticles and wires (20–80 nm in diameter, up to 6 μm in length, density <40 nm apart at substrate temperatures down to 300°C. Electron microscopy and other characterization techniques show nanowires with distinct morphologies when grown under different conditions. The effect of reaction parameters including reaction time, temperature, and carrier gas flow rate on the size, morphology, crystalline structure, and density of ZnO nanowires has been investigated. The nanowires grown by this method have a diameter, length, and density appropriate for use in fabricating hybrid polymer/metal oxide nanostructure solar cells. For example, it is preferable to have nanowires no more than 40 nm apart to minimize exciton recombination in polymer solar cells.

  20. Vapor-phase polymerization of nanofibrillar poly(3,4-ethylenedioxythiophene) for supercapacitors. (United States)

    D'Arcy, Julio M; El-Kady, Maher F; Khine, Pwint P; Zhang, Linghong; Lee, Sun Hwa; Davis, Nicole R; Liu, David S; Yeung, Michael T; Kim, Sung Yeol; Turner, Christopher L; Lech, Andrew T; Hammond, Paula T; Kaner, Richard B


    Nanostructures of the conducting polymer poly(3,4-ethylenedioxythiophene) with large surface areas enhance the performance of energy storage devices such as electrochemical supercapacitors. However, until now, high aspect ratio nanofibers of this polymer could only be deposited from the vapor-phase, utilizing extrinsic hard templates such as electrospun nanofibers and anodized aluminum oxide. These routes result in low conductivity and require postsynthetic template removal, conditions that stifle the development of conducting polymer electronics. Here we introduce a simple process that overcomes these drawbacks and results in vertically directed high aspect ratio poly(3,4-ethylenedioxythiophene) nanofibers possessing a high conductivity of 130 S/cm. Nanofibers deposit as a freestanding mechanically robust film that is easily processable into a supercapacitor without using organic binders or conductive additives and is characterized by excellent cycling stability, retaining more than 92% of its initial capacitance after 10,000 charge/discharge cycles. Deposition of nanofibers on a hard carbon fiber paper current collector affords a highly efficient and stable electrode for a supercapacitor exhibiting gravimetric capacitance of 175 F/g and 94% capacitance retention after 1000 cycles.

  1. Vapor Phase Hydrogenation of Nitrobenzene to Aniline Over Carbon Supported Ruthenium Catalysts. (United States)

    Srikanth, Chakravartula S; Kumar, Vanama Pavan; Viswanadham, Balaga; Srikanth, Amirineni; Chary, Komandur V R


    A series of Ru/Carbon catalysts (0.5-6.0 wt%) were prepared by impregnation method. The catalysts were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), temperature programmed reduction (TPR), X-ray photoelectron spectroscopy (XPS), CO-chemisorption, surface area and pore-size distribution measurements. The catalytic activities were evaluated for the vapor phase hydrogenation of nitrobenzene. The dispersion measured by CO-uptake values suggests that a decrease of dispersion is observed with increasing Ru loading on carbon support. These findings are well supported by the crystallite size measured from XRD measurements. XPS study reveals the formation of Ru0 after reduction at 573 K for 3 h. The catalysts exhibit high conversion/selectivity at 4.5 wt% Ru loading during hydrogenation reaction. The particle size measured from CO-chemisorption and TEM analysis are related to the TOF during the hydrogenation reaction. Ru/C catalysts are found to show higher conversion/selectivities during hydrogenation of nitrobenzene to aniline.

  2. AlN thin film grown on different substrates by hydride vapor phase epitaxy (United States)

    Sun, M. S.; Zhang, J. C.; Huang, J.; Wang, J. F.; Xu, K.


    AlN thin films have been grown on GaN/sapphire templates, 6 H-SiC and sapphire by hydride vapor phase epitaxy. The influence of growth conditions and substrates on the crystal qualities and growth mode has been investigated by X-ray diffraction (XRD) and atomic force microscopy (AFM). The results showed that the low pressure was favorable for high-quality AlN thin film growth around 1000 °C. The full-width at half-maximum (FWHM) of (0002) XRD of 200-nm AlN thin film grown on GaN/sapphire, 6 H-SiC and sapphire are 220, 187 and 260 arc s, respectively. While the corresponding counterparts of (10-12) are 1300, 662 and 2650 arc s, respectively. Both suggested that low dislocation density in AlN grown on 6 H-SiC. The morphology of AlN thin film on sapphire showed islands without coalescence initially, and then changed to be coalescent with atomic steps at 1200 nm. However, those for samples on 6 H-SiC and GaN/sapphire showed smooth surface with clear atomic steps at thickness of 200 nm. The result indicated different growth modes of AlN on different substrates. It was believed that the different lattice mismatchs between AlN and substrates led to the different crystal qualities and growth modes.

  3. Island dynamics and anisotropy during vapor phase epitaxy of m-plane GaN

    Energy Technology Data Exchange (ETDEWEB)

    Perret, Edith [Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439, USA; University of Fribourg, Department of Physics and Fribourg Center for Nanomaterials, Chemin du Musée 3, CH-1700 Fribourg, Switzerland; Xu, Dongwei [Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439, USA; Highland, M. J. [Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439, USA; Stephenson, G. B. [Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439, USA; Zapol, P. [Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439, USA; Fuoss, P. H. [Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439, USA; Munkholm, A. [Munkholm Consulting, Mountain View, California 94043, USA; Thompson, Carol [Department of Physics, Northern Illinois University, DeKalb, Illinois 60115, USA


    Using in situ grazing-incidence x-ray scattering, we have measured the diffuse scattering from islands that form during layer-by-layer growth of GaN by metal-organic vapor phase epitaxy on the (1010) m-plane surface. The diffuse scattering is extended in the (0001) in-plane direction in reciprocal space, indicating a strong anisotropy with islands elongated along [1210] and closely spaced along [0001]. This is confirmed by atomic force microscopy of a quenched sample. Islands were characterized as a function of growth rate F and temperature. The island spacing along [0001] observed during the growth of the first monolayer obeys a power-law dependence on growth rate F-n, with an exponent n = 0:25 + 0.02. The results are in agreement with recent kinetic Monte Carlo simulations, indicating that elongated islands result from the dominant anisotropy in step edge energy and not from surface diffusion anisotropy. The observed power-law exponent can be explained using a simple steady-state model, which gives n = 1/4.

  4. Development of an acoustic wave based biosensor for vapor phase detection of small molecules (United States)

    Stubbs, Desmond

    For centuries scientific ingenuity and innovation have been influenced by Mother Nature's perfect design. One of her more elusive designs is that of the sensory olfactory system, an array of highly sensitive receptors responsible for chemical vapor recognition. In the animal kingdom this ability is magnified among canines where ppt (parts per trillion) sensitivity values have been reported. Today, detection dogs are considered an essential part of the US drug and explosives detection schemes. However, growing concerns about their susceptibility to extraneous odors have inspired the development of highly sensitive analytical detection tools or biosensors known as "electronic noses". In general, biosensors are distinguished from chemical sensors in that they use an entity of biological origin (e.g. antibody, cell, enzyme) immobilized onto a surface as the chemically-sensitive film on the device. The colloquial view is that the term "biosensors" refers to devices which detect the presence of entities of biological origin, such as proteins or single-stranded DNA and that this detection must take place in a liquid. Our biosensor utilizes biomolecules, specifically IgG monoclonal antibodies, to achieve molecular recognition of relatively small molecules in the vapor phase.

  5. Synthesis of functional materials by radiation

    Energy Technology Data Exchange (ETDEWEB)

    Nho, Young Chang; Kim, Ki Yup; Kang, Phil Hyun and others


    The radiation can induce chemical reaction to modify polymer under even the solid condition or in the low temperature. Therefore, the radiation processing is used as the means to develop the high functional polymer and new material which is impossible by chemical process. The radiation grafting process has the advantage to endow the adsorption function to the existing materials such as polymer membrane, fabric, non-fabric, non-woven fabric and film. Radiation crosslinking is effected with no pressure and is performed at low temperatures. Thus, temperature sensitive additives can be used in radiation crosslinking. The radiation crosslinking and grafting can be easily adjusted and is easily reproducible by controlling the radiation dose. The finished product contains no residuals of substances required to initiate the chemical crosslinking and grafting which can restrict the application possibilities, or can increase the failure rate. In these studies, radiation grafting and crosslinking were used to develop the toxic gas adsorbent, blood compatible polymer, acetabular cup of artificial joint, urokinase adsorbent, hydrogel, hollow fiber membrane adsorbing the heavy metals, and battery separator membrane. Because cable in nuclear power plant is directly related to safe operation, the life assessment of the cable system is an important issue. To assess the degradation and life time of cable is complicated owing to the various types and the different formulation of cable. In order to make an estimate the long term degradation occurring in a material, it is necessary to carry out the accelerated aging studies and to establish the appropriate test method to characterize the degradation. These studies are aimed at the evaluation technique on radiation degradation of polymer material and applying these results to nuclear equipment qualification.

  6. Mechanochemical synthesis of Fe-S materials

    DEFF Research Database (Denmark)

    Jiang, Jianzhong; Larsen, R.K.; Lin, R.


    Powder mixtures of metallic iron and sulfur have been milled in a high-energy planetary ball mill and the formation of iron sulfides has been studied by x-ray diffraction, Mossbauer spectroscopy, and scanning electron microscopy. For Fe:S ratios of 1:1 and 1:2 the final products are FeS with the ......Powder mixtures of metallic iron and sulfur have been milled in a high-energy planetary ball mill and the formation of iron sulfides has been studied by x-ray diffraction, Mossbauer spectroscopy, and scanning electron microscopy. For Fe:S ratios of 1:1 and 1:2 the final products are Fe......S with the modified NiAs structure and FeS2 (pyrite), respectively. No other iron sulfides were formed for any of the Fe:S ratios studied. The FeS phase has been tested as an electrode material in lithium batteries....

  7. Perspective: Toward “synthesis by design”: Exploring atomic correlations during inorganic materials synthesis

    Directory of Open Access Journals (Sweden)

    L. Soderholm


    Full Text Available Synthesis of inorganic extended solids is a critical starting point from which real-world functional materials and their consequent technologies originate. However, unlike the rich mechanistic foundation of organic synthesis, with its underlying rules of assembly (e.g., functional groups and their reactivities, the synthesis of inorganic materials lacks an underpinning of such robust organizing principles. In the latter case, any such rules must account for the diversity of chemical species and bonding motifs inherent to inorganic materials and the potential impact of mass transport on kinetics, among other considerations. Without such assembly rules, there is less understanding, less predictive power, and ultimately less control of properties. Despite such hurdles, developing a mechanistic understanding for synthesis of inorganic extended solids would dramatically impact the range of new material discoveries and resulting new functionalities, warranting a broad call to explore what is possible. Here we discuss our recent approaches toward a mechanistic framework for the synthesis of bulk inorganic extended solids, in which either embryonic atomic correlations or fully developed phases in solutions or melts can be identified and tracked during product selection and crystallization. The approach hinges on the application of high-energy x-rays, with their penetrating power and large Q-range, to explore reaction pathways in situ. We illustrate this process using two examples: directed assembly of Zr clusters in aqueous solution and total phase awareness during crystallization from K–Cu–S melts. These examples provide a glimpse of what we see as a larger vision, in which large scale simulations, data-driven science, and in situ studies of atomic correlations combine to accelerate materials discovery and synthesis, based on the assembly of well-defined, prenucleated atomic correlations.

  8. Development of a Rapid Cell-free Method for Cytotoxicity Assessment of Vapor Phase of Cigarette Smoke

    Directory of Open Access Journals (Sweden)

    Cahours X


    Full Text Available Currently, several in vitro tests are widely used to measure toxicological properties of mainstream smoke (Neutral Red Uptake Assay, Micronucleus assay, Ames Test. These tests are necessary to assess cytotoxicity, genotoxicity, and mutagenicity, but are time consuming. This is essentially due to the preparation and the handling of cells. It is difficult to use these in vitro tests as screening method for product testing and development. For a better assessment of the cytotoxicity of the vapor phase, a rapid cell-free method has been developed. This paper describes a capillary electrophoresis cell-free method, based on the depletion of an anti-oxidant L-gamma-glutamyl-L-cysteinylglycine (GSH, applied to an aliquot of vapor phase phosphate buffered saline (PBS-trapped cigarette smoke (as recommended for in vitro testing. The correlation between this method and the survival/viability test (Neutral Red cytotoxicity is excellent (coefficient of correlation (r = 0.99.

  9. Mechanochemical synthesis of nanocrystalline materials in an industrial mill

    Directory of Open Access Journals (Sweden)

    Eberhard Gock


    Full Text Available Nanosized materials are polycrystalline materials, whose crystal size is a few (typically 1-100 nanometers in at least one dimension. It has been proposed that as particles become smaller in size they may take on different chemical and physical properties. One of the most intriguing observations was that nanocrystals prepared by the altered “nano“ approach exhibited a higher surface chemical reactivity than more conventionally prepared samples. Nanocrystalline materials have many potential applications in the area of advanced materials. Their strongly size-dependent optical properties render them attractive candidates as tunable light absorbers and emitters in optoelectronic devices such as light-emitting diodes and quantum-dot lasers. These materials can be synthesized via solid state reactions where the efficiency of synthesis can be strongly enhanced by an intervention of high-energy milling (mechanochemical synthesis. The mechanochemical synthesis can effectively control and regulate the course of solid state reactions. Nanocrystalline materials MeS (Me=Pb, Zn, Cd, Cu were successfully synthesized by the mechanochemical route from the corresponding metal acetates and natrium sulphide in an industrial mill. Structure properties of the as-prepared products were characterized by the X-ray powder diffraction, revealing the crystalline nature of the MeS nanoparticles. The methods of TEM, particle size analysis and the low temperature nitrogen sorption were used to analyze the particle morphology and the surface composition. The average sizes of MeS particles of 4-18 nm were estimated by Scherrer´s formula. The nanocrystalline materials are obtained in the simple step, making the process attractive for industrial applications. The main advantage of the application of the industrial mill is that it is a “quantity” process, permitting kilograms of material to be produced at an ambient temperature in a very short processing time. Moreover

  10. Synthesis of Zeolite Materials for Noble Gas Separation

    Energy Technology Data Exchange (ETDEWEB)

    Achey, R. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Rivera, O. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Wellons, M. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Hunter, D. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)


    Microporous zeolite adsorbent materials are widely used as a medium for separating gases. Adsorbent gas separation systems can run at ambient temperature and require minimal pressure to flow the input gas stream across the adsorbent bed. This allows for low energy consumption relative to other types of separation systems. Specific zeolites also have a high capacity and selectivity for the gases of interest, leading to compact and efficient separation systems. These characteristics are particularly advantageous for the application of signatures detection for non-proliferation, which often requires portable systems with low power draw. Savannah River National Laboratory currently is the leader in using zeolites for noble gas sampling for non-proliferation detection platforms. However, there is a constant customer need for improved sampling capabilities. Development of improved zeolite materials will lead to improved sampling technology. Microwave-assisted and conventional hydrothermal synthesis have been used to make a variety of zeolites tailored for noble gas separation. Materials characterization data collected in this project has been used to help guide the synthesis of improved zeolite materials. Candidate materials have been down-selected based on highest available surface area, maximum overall capacity for gas adsorption and highest selectivity. The creation of improved adsorbent materials initiated in this project will lead to development of more compact, efficient and effective noble gas collectors and concentrators. The work performed in this project will be used as a foundation for funding proposals for further material development as well as possible industrial applications.

  11. Characterization of vapor phase mercury released from concrete processing with baghouse filter dust added cement. (United States)

    Wang, Jun; Hayes, Josh; Wu, Chang-Yu; Townsend, Timothy; Schert, John; Vinson, Tim; Deliz, Katherine; Bonzongo, Jean-Claude


    The fate of mercury (Hg) in cement processing and products has drawn intense attention due to its contribution to the ambient emission inventory. Feeding Hg-loaded coal fly ash to the cement kiln introduces additional Hg into the kiln's baghouse filter dust (BFD), and the practice of replacing 5% of cement with the Hg-loaded BFD by cement plants has recently raised environmental and occupational health concerns. The objective of this study was to determine Hg concentration and speciation in BFD as well as to investigate the release of vapor phase Hg from storing and processing BFD-added cement. The results showed that Hg content in the BFD from different seasons ranged from 0.91-1.44 mg/kg (ppm), with 62-73% as soluble inorganic Hg, while Hg in the other concrete constituents were 1-3 orders of magnitude lower than the BFD. Up to 21% of Hg loss was observed in the time-series study while storing the BFD in the open environment by the end of the seventh day. Real-time monitoring in the bench system indicated that high temperature and moisture can facilitate Hg release at the early stage. Ontario Hydro (OH) traps showed that total Hg emission from BFD is dictated by the air exchange surface area. In the bench simulation of concrete processing, only 0.4-0.5% of Hg escaped from mixing and curing BFD-added cement. A follow-up headspace study did not detect Hg release in the following 7 days. In summary, replacing 5% of cement with the BFD investigated in this study has minimal occupational health concerns for concrete workers, and proper storing and mixing of BFD with cement can minimize Hg emission burden for the cement plant.

  12. InGaAsP Solar Cells Grown by Hydride Vapor Phase Epitaxy

    Energy Technology Data Exchange (ETDEWEB)

    Jain, Nikhil; Simon, John; Schulte, Kevin L.; Dippo, Patricia; Young, Michelle; Young, David L.; Ptak, Aaron J.


    Hydride vapor phase epitaxy (HVPE) has recently reemerged as a low-cost, high-throughput alternative to metalorganic chemical vapor deposition (MOCVD) for the growth of high-efficiency III-V solar cells. Quaternary InGaAsP solar cells in the bandgap range of ~1.7-1.8 eV are promising top-cell candidates for integration in Ill-V/Si tandem cells with projected one-sun efficiencies exceeding 30%. In this work, we report on the development of lattice-matched InGaAsP solar cells grown on GaAs substrates via HVPE at very high growth rates of ~0.7 um/min. We demonstrate prototype 1.7 eV InGaAsP solar cells with an open-circuit voltage of 1.11 V. The short-circuit current is limited by the lack of a window layer in these early stage devices. The photo response of 1.7 InGaAsP solar cell with ~1.1 um thick base layer is found to be nearly insensitive to variation in p-type base doping concentration in the range from Na - 4x1016 to - 1x1017 cm-3, indicating an effective carrier collection length on the order of - 1.1 um or higher in our devices. These initial InGaAsP cell results are encouraging and highlight the viability of HVPE to produce mixed arsenide-phosphide solar cells grown lattice-matched on GaAs.

  13. Fabrication of polyimide shells by vapor phase deposition for use as ICF targets

    Energy Technology Data Exchange (ETDEWEB)

    Alfonso, E.L.; Tsai, F.Y.; Chen, S.H.; Gram, R.Q.; Harding, D.R. [Univ. of Rochester, NY (United States). Lab. for Laser Energetics


    Hollow polyimide shells, for use as ICF targets, were fabricated by co-depositing monomer precursors from the vapor phase onto bounced spherical mandrels. The process involved two stages: first, the deposited monomers (pyromellitic dianhydride and 4,4{prime}-oxydianiline) reacted on the mandrel surface to form polyamic acid; second, the mandrel was heated to 300 C to imidize the polyamic acid and to decompose the mandrel. During this latter process the decomposed mandrel diffused through the thermally stable coating, leaving a polyimide shell. Depositions were performed under low ({approximately}10{sup {minus}3} Torr) and high ({approximately}10{sup {minus}6} Torr) vacuum. Also, flat witness films of polyimide deposited on Si wafers and NaCl allowed the mechanical properties and chemical composition of the film during the heating cycle to be measured. Polyimide shells with diameters ranging from 700 to 950 {micro}m and wall thicknesses ranging from 2 to 13 {micro}m were produced. The shell`s sphericity was greater than 99%. Burst and buckle pressure tests on these shells yielded the estimated mechanical strength properties. The elastic modulus and tensile strength were {approximately}15 GPa and {approximately}300 MPa, respectively. The permeability of D{sub 2} through polyamic acid at 25 C was 7.4 {times} 10{sup {minus}17} mol{center_dot}m/m{sup 2}{center_dot}Pa{center_dot}s and increased to 6.4 {times} 10{sup {minus}16} mol{center_dot}m/m{sup 2}{center_dot}Pa{center_dot}s at 25 C upon curing the shell to 150 C. The permeability of D{sub 2} at 25 C through vapor-deposited polyimide flat films was measured to be 240 times greater than through the as-deposited polyamic acid, and about 7 times greater than through commercially available solution-cast Kapton.


    Energy Technology Data Exchange (ETDEWEB)

    Lynn E. Katz; Kerry A. Kinney; R.S. Bowman; E.J. Sullivan


    Co-produced water from the oil and gas industry accounts for a significant waste stream in the United States. It is by some estimates the largest single waste stream in the country, aside from nonhazardous industrial wastes. Characteristics of produced water include high total dissolved solids content, dissolved organic constituents such as benzene and toluene, an oil and grease component, and chemicals added during the oil-production process. While most of the produced water is disposed via reinjection, some of them must be treated to remove organic constituents before the water is discharged. Current treatment options are successful in reducing the organic content; however, they cannot always meet the levels of current or proposed regulations for discharged water. Therefore, an efficient, cost-effective treatment technology is needed. Surfactant-modified zeolite (SMZ) has been used successfully to treat contaminated ground water for organic and inorganic constituents. In addition, the low cost of natural zeolites makes their use attractive in water-treatment applications. Our previous DOE research work (DE-AC26-99BC15221) demonstrated that SMZ could successfully remove BTEX compounds from the produced water. In addition, SMZ could be regenerated through a simple air sparging process. The primary goal of this project is to develop a robust SMZ/VPB treatment system to efficiently remove the organic constituents from produced water in a cost-effective manner. This report summarizes work of this project from October 2002 to March 2003. In this starting stage of this study, we have continued our investigation of SMZ regeneration from our previous DOE project. Two saturation/stripping cycles have been completed for SMZ columns saturated with BTEX compounds. Preliminary results suggest that BTEX sorption actually increases with the number of saturation/regeneration cycles. Furthermore, the experimental vapor phase bioreactors for this project have been designed and are

  15. Advanced Life Support Water Recycling Technologies Case Studies: Vapor Phase Catalytic Ammonia Removal and Direct Osmotic Concentration (United States)

    Flynn, Michael


    Design for microgravity has traditionally not been well integrated early on into the development of advanced life support (ALS) technologies. NASA currently has a many ALS technologies that are currently being developed to high technology readiness levels but have not been formally evaluated for microgravity compatibility. Two examples of such technologies are the Vapor Phase Catalytic Ammonia Removal Technology and the Direct Osmotic Concentration Technology. This presentation will cover the design of theses two systems and will identify potential microgravity issues.

  16. Adsorptive water removal from dichloromethane and vapor-phase regeneration of a molecular sieve 3A packed bed


    Jovic, S Slavisa; Laxminarayan, Y; Keurentjes, JTF Jos; Schouten, JC Jaap; Schaaf, van der, S.


    The drying of dichloromethane with a molecular sieve 3A packed bed process is modeled and experimentally verified. In the process, the dichloromethane is dried in the liquid phase and the adsorbent is regenerated by water desorption with dried dichloromethane product in the vapor phase. Adsorption equilibrium experiments show that dichloromethane does not compete with water adsorption, because of size exclusion; the pure water vapor isotherm from literature provides an accurate representation...

  17. Synthesis Methods of Carbon Nanotubes and Related Materials

    Directory of Open Access Journals (Sweden)

    Andrea Szabó


    Full Text Available The challenge on carbon nanotubes is still the subject of many research groups. While in the first years the focus was on the new synthesis methods, new carbon sources and support materials, recently, the application possibilities are the principal arguments of the studies. The three main synthesis methods discussed in this review are the arc discharge, the laser ablation and the chemical vapour deposition (CVD with a special regard to the latter one. In the early stage of the nanotube production the first two methods were utilized mainly for the production of SWNTs while the third one produced mainly MWNTs. The principle of CVD is the decomposition of various hydrocarbons over transition metal supported catalyst. Single-walled (SWNT, multi-walled (MWNT and coiled carbon nanotubes are produced. In some case, interesting carbonaceous materials are formed during the synthesis process, such as bamboo-like tubes, onions, horn-like structures. In this paper, we refer to the progresses made in the field of the synthesis techniques of carbon nanotubes in the last decade.

  18. Synthesis Methods of Carbon Nanotubes and Related Materials (United States)

    Szabó, Andrea; Perri, Caterina; Csató, Anita; Giordano, Girolamo; Vuono, Danilo; Nagy, János B.


    The challenge on carbon nanotubes is still the subject of many research groups. While in the first years the focus was on the new synthesis methods, new carbon sources and support materials, recently, the application possibilities are the principal arguments of the studies. The three main synthesis methods discussed in this review are the arc discharge, the laser ablation and the chemical vapour deposition (CVD) with a special regard to the latter one. In the early stage of the nanotube production the first two methods were utilized mainly for the production of SWNTs while the third one produced mainly MWNTs. The principle of CVD is the decomposition of various hydrocarbons over transition metal supported catalyst. Single-walled (SWNT), multi-walled (MWNT) and coiled carbon nanotubes are produced. In some case, interesting carbonaceous materials are formed during the synthesis process, such as bamboo-like tubes, onions, horn-like structures. In this paper, we refer to the progresses made in the field of the synthesis techniques of carbon nanotubes in the last decade.

  19. The effect of heated vapor-phase acidification on organic carbon concentrations and isotopic values in geologic rock samples (United States)

    Wang, R. Z.; West, A. J.; Yager, J. A.; Rollins, N.; Li, G.; Berelson, W.


    Carbon signatures recorded in the modern and geologic rock record can give insight on the Earth's carbon cycle through time. This is especially true for organic carbon (OC), which can help us understand how the biosphere has evolved over Earth's history. However, carbon recorded in rocks is a combination of OC and inorganic carbon (IC) mostly in the form of carbonate minerals. To measure OC, IC must therefore first be removed through a process called "decarbonation." This is often done through a leaching process with hydrochloric acid (HCl). However, three well known problems exist for the decarbonation process: 1) Incomplete removal of IC, 2) Unintentional removal of OC, and 3) Addition of false carbon blank. Currently, vapor (gas) phase removal of OC is preferred to liquid phase treatment because it has been shown that OC is lost to solubilization during liquid phase acidification. Vapor phase treatment is largely thought to avoid the problem of OC loss, but this has not yet been rigorously investigated. This study investigates that assumption and shows that vapor phase treatment can cause unintentional OC loss. We show that vapor phase treatment must be sensitive to rock type and treatment length to produce robust OC isotopic measurements and concentrations.

  20. Simultaneous Determination of Furan and Vinyl Acetate in Vapor Phase of Mainstream Cigarette Smoke by GC-MS

    Directory of Open Access Journals (Sweden)


    Full Text Available ABSTRACT A simple and sensitive method for simultaneous determination of furan and vinyl acetate (VA in vapor phase of mainstream cigarette smoke with cold trap and gas chromatography-mass spectrometry (GC-MS was developed. A Cambridge filter pad (CFP was placed in front of the impingers of smoking machine to remove the particle phase from cigarette smoke. Furan and VA in vapor phase of mainstream cigarette smoke were collected in two impingers connected in series by filled with methanol at -78°C. The solutions were added with deuterium-labeled furan-d4 and VA-d6 as internal standards and analyzed by GC-MS. The results showed that the calibration curves for furan and VA were linear (r2 > 0.9995 over the studied concentration range. The intra- and inter-day precision values for furan and VA were <7.07% and <9.62%, respectively. The extraction recoveries of furan and VA were in the range of 94.5-97.7% and 92.3-94.9%, respectively. Moreover, the limits of detection for furan and VA were 0.028 µg mL-1 and 1.3 ng mL-1, respectively. The validated method has been successfully applied to determine the emissions of furan and VA in the vapor phase of mainstream cigarette smoke under International Organization for Standardization (ISO and Canadian Intense (CI smoking regimen.

  1. Synthesis, Properties and Mineralogy of Important Inorganic Materials

    DEFF Research Database (Denmark)

    Warner, Terence Edwin

    , ferroelectric, thermoelectric, luminescent, photochromic and magnetic materials; are technologically important classes of material, that are represented by numerous inorganic phases. Yet how many of us are aware of their precise chemical compositions, and have sufficient knowledge to actually make them......The synthesis of high quality material is an essential step in the process of obtaining meaningful information about the material’s properties, and therefore, is an important link between physics and chemistry. Semiconductors; superconductors; solid-electrolytes; glasses; pigments; dielectric......? This book attempts to address this problem by offering the reader clear and detailed descriptions on how to prepare a selection of fifteen inorganic materials that exhibit important optical, magnetic, electrical and thermal properties; on a laboratory scale. The materials and chemical syntheses have been...

  2. Graphene-based materials: synthesis, characterization, properties, and applications. (United States)

    Huang, Xiao; Yin, Zongyou; Wu, Shixin; Qi, Xiaoying; He, Qiyuan; Zhang, Qichun; Yan, Qingyu; Boey, Freddy; Zhang, Hua


    Graphene, a two-dimensional, single-layer sheet of sp(2) hybridized carbon atoms, has attracted tremendous attention and research interest, owing to its exceptional physical properties, such as high electronic conductivity, good thermal stability, and excellent mechanical strength. Other forms of graphene-related materials, including graphene oxide, reduced graphene oxide, and exfoliated graphite, have been reliably produced in large scale. The promising properties together with the ease of processibility and functionalization make graphene-based materials ideal candidates for incorporation into a variety of functional materials. Importantly, graphene and its derivatives have been explored in a wide range of applications, such as electronic and photonic devices, clean energy, and sensors. In this review, after a general introduction to graphene and its derivatives, the synthesis, characterization, properties, and applications of graphene-based materials are discussed. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Treatment of Produced Water Using a Surfactant Modified Zeolite/Vapor Phase Bioreactor System

    Energy Technology Data Exchange (ETDEWEB)

    Lynn E. Katz; Kerry A. Kinney; Robert S. Bowman; Enid J. Sullivan; Soondong Kwon; Elaine B. Darby; Li-Jung Chen; Craig R. Altare


    Co-produced water from the oil and gas industry accounts for a significant waste stream in the United States. Produced waters typically contain a high total dissolved solids content, dissolved organic constituents such as benzene and toluene, an oil and grease component as well as chemicals added during the oil-production process. It has been estimated that a total of 14 billion barrels of produced water were generated in 2002 from onshore operations (Veil, 2004). Although much of this produced water is disposed via reinjection, environmental and cost considerations can make surface discharge of this water a more practical means of disposal. In addition, reinjection is not always a feasible option because of geographic, economic, or regulatory considerations. In these situations, it may be desirable, and often necessary from a regulatory viewpoint, to treat produced water before discharge. It may also be feasible to treat waters that slightly exceed regulatory limits for re-use in arid or drought-prone areas, rather than losing them to reinjection. A previous project conducted under DOE Contract DE-AC26-99BC15221 demonstrated that surfactant modified zeolite (SMZ) represents a potential treatment technology for produced water containing BTEX. Laboratory and field experiments suggest that: (1) sorption of benzene, toluene, ethylbenzene and xylenes (BTEX) to SMZ follows linear isotherms in which sorption increases with increasing solute hydrophobicity; (2) the presence of high salt concentrations substantially increases the capacity of the SMZ for BTEX; (3) competitive sorption among the BTEX compounds is negligible; and, (4) complete recovery of the SMZ sorption capacity for BTEX can be achieved by air sparging the SMZ. This report summarizes research for a follow on project to optimize the regeneration process for multiple sorption/regeneration cycles, and to develop and incorporate a vapor phase bioreactor (VPB) system for treatment of the off-gas generated during

  4. Synthesis and self-assembly of complex hollow materials

    KAUST Repository

    Zeng, Hua Chun


    Hollow materials with interiors or voids and pores are a class of lightweight nanostructured matters that promise many future technological applications, and they have received significant research attention in recent years. On the basis of well-known physicochemical phenomena and principles, for example, several solution-based protocols have been developed for the general preparation of these complex materials under mild reaction conditions. This article is thus a short introductory review on the synthetic aspects of this field of development. The synthetic methodologies can be broadly divided into three major categories: (i) template-assisted synthesis, (ii) self-assembly with primary building blocks, and (iii) induced matter relocations. In most cases, both synthesis and self-assembly are involved in the above processes. Further combinations of these methodologies appear to be very important, as they will allow one to prepare functional materials at a higher level of complexity and precision. The synthetic strategies are introduced through some simple case studies with schematic illustrations. Salient features of the methods developed have been summarized, and some urgent issues of this field have also been indicated. © 2011 The Royal Society of Chemistry.

  5. Treatment of Produced Waters Using a Surfactant Modified Zeolite/Vapor Phase Bioreactor System

    Energy Technology Data Exchange (ETDEWEB)

    Soondong Kwon; Elaine B. Darby; Li-Jung Chen; Lynn E. Katz; Kerry A. Kinney; R. S. Bowman; E. J. Sullivan


    second residence time, the GAC bed reduced peak contaminant concentrations by 97%. After the initial peak, the inlet VOC concentration in the SMZ regeneration gas stream drops exponentially with time. During this period, the contaminants on the GAC subsequently desorbed at a nearly steady rate over the next 45 hours resulting in a relatively steady effluent concentration of approximately 25 ppm{sub v}. This lower concentration is readily degradable by a downstream vapor phase biofilter (VPB) and the steady nature of the feed stream will prevent the biomass in the VPB from enduring starvation conditions between SMZ regeneration cycles. Repetitive sorption and desorption cycles that would be expected in the field were also investigated. It was determined that although the GAC initially lost some VOC sorption capacity, the adsorption and desorption profiles stabilized after approximately 6 cycles indicating that a GAC bed should be suitable for continuous operation. In preparation for the pilot field testing of the SMZ/VPB system, design, ''in-house'' construction and testing of the field system were completed during this project period. The design of the SMZ system for the pilot test was based on previous investigations by the PI's in Wyoming, 2002 and on analyses of the produced water at the field site in New Mexico. The field tests are scheduled for summer, 2005. A cost survey, feasibility of application and cost analyses were completed to investigate the long term effectiveness of the SMZ/VPB system as a method of treating produced water for re-use. Several factors were investigated, including: current costs to treat and dispose of produced water, end-use water quality requirements, and state and federal permitting requirements.

  6. Identification of vapor-phase chemical warfare agent simulants and rocket fuels using laser-induced breakdown spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Stearns, Jaime A.; McElman, Sarah E.; Dodd, James A.


    Application of laser-induced breakdown spectroscopy (LIBS) to the identification of security threats is a growing area of research. This work presents LIBS spectra of vapor-phase chemical warfare agent simulants and typical rocket fuels. A large dataset of spectra was acquired using a variety of gas mixtures and background pressures and processed using partial least squares analysis. The five compounds studied were identified with a 99% success rate by the best method. The temporal behavior of the emission lines as a function of chamber pressure and gas mixture was also investigated, revealing some interesting trends that merit further study.

  7. Growth of Cd0.96Zn0.04Te single crystals by vapor phase gas transport method

    Directory of Open Access Journals (Sweden)

    S. H. Tabatabai Yazdi


    Full Text Available   Cd0.96Zn0.04Te crystals were grown using vapor phase gas transport method (VPGT. The results show that dendritic crystals with grain size up to 3.5 mm can be grown with this technique. X-ray diffraction and Laue back-reflection patterns show that dendritic crystals are single-phase, whose single crystal grains are randomly oriented with respect to the gas-transport axis. Electrical measurements, carried out using Van der Pauw method, show that the as-grown crystals have resistivity of about 104 Ω cm and n-type conductivity.

  8. Growth of low-threading-dislocation-density GaN on graphene by hydride vapor phase epitaxy (United States)

    He, Shunyu; Xu, Yu; Qi, Lin; Li, Zongyao; Cao, Bing; Wang, Chinhua; Zhang, Jicai; Wang, Jianfeng; Xu, Ke


    Recently, gallium nitride (GaN) films grown on graphene have been widely studied. Here, we have grown low-threading-dislocation-density GaN films on graphene by hydride vapor phase epitaxy (HVPE). The full widths at half maximum (FWHMs) of X-ray rocking curves (XRCs) of the GaN films were 276 and 350 arcsec at the 0002 and 10\\bar{1}2 reflections, respectively. This shows that the threading dislocation densities are on the order of magnitude of 108 cm-2, which is consistent with the results of cathodoluminescence (CL).

  9. Mathematical Modelling of the Synthesis of New Materials

    Directory of Open Access Journals (Sweden)

    Antonov Valery


    Full Text Available The paper focuses primarily on a magnetohydrodynamical approach to solving the numerical problems arising in studying the high energy input technologies of the synthesis of new materials. The underlining mathematical model combines the description of both electromagnetic and hydrodynamic phenomena for the metals and surrounding media in supercritical conditions. A detailed specification of this model is provided. The crucial role of the correct choice of equation of state is outlined. The results section includes the latest finding regarding the numerical simulation of underwater electrical explosion.

  10. Aerosol Route Synthesis and Applications of Doped Nanostructured Materials (United States)

    Sahu, Manoranjan

    Nanotechnology presents an attractive opportunity to address various challenges in air and water purification, energy, and other environment issues. Thus, the development of new nanoscale materials in low-cost scalable synthesis processes is important. Furthermore, the ability to independently manipulate the material properties as well as characterize the material at different steps along the synthesis route will aide in product optimization. In addition, to ensure safe and sustainable development of nanotechnology applications, potential impacts need to be evaluated. In this study, nanomaterial synthesis in a single-step gas phase reactor to continuously produce doped metal oxides was demonstrated. Copper-doped TiO2 nanomaterial properties (composition, size, and crystal phase) were independently controlled based on nanoparticle formation and growth mechanisms dictated by process control parameters. Copper dopant found to significantly affect TiO2 properties such as particle size, crystal phase, stability in the suspension, and absorption spectrum (shift from UV to visible light absorption). The in-situ charge distribution characterization of the synthesized nanomaterials was carried out by integrating a tandem differential mobility analyzer (TDMA) set up with the flame reactor synthesis system. Both singly- and doubly- charged nanoparticles were measured, with the charged fractions dependent on particle mobility and dopant concentration. A theoretical calculation was conducted to evaluate the relative importance of the two charging mechanisms, diffusion and thermo-ionization, in the flame. Nanoparticle exposure characterization was conducted during synthesis as a function of operating condition, product recovery and handling technique, and during maintenance of the reactors. Strategies were then indentified to minimize the exposure risk. The nanoparticle exposure potential varied depending on the operating conditions such as precursor feed rate, working

  11. Antibacterial effects of allspice, garlic, and oregano essential oils in tomato films determined by overlay and vapor-phase methods. (United States)

    Du, W-X; Olsen, C W; Avena-Bustillos, R J; McHugh, T H; Levin, C E; Mandrell, R; Friedman, Mendel


    Physical properties as well as antimicrobial activities against Escherichia coli O157:H7, Salmonella enterica, and Listeria monocytogenes of allspice, garlic, and oregano essential oils (EOs) in tomato puree film-forming solutions (TPFFS) formulated into edible films at 0.5% to 3% (w/w) concentrations were investigated in this study. Antimicrobial activities were determined by 2 independent methods: overlay of the film on top of the bacteria and vapor-phase diffusion of the antimicrobial from the film to the bacteria. The results indicate that the antimicrobial activities against the 3 pathogens were in the following order: oregano oil > allspice oil > garlic oil. Listeria monocytogenes was less resistant to EO vapors, while E. coli O157:H7 was more resistant to EOs as determined by both overlay and vapor-phase diffusion tests. The presence of plant EO antimicrobials reduced the viscosity of TPFFS at the higher shear rates, but did not affect water vapor permeability of films. EOs increased elongation and darkened the color of films. The results of the present study show that the 3 plant-derived EOs can be used to prepare tomato-based antimicrobial edible films with good physical properties for food applications by both direct contact and indirectly by vapors emanating from the films.

  12. Synthesis, Characterization and Application of Multiscale Porous Materials

    Energy Technology Data Exchange (ETDEWEB)

    Hussami, Linda


    This thesis work brings fresh insights and improved understanding of nano scale materials through introducing new hybrid composites, 2D hexagonal in MCM-41 and 3D random interconnected structures of different materials, and application relevance for developing fields of science, such as fuel cells and solar cells. New types of porous materials and organometallic crystals have been prepared and characterized in detail. The porous materials have been used in several studies: as hosts to encapsulate metal-organic complexes; as catalyst supports and electrode materials in devices for alternative energy production. The utility of the new porous materials arises from their unique structural and surface chemical characteristics as demonstrated here using various experimental and theoretical approaches. New single crystal structures and arene-ligand exchange properties of f-block elements coordinated to ligand arene and halogallates are described in Paper I. These compounds have been incorporated into ordered 2D-hexagonal MCM-41 and polyhedral silica nano foam (PNF-SiO{sub 2}) matrices without significant change to the original porous architectures as described in Paper II and III. The resulting inorganic/organic hybrids exhibited enhanced luminescence activity relative to the pure crystalline complexes. A series of novel polyhedral carbon nano foams (PNF-C's) and inverse foams were prepared by nano casting from PNF-SiO{sub 2}'s. These are discussed in Paper IV. The synthesis conditions of PNF-C's were systematically varied as a function of the filling ratio of carbon precursor and their structures compared using various characterization methods. The carbonaceous porous materials were further tested in Paper V and VI as possible catalysts and catalyst supports in counter- and working electrodes for solar- and fuel cell applications

  13. Controlling the polarity of metalorganic vapor phase epitaxy-grown GaP on Si(111) for subsequent III-V nanowire growth

    Energy Technology Data Exchange (ETDEWEB)

    Paszuk, A.; Steidl, M.; Zhao, W.; Dobrich, A.; Kleinschmidt, P. [Technische Universität Ilmenau, Institut für Physik, 98693 Ilmenau (Germany); Brückner, S.; Supplie, O.; Hannappel, T. [Technische Universität Ilmenau, Institut für Physik, 98693 Ilmenau (Germany); Helmholtz-Zentrum Berlin, Institute for Solar Fuels, 14109 Berlin (Germany); Prost, W. [Center for Semiconductor Technology and Optoelectronics (ZHO), University of Duisburg-Essen, 47057 Duisburg (Germany)


    Nanowire growth on heteroepitaxial GaP/Si(111) by metalorganic vapor phase epitaxy requires the [-1-1-1] face, i.e., GaP(111) material with B-type polarity. Low-energy electron diffraction (LEED) allows us to identify the polarity of GaP grown on Si(111), since (2×2) and (1×1) surface reconstructions are associated with GaP(111)A and GaP(111)B, respectively. In dependence on the pre-growth treatment of the Si(111) substrates, we were able to control the polarity of the GaP buffers. GaP films grown on the H-terminated Si(111) surface exhibited A-type polarity, while GaP grown on Si surfaces terminated with arsenic exhibited a (1×1) LEED pattern, indicating B-type polarity. We obtained vertical GaAs nanowire growth on heteroepitaxial GaP with (1×1) surface reconstruction only, in agreement with growth experiments on homoepitaxially grown GaP(111)

  14. Strained In1-xGaxAsyP1-y/InP quantum well heterostructures grown by low-pressure metalorganic vapor phase epitaxy

    Directory of Open Access Journals (Sweden)

    Carvalho Jr Wilson de


    Full Text Available We have investigated the optical and the structural properties of strained In1-xGaxAsyP1-y/InP and strain compensated In1-xGaxAsyP1-y/In1-zGazAsqP1-q/InP multi-quantum well heterostructures grown by low-pressure metalorganic vapor phase epitaxy at different growth conditions. Our results indicate an increase of the compositional fluctuation of quaternary materials as the alloy composition moves from the outer spinodal isotherm into the miscibility gap region. In1-xGaxAsyP1-y layers grown at high tensile strained values exhibit a three-dimensional-like growth mode. Strain compensated structures revealed the presence of a broad photoluminescence emission band below the fundamental quantum well transition, well defined elongated features along the [011] direction and interface undulations. All these effects were found to be strongly dependent on the growth temperature and the number of wells.

  15. Multiphase microfluidics: from flow characteristics to chemical and materials synthesis. (United States)

    Günther, Axel; Jensen, Klavs F


    We review transport characteristics of pressure-driven, multiphase flows through microchannel networks tens of nanometres to several hundred of micrometres wide with emphasis on conditions resulting in enhanced mixing and reduced axial dispersion. Dimensionless scaling parameters useful in characterizing multiphase flows are summarized along with experimental flow visualization techniques. Static and dynamic stability considerations are also included along with methods for stabilizing multiphase flows through surface modifications. Observed gas-liquid and immiscible liquid-liquid flows are summarized in terms of flow regime diagrams and the different flows are related to applications in chemistry and materials synthesis. Means to completely separate multiphase flows on the microscale and guidelines for design of scalable multiphase systems are also discussed.

  16. Materials production and synthesis/2005 MT-0.3201. Proceedings

    Energy Technology Data Exchange (ETDEWEB)

    Kekkonen, M. (ed.)


    In order to promote internationalisation of metallurgy students a co-operation was started between Helsinki University of Technology (TKK) and Royal Institute of Technology (KTH), Stockholm in 1996. As a collaboration form joint student seminars on process metallurgy were decided to be arranged once a year. The first seminar was held at Helsinki University of Technology (TKK), and then in turn at K{sup I}'II and TKK. Since 1998 a third partner was received when the metallurgy students of Professor Ken Mills at Imperial College of Science, Technology and Medicine (ICSTM), London U.K. attended the seminars until the year 2000, when due to the retirement of Ken Mills, ICSTM withdraw from the co-operation. As a new partner, NTNU, Trondheim Norway joined the group in the autumn 2001 after which the seminar was twice arranged in Trondheim in 2001 and 2004 hosted by Professor Leis Kolbeinsen and his colleagues. Initiated by the Bologna Process many changes in the education programme and its structure were carried out in 2005. At TKK the seminar course belongs now to Materials Production and synthesis course. The general aim is to improve the students' knowledge on central pyro- and hvdrouictallurgical processes, their thermodynamic, kinetic, physical and electrochemical basis. The course comprises of a series of lectures on selected topics e.g. novel processes in ferrous and non-ferrous metallurgy, hydrometallurgical processes and materials synthesis. The course is driven by three professor chairs all giving a few lectures and then supervising seminar working. As earlier, the main emphasis is still directed to conduct students to prepare scientific contributions both as written and oral presentations. Accordingly, the students have prepared a report on a given topic and they give an oral contribution in the seminar with discussion and criticism. This year the seminar will be held at KTH on November 28-29, 2005.

  17. Prediction, synthesis and characterization of new topological materials (United States)

    Gibson, Quinn Davis

    Over the past few years, a rediscovery of the concept of topology as it applies to the electronic structure of materials has created an explosion of research and discovery of new materials properties. While this field has been mainly of interest to the condensed matter physics community, this work explores it from a materials chemistry perspective, to both develop new materials, via a combination of computation, synthesis and measurement, to understand how the electronic topology can relate to structure and bonding. As such, adding chemical complexity to existing topological materials has been a focus of this study. In order to expand upon the archetypal topological insulator family of Bi2X3 (X=Se,Te), the super lattice materials, which contain alternating layers of Bi2 or Sb2 and Bi 2X3 or Sb2Te3, were investigated, revealing novel properties. The compound Bi4Se3 was shown to have termination dependent surface states, revealing a relationship between the nature of the surface states and the chemical nature of the surface, as well as novel mirror symmetry protected surface states. The 2:1 family (in the Sb2Te structure) were shown to be new topological insulators, with a novel Sb/Bi ordering when Bi is substituted for Sb in Sb2Te. Finally the 1:1 family was shown to, unexpectedly, be strong topological insulators, despite the theoretical prediction that they are weak topological insulators. Furthermore, other materials families were investigated as topological insulators, such as the chimney ladder family. Ir4Ge5 is identified as a likely candidate, and Ru2Sn3 was shown to have novel, quasi one-dimensional surface states. The exact reason for the existence of these states is not known and is under investigation. Finally, possible 3D Dirac and Weyl semi-metals were investigated. A set of rules to predict 3D Dirac semi-metals were developed, and Cd3 As2 was experimentally verified as the first of this kind of material. Studies towards Weyl semi-metals involved the

  18. Material synthesis and evaluation of metrological characteristics of potassium fluozirconate certified reference material

    Directory of Open Access Journals (Sweden)

    D. G. Lisienko


    Full Text Available The relevance of the study. For metrological support of control methods for composition ofpotassium fluozirconate, used in the production of metallic zirconium, applied in various technical fields, including nuclear power, electronics, chemical engineering. The purpose: development of synthesis technology, and determination of metrological characteristics of certified reference material for composition ofpotassium fluozirconate (set, intended for metrological support of measuring element mass fraction: hafnium (Hf, silicon (Si, iron (Fe, aluminium (Al, chromium (Cr, tin (Sn, titanium (Ti in potassium fluozirconate. Research methods: X-ray diffraction, differential scanning colorimetry, thermogravimetric analysis, atomic-emission spectral analysis with arc excitation, mass spectral analysis, X-ray fluorescence analysis. Results. As a result of research a set of certified reference materials for composition of potassium fluozirconate is developed and produced. The CRM type is approved by Federal Agency on Technical Regulating and Metrology and registered in State Register of Approved Reference Material Types under number GSO 10593-2015.

  19. Characterization of (211) and (100) CdTe Layers Grown on Si Substrates by Metalorganic Vapor-Phase Epitaxy (United States)

    Yasuda, K.; Niraula, M.; Kojima, M.; Kitagawa, S.; Tsubota, S.; Yamaguchi, T.; Ozawa, J.; Agata, Y.


    Single-crystal (211) and (100) CdTe layers have been grown by metalorganic vapor-phase epitaxy using the same condition on (211) and (100) Si substrates, respectively. Prior to the growth, substrates of both orientations were pretreated using the same pretreatment procedure. The crystal qualities of the grown layers were evaluated by full-width at half-maximum values of double-crystal x-ray rocking curves, and photoluminescence spectra at 4.2 K. (211) CdTe layers showed better crystallinity than (100) layers. The crystal quality of the (100) CdTe layers was also compared with that of layers grown on an epitaxial (100) GaAs layer on Si substrate. The results suggest that (100) CdTe layers with improved crystal quality could be obtained by optimizing the procedure of the Si substrates.

  20. ZnO/Cu(InGa)Se.sub.2 solar cells prepared by vapor phase Zn doping (United States)

    Ramanathan, Kannan; Hasoon, Falah S.; Asher, Sarah E.; Dolan, James; Keane, James C.


    A process for making a thin film ZnO/Cu(InGa)Se.sub.2 solar cell without depositing a buffer layer and by Zn doping from a vapor phase, comprising: depositing Cu(InGa)Se.sub.2 layer on a metal back contact deposited on a glass substrate; heating the Cu(InGa)Se.sub.2 layer on the metal back contact on the glass substrate to a temperature range between about C. to about C.; subjecting the heated layer of Cu(InGa)Se.sub.2 to an evaporant species from a Zn compound; and sputter depositing ZnO on the Zn compound evaporant species treated layer of Cu(InGa)Se.sub.2.

  1. Significance of vapor phase chemical reactions on CVD rates predicted by chemically frozen and local thermochemical equilibrium boundary layer theories (United States)

    Gokoglu, Suleyman A.


    This paper investigates the role played by vapor-phase chemical reactions on CVD rates by comparing the results of two extreme theories developed to predict CVD mass transport rates in the absence of interfacial kinetic barrier: one based on chemically frozen boundary layer and the other based on local thermochemical equilibrium. Both theories consider laminar convective-diffusion boundary layers at high Reynolds numbers and include thermal (Soret) diffusion and variable property effects. As an example, Na2SO4 deposition was studied. It was found that gas phase reactions have no important role on Na2SO4 deposition rates and on the predictions of the theories. The implications of the predictions of the two theories to other CVD systems are discussed.

  2. Biomass-based composites from poly(lactic acid) and wood flour by vapor-phase assisted surface polymerization. (United States)

    Kim, Donghee; Andou, Yoshito; Shirai, Yoshihito; Nishida, Haruo


    To prepare biomass-based composites in an environmentally benign manner, vapor-phase assisted surface polymerization (VASP) was applied to prepare the composites from wood flour and poly(l-lactic acid) (PLLA) without solvent. VASP of l,l-lactide successfully proceeded on the wood flour surfaces, resulting in surface coverage by newly generated PLLA. For obtained PLLA/wood flour composites, it was clarified that grafting of PLLA on wood flour surfaces had occurred to form covalently bonded composites, with the accumulated PLLA layers having crystallized in situ during VASP. Resulting PLLA layers showed very high crystallinity of 79.2% and a high melting point close to the equilibrium melting point. Moreover, thermal degradation behavior of the composites suggested a cooperative degradation manner of the components.

  3. Adsorptive Water Removal from Dichloromethane and Vapor-Phase Regeneration of a Molecular Sieve 3A Packed Bed. (United States)

    Jović, Slaviša; Laxminarayan, Yashasvi; Keurentjes, Jos; Schouten, Jaap; van der Schaaf, John


    The drying of dichloromethane with a molecular sieve 3A packed bed process is modeled and experimentally verified. In the process, the dichloromethane is dried in the liquid phase and the adsorbent is regenerated by water desorption with dried dichloromethane product in the vapor phase. Adsorption equilibrium experiments show that dichloromethane does not compete with water adsorption, because of size exclusion; the pure water vapor isotherm from literature provides an accurate representation of the experiments. The breakthrough curves are adequately described by a mathematical model that includes external mass transfer, pore diffusion, and surface diffusion. During the desorption step, the main heat transfer mechanism is the condensation of the superheated dichloromethane vapor. The regeneration time is shortened significantly by external bed heating. Cyclic steady-state experiments demonstrate the feasibility of this novel, zero-emission drying process.

  4. Characteristics of stimulated emission from optically pumped freestanding GaN grown by hydride vapor-phase epitaxy

    CERN Document Server

    Lee, M H; Kim, S T; Chung, S H; Moon, D C


    In this study, we observed optically pumped stimulated emission at room temperature in quasi-bulk GaN prepared from thick-film GaN grown on a sapphire substrate by using hydride vapor-phase epitaxy and subsequent mechanical removal of the sapphire substrate. The stimulated emission from the surface and 1-mm-wide-cleaved cavity of the GaN was red-shifted compared to the spontaneous emission by increasing the optical pumping-power density, and the full width at half maximum (FWHM) of the peak decreased. The stimulated emission was demonstrated to have a highly TE-mode polarized nature, and the super-linear dependence of the integrated emission intensity on the excitation power indicated a threshold pump-power density of I sub t sub h = 2 MW/cm sup 2 for one set of stimulated emissions.

  5. Direct Growth of CdTe on a (211) Si Substrate with Vapor Phase Epitaxy Using a Metallic Cd Source (United States)

    Iso, Kenji; Gokudan, Yuya; Shiraishi, Masumi; Murakami, Hisashi; Koukitu, Akinori


    We successfully performed epitaxial CdTe growth on a Si (211) substrate with vapor-phase epitaxy using a cost-effective metallic cadmium source as a group-II precursor. The thermodynamic data demonstrate that the combination of metallic Cd and diisopropyl-telluride (DiPTe) with a H2 carrier gas enables the growth of CdTe crystals. A CdTe single crystal with a (422) surface orientation was obtained when a growth temperature between 600°C and 650°C was employed. The surface morphology and crystalline quality were improved with increasing film thickness. The full-width at half-maximum of the x-ray rocking curves with a film thickness of 15.7 μm for the skew-symmetrical (422) and asymmetrical (111) reflection were 528 arcsec and 615 arcsec, respectively.

  6. Growth of GaN on ZrB 2 substrate by metal-organic vapor phase epitaxy (United States)

    Tomida, Yoshihito; Nitta, Shugo; Kamiyama, Satoshi; Amano, Hiroshi; Akasaki, Isamu; Otani, Shigeki; Kinoshita, Hiroyuki; Liu, Rong; Bell, Abigail; Ponce, Fernando A.


    Growth of GaN by metal-organic vapor phase epitaxy (MOVPE) on metallic zirconium diboride (ZrB 2) substrate was investigated. Cross-sectional transmission electron microscopy (TEM) showed that cubic ZrB xN 1- x is formed on the surface when ZrB 2 is exposed to ammonia-containing atmosphere, which protects the nucleation of GaN or AlN. We solved the problem by covering ZrB 2 surface with very thin AlN or GaN at low temperature, thereby achieving high-quality GaN growth with a dislocation density less than 10 8 cm -2. Direct conduction was achieved through the back of ZrB 2 and the surface of Si-doped GaN.

  7. Vapor-phase hydrothermal transformation of HTiOF3 intermediates into {001} faceted anatase single-crystalline nanosheets. (United States)

    Liu, Porun; Wang, Yun; Zhang, Haimin; An, Taicheng; Yang, Huagui; Tang, Zhiyong; Cai, Weiping; Zhao, Huijun


    For the first time, a facile, one-pot hydrofluoric acid vapor-phase hydrothermal (HF-VPH) method is demonstrated to directly grow single-crystalline anatase TiO(2) nanosheets with 98.2% of exposed {001} faceted surfaces on the Ti substrate via a distinctive two-stage formation mechanism. The first stage produces a new intermediate crystal (orthorhombic HTiOF(3) ) that is transformed into anatase TiO(2) nanosheets during the second stage. The findings reveal that the HF-VPH reaction environment is unique and differs remarkably from that of liquid-phase hydrothermal processes. The uniqueness of the HF-VPH conditions can be readily used to effectively control the nanostructure growth. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Material synthesis and hydrogen storage of palladium-rhodium alloy.

    Energy Technology Data Exchange (ETDEWEB)

    Lavernia, Enrique J. (University of California, Davis); Yang, Nancy Y. C.; Ong, Markus D. (Whithworth University, Spokane, WA)


    Pd and Pd alloys are candidate material systems for Tr or H storage. We have actively engaged in material synthesis and studied the material science of hydrogen storage for Pd-Rh alloys. In collaboration with UC Davis, we successfully developed/optimized a supersonic gas atomization system, including its processing parameters, for Pd-Rh-based alloy powders. This optimized system and processing enable us to produce {le} 50-{mu}m powders with suitable metallurgical properties for H-storage R&D. In addition, we studied hydrogen absorption-desorption pressure-composition-temperature (PCT) behavior using these gas-atomized Pd-Rh alloy powders. The study shows that the pressure-composition-temperature (PCT) behavior of Pd-Rh alloys is strongly influenced by its metallurgy. The plateau pressure, slope, and H/metal capacity are highly dependent on alloy composition and its chemical distribution. For the gas-atomized Pd-10 wt% Rh, the absorption plateau pressure is relatively high and consistent. However, the absorption-desorption PCT exhibits a significant hysteresis loop that is not seen from the 30-nm nanopowders produced by chemical precipitation. In addition, we observed that the presence of hydrogen introduces strong lattice strain, plastic deformation, and dislocation networking that lead to material hardening, lattice distortions, and volume expansion. The above observations suggest that the H-induced dislocation networking is responsible for the hysteresis loop seen in the current atomized Pd-10 wt% Rh powders. This conclusion is consistent with the hypothesis suggested by Flanagan and others (Ref 1) that plastic deformation or dislocations control the hysteresis loop.

  9. Columnar jointing in vapor-phase-altered, non-welded Cerro Galán Ignimbrite, Paycuqui, Argentina (United States)

    Wright, Heather M.; Lesti, Chiara; Cas, Ray A.F.; Porreca, Massimiliano; Viramonte, Jose G.; Folkes, Christopher B.; Giordano, Guido


    Columnar jointing is thought to occur primarily in lavas and welded pyroclastic flow deposits. However, the non-welded Cerro Galán Ignimbrite at Paycuqui, Argentina, contains well-developed columnar joints that are instead due to high-temperature vapor-phase alteration of the deposit, where devitrification and vapor-phase crystallization have increased the density and cohesion of the upper half of the section. Thermal remanent magnetization analyses of entrained lithic clasts indicate high emplacement temperatures, above 630°C, but the lack of welding textures indicates temperatures below the glass transition temperature. In order to remain below the glass transition at 630°C, the minimum cooling rate prior to deposition was 3.0 × 10−3–8.5 × 10−2°C/min (depending on the experimental data used for comparison). Alternatively, if the deposit was emplaced above the glass transition temperature, conductive cooling alone was insufficient to prevent welding. Crack patterns (average, 4.5 sides to each polygon) and column diameters (average, 75 cm) are consistent with relatively rapid cooling, where advective heat loss due to vapor fluxing increases cooling over simple conductive heat transfer. The presence of regularly spaced, complex radiating joint patterns is consistent with fumarolic gas rise, where volatiles originated in the valley-confined drainage system below. Joint spacing is a proxy for cooling rates and is controlled by depositional thickness/valley width. We suggest that the formation of joints in high-temperature, non-welded deposits is aided by the presence of underlying external water, where vapor transfer causes crystallization in pore spaces, densifies the deposit, and helps prevent welding.

  10. Indium tin oxide thin-films prepared by vapor phase pyrolysis for efficient silicon based solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Simashkevich, Alexei, E-mail: [Institute of Applied Physics, 5 Academiei str., Chisinau, MD-2028, Republic of Moldova (Moldova, Republic of); Serban, Dormidont; Bruc, Leonid; Curmei, Nicolai [Institute of Applied Physics, 5 Academiei str., Chisinau, MD-2028, Republic of Moldova (Moldova, Republic of); Hinrichs, Volker [Institut für Heterogene Materialsysteme, Helmholtz-Zentrum Berlin für Materialien und Energie GmbH, Lise-Meitner Campus, Hahn-Meitner-Platz 1, 14109 Berlin (Germany); Rusu, Marin [Institute of Applied Physics, 5 Academiei str., Chisinau, MD-2028, Republic of Moldova (Moldova, Republic of); Institut für Heterogene Materialsysteme, Helmholtz-Zentrum Berlin für Materialien und Energie GmbH, Lise-Meitner Campus, Hahn-Meitner-Platz 1, 14109 Berlin (Germany)


    The vapor phase pyrolysis deposition method was developed for the preparation of indium tin oxide (ITO) thin films with thicknesses ranging between 300 and 400 nm with the sheet resistance of 10–15 Ω/sq. and the transparency in the visible region of the spectrum over 80%. The layers were deposited on the (100) surface of the n-type silicon wafers with the charge carriers concentration of ~ 10{sup 15} cm{sup −3}. The morphology of the ITO layers deposited on Si wafers with different surface morphologies, e.g., smooth (polished), rough (irregularly structured) and textured (by inversed pyramids) was investigated. The as-deposited ITO thin films consist of crystalline columns with the height of 300–400 nm and the width of 50–100 nm. Photovoltaic parameters of mono- and bifacial solar cells of Cu/ITO/SiO{sub 2}/n–n{sup +} Si/Cu prepared on Si (100) wafers with different surface structures were studied and compared. A maximum efficiency of 15.8% was achieved on monofacial solar cell devices with the textured Si surface. Bifacial photovoltaic devices from 100 μm thick Si wafers with the smooth surface have demonstrated efficiencies of 13.0% at frontal illumination and 10% at rear illumination. - Highlights: • ITO thin films prepared by vapor phase pyrolysis on Si (100) wafers with a smooth (polished), rough (irregularly structured) and textured (by inversed pyramids) surface. • Monofacial ITO/SiO2/n-n+Si solar cells with an efficiency of 15.8% prepared and bifacial PV devices with front- and rear-side efficiencies up to 13% demonstrated. • Comparative studies of photovoltaic properties of solar cells with different morphologies of the Si wafer surface presented.

  11. APTS and rGO co-functionalized pyrenated fluorescent nanonets for representative vapor phase nitroaromatic explosive detection (United States)

    Guo, Linjuan; Zu, Baiyi; Yang, Zheng; Cao, Hongyu; Zheng, Xuefang; Dou, Xincun


    For the first time, flexible PVP/pyrene/APTS/rGO fluorescent nanonets were designed and synthesized via a one-step electrospinning method to detect representative subsaturated nitroaromatic explosive vapor. The functional fluorescent nanonets, which were highly stable in air, showed an 81% quenching efficiency towards TNT vapor (~10 ppb) with an exposure time of 540 s at room temperature. The nice performance of the nanonets was ascribed to the synergistic effects induced by the specific adsorption properties of APTS, the fast charge transfer properties and the effective π-π interaction with pyrene and TNT of rGO. Compared to the analogues of TNT, the PVP/pyrene/APTS/rGO nanonets showed notable selectivity towards TNT and DNT vapors. The explored functionalization method opens up brand new insight into sensitive and selective detection of vapor phase nitroaromatic explosives.For the first time, flexible PVP/pyrene/APTS/rGO fluorescent nanonets were designed and synthesized via a one-step electrospinning method to detect representative subsaturated nitroaromatic explosive vapor. The functional fluorescent nanonets, which were highly stable in air, showed an 81% quenching efficiency towards TNT vapor (~10 ppb) with an exposure time of 540 s at room temperature. The nice performance of the nanonets was ascribed to the synergistic effects induced by the specific adsorption properties of APTS, the fast charge transfer properties and the effective π-π interaction with pyrene and TNT of rGO. Compared to the analogues of TNT, the PVP/pyrene/APTS/rGO nanonets showed notable selectivity towards TNT and DNT vapors. The explored functionalization method opens up brand new insight into sensitive and selective detection of vapor phase nitroaromatic explosives. Electronic supplementary information (ESI) available: Vapor pressure of TNT and its analogues, fluorescence quenching kinetics, fluorescence quenching efficiencies and additional SEM images. See DOI: 10.1039/c3nr04960d

  12. Heterocyclic energetic materials: Synthesis, characterization and computational design (United States)

    Tsyshevsky, Roman; Pagoria, Philip; Smirnov, Aleksander; Kuklja, Maija


    Achievement of the tailored properties (high performance, low sensitivity, etc.) in targeted new energetic materials (EM) remains a great challenge. Recently, attention of researchers has shifted from conventional nitroester-, nitramine-, and nitroaromatic-based explosives to new heterocyclic EM with oxygen- and nitrogenrich molecular structures. They have increased densities and formation enthalpies complemented by attractive performance and high stability to external stimuli. We will demonstrate that oxadiazol-containing heterocycles offer a convenient playground to probe specific chemical functional groups as building blocks for design of EM. We discuss a joint experimental and computational approach for design, characterization, synthesis, and modeling of novel heterocyclic EM. Combinatorically, we comprehensively analyzed how overall stability and performance of each material in the family (BNFF, LLM-172, LLM-175, LLM-191, LLM-192, LLM-200) depends upon their chemical composition and details of the molecular structure (such as a substitution of a nitro group by an amino group and 1,2,5-oxadiazole fragment by 1,2,3- or 1,2,4-oxadiazol ring). We will also discuss proposed new EM with predicted superior chemical and physical properties. P. Pagoria, R. Tsyshevsky, A. Smirnov.

  13. Ultrasound-assisted synthesis and processing of carbon materials (United States)

    Fortunato, Maria E.


    Part I: Porous carbons are of interest in many applications because of their high surface areas and other physicochemical properties, and much effort has been directed towards developing new methods for controlling the porosity of carbons. Ultrasonic spray pyrolysis (USP) is an aerosol method suitable for large-scale, continuous synthesis of materials. Ultrasound is used to create aerosol droplets of a precursor solution which serve as micron-sized spherical reactors for materials synthesis. This work presents a precursor system for the template-free USP synthesis of porous carbons using low-cost precursors that do not evolve or require hazardous chemicals: sucrose was used as the carbon source, and sodium carbonate, sodium bicarbonate, or sodium nitrate was added as a decomposition catalyst and porogen. The USP carbons had macroporous interiors and microporous shells with surface areas as high as 800 m2/g and a narrow pore size distribution. It was determined that the interior porosity was a result of the gas evolution from salt decomposition and not from the presence of a salt template. Porous carbon is frequently used as a catalyst support because it provides high surface area and it is chemically and physically stable under many anoxic reaction conditions. Typically, the preparation of supported catalysts requires multiple steps for carbonization and metal impregnation. In this work, iron-impregnated porous carbon microspheres (Fe-C) were prepared by a one-step USP process by incorporating both the carbon and metal sources into the precursor solution. Carbonization, pore formation, metal impregnation, and metal activation occurred simultaneously to produce Fe-C materials with surface areas as high as 800 m2/g and up to 10 wt% Fe incorporated as nanoparticles 109 K/sec). In solid-liquid slurries, surface erosion and particle fracture occur due to the shockwaves and microjets formed from asymmetric bubble collapse at extended surfaces. The chemical and physical


    Novel organic sulfide modified bimetallic iron-copper nanoparticle aggregate sorbent materials have been synthesized for removing elemental mercury from vapor streams at elevated temperatures (120-140 °C). Silane based (disulfide silane and tetrasulfide silane) and alkyl sulfide ...

  15. Critical issues for homoepitaxial GaN growth by molecular beam epitaxy on hydride vapor-phase epitaxy-grown GaN substrates (United States)

    Storm, D. F.; Hardy, M. T.; Katzer, D. S.; Nepal, N.; Downey, B. P.; Meyer, D. J.; McConkie, Thomas O.; Zhou, Lin; Smith, David J.


    While the heteroepitaxial growth of gallium nitride-based materials and devices on substrates such as SiC, sapphire, and Si has been well-documented, the lack of a cost-effective source of bulk GaN crystals has hindered similar progress on homoepitaxy. Nevertheless, freestanding GaN wafers are becoming more widely available, and there is great interest in growing GaN films and devices on bulk GaN substrates, in order to take advantage of the greatly reduced density of threading dislocations, particularly for vertical devices. However, homoepitaxial GaN growth is far from a trivial task due to the reactivity and different chemical sensitivities of N-polar (0001) and Ga-polar (0001) GaN surfaces, which can affect the microstructure and concentrations of impurities in homoepitaxial GaN layers. In order to achieve high quality, high purity homoepitaxial GaN, it is necessary to investigate the effect of the ex situ wet chemical clean, the use of in situ cleaning procedures, the sensitivity of the GaN surface to thermal decomposition, and the effect of growth temperature. We review the current understanding of these issues with a focus on homoepitaxial growth of GaN by molecular beam epitaxy (MBE) on c-plane surfaces of freestanding GaN substrates grown by hydride vapor phase epitaxy (HVPE), as HVPE-grown substrates are most widely available. We demonstrate methods for obtaining homoepitaxial GaN layers by plasma-assisted MBE in which no additional threading dislocations are generated from the regrowth interface and impurity concentrations are greatly reduced.

  16. Up-Scaled Supercritical Flow Synthesis of Hybrid Materials

    DEFF Research Database (Denmark)

    Hellstern, Henrik Christian; Becker, Jacob; Hald, Peter

    A new, up-scaled supercritical flow synthesis apparatus is currently under construction in Aarhus. A module based system allows for a range of parameter studies with improved parameter control. The dual-reactor setup enables both single phase and core-shell nanoparticle synthesis, and the large...

  17. Structures and properties of poly(3-alkylthiophene) thin-films fabricated though vapor-phase polymerization. (United States)

    Back, Ji-Woong; Song, Eun-Ah; Lee, Keum-Joo; Lee, Youn-Kyung; Hwang, Chae-Ryong; Jo, Sang-Hyun; Jung, Woo-Gwang; Kim, Jin-Yeol


    Organic semiconducting polymer thin-films of 3-hexylthiophene, 3-octylthiophene, 3-decylthiophene, containing highly oriented crystal were fabricated by gas-phase polymerization using the CVD technique. These poly(3-alkylthiophene) films had a crystallinity up to 80%, and possessed a Hall mobility up to 10 cm2/Vs. The degree of crystalinity and the mobility values increased as the alkyl chain length increased. The crystal structure of the polymers was composed of stacked layers constructed by a side-by-side arrangement of alkyl chains and in-plane pi-pi stacking. These thin films are capable of being applied to organic electronics as the active materials used in thin-film transistors and organic photovoltaic cells.

  18. Synthesis and characterization of inverse spinels, intercalation materials for Li-ion batteries

    NARCIS (Netherlands)

    Van Landschoot, N.


    Chapter 2 describes the solid-state synthesis of LiNiVO4 and LiCoVO4. The materials are prepared at 800C and are phase pure, as shown by X-ray diffraction and have the inverse spinel structure. Due to the solid-state synthesis the particle size is quite large and the particle size distribution is

  19. Optimization Problem of Thermal Field on Surface of Revolving Susceptor in Vapor-Phase Epitaxy Reactor (United States)

    Zhilenkov, A. A.; Chernyi, S. G.; Nyrkov, A. P.; Sokolov, S. S.


    Nitrides of group III elements are a very suitable basis for deriving light-emitting devices with the radiating modes lengths of 200-600 nm. The use of such semiconductors allows obtaining full-color RGB light sources, increasing record density of a digital data storage device, getting high-capacity and efficient sources of white light. Electronic properties of such semi-conductors allow using them as a basis for high-power and high-frequency transistors and other electronic devices, the specifications of which are competitive with those of SiC-based devices. Only since 2000, the technology of cultivation of crystals III-N of group has come to the level of wide recognition by both abstract science, and the industry that has led to the creation of the multi-billion dollar market. And this is despite a rather low level of development of the production technology of devices on the basis of III-N of materials. The progress that has happened in the last decade requires the solution of the main problem, constraining further development of this technology today – ensuring cultivation of III-N structures of necessary quality. For this purpose, it is necessary to solve problems of the analysis and optimization of processes in installations of epitaxial growth, and, as a result, optimization of its constructions.

  20. Effect of gas flow on the selective area growth of gallium nitride via metal organic vapor phase epitaxy (United States)

    Rodak, L. E.; Kasarla, K. R.; Korakakis, D.


    The effect of gas flow on the selective area growth (SAG) of gallium nitride (GaN) grown via metal organic vapor phase epitaxy (MOVPE) has been investigated. In this study, the SAG of GaN was carried out on a silicon dioxide striped pattern along the GaN direction. SAG was initiated with the striped pattern oriented parallel and normal to the incoming gas flow in a horizontal reactor. The orientation of the pattern did not impact cross section of the structure after re-growth as both orientations resulted in similar trapezoidal structures bounded by the (0 0 0 1) and {1 1 2¯ n} facets ( n≈1.7-2.2). However, the growth rates were shown to depend on the orientation of the pattern as the normally oriented samples exhibited enhanced vertical and cross-sectional growth rates compared to the parallel oriented samples. All growths occurred under identical conditions and therefore the difference in growth rates must be attributed to a difference in mass transport of species.

  1. Highly Ordered Boron Nitride Nanotube Arrays with Controllable Texture from Ammonia Borane by Template-Aided Vapor-Phase Pyrolysis

    Directory of Open Access Journals (Sweden)

    Yuting Wang


    Full Text Available An efficient approach for the preparation of good-quality boron nitride nanotubes (BNNTs is developed. BNNTs with specific texture were prepared from ammonia borane (BH3NH3 by vapor-phase pyrolysis with the aid of a template in two independent temperature-controlled furnaces. Two kinds of BNNTs, 200–300 nm wide ×60 μm long and 70–80 nm wide ×40 μm long, were produced after removal of the templates. The as-produced BNNTs were heated at different temperatures in the range of 1300–1700°C in NH3. FT-IR and XPS results confirmed the formation of BN from BH3NH3. Ordered arrays of BNNTs without cracks on the surface were seen using microstructural observations. The diameter and length of the BNNTs are controlled using templates with different pore sizes and thickness. The wall thickness of the nanotubes was increased by increasing the number of deposition cycles. The crystallinity of the BNNTs was improved by heating at a high temperature (1700°C in NH3.

  2. Properties of (In,Ga)(As,P)/GaAs interfaces grown under different metalorganic vapor phase epitaxy conditions (United States)

    Knauer, A.; Krispin, P.; Balakrishnan, V. R.; Weyers, M.


    The mechanisms for formation of interlayers at the interface of GaAs on (In,Ga)P and In 0.15Ga 0.85As 0.7P 0.3 grown by metalorganic vapor phase epitaxy have been studied by capacitance-voltage profiling of the electron concentration. Shallow In-rich quantum wells (QWs) are formed in (In,Ga)P during growth interruptions under PH 3 stabilization. These QWs are seen in C-V profiles, but not in photoluminescence and X-ray diffraction. Stabilization of (In,Ga)P under AsH 3 yields thin (1-2 nm thick) (In,Ga)(As,P) interlayers, which are observed by X-ray diffraction and capacitance-voltage profiles. Under optimized conditions, these interlayers exhibit negligibly small band offsets. When growing GaAs on quaternary (In,Ga)(As,P), interlayers can be avoided even at high growth temperatures and long growth interruptions. Independent on the chosen growth conditions, the (In,Ga)P and (In,Ga)(As,P) layers as well as the investigated interfaces are practically free of defect levels as determined by deep-level transient Fourier spectroscopy.

  3. Influence of lateral growth on the optical properties of GaN nanowires grown by hydride vapor phase epitaxy (United States)

    Wu, Shaoteng; Wang, Liancheng; Yi, Xiaoyan; Liu, Zhiqiang; Wei, Tongbo; Yuan, Guodong; Wang, Junxi; Li, Jinmin


    GaN nanowires (NWs) are synthesized on Si (111) using vapor-liquid-solid hydride vapor phase epitaxy at low temperature (740-780 °C). We find that the flow rate of the GaCl (HCl) gas has a large impact on the NW lateral growth rate, which affects the NW morphology, axial growth rate, and optical property. Upon increasing the flow rate of GaCl, the uncatalyzed vapor solid lateral growth increases rapidly, leading to variations in NW morphology from wire-like to tower-like and rod-like. The photoluminescence spectrum shows a broad red luminescence (RL) at around 660 nm and a weak near-band-edge luminescence at around 400 nm when lateral growth is at a significant level. Furthermore, spatially resolved cathodoluminescence and high-resolution transmission electron microscopy observations confirmed that this RL originates from the defective lateral growth. Finally, by inhibiting the lateral growth, GaN NWs with a high aspect ratio and excellent crystal quality (no RL observed at around 660 nm) were successfully synthesized with a rapid growth rate of 170 μm/h.

  4. Using vapor phase tomography to measure the spatial distribution of vapor concentrations and flux for vadose-zone VOC sources. (United States)

    Mainhagu, J; Morrison, C; Brusseau, M L


    A test was conducted at a chlorinated-solvent contaminated site in Tucson, AZ, to evaluate the effectiveness of vapor-phase tomography (VPT) for characterizing the distribution of volatile organic contaminants (VOC) in the vadose zone. A soil vapor extraction (SVE) system has been in operation at the site since 2007. Vapor concentration and vacuum pressure were measured at four different depths in each of the four monitoring wells surrounding the extraction well. The test provided a 3D characterization of local vapor concentrations under induced-gradient conditions. Permeability data obtained from analysis of borehole logs were used along with pressure and the vapor-concentration data to determine VOC mass flux within the test domain. A region of higher mass flux was identified in the deepest interval of the S-SW section of the domain, indicating the possible location of a zone with greater contaminant mass. These results are consistent with the TCE-concentration distribution obtained from sediment coring conducted at the site. In contrast, the results of a standard soil gas survey did not indicate the presence of a zone with greater contaminant mass. These results indicate that the VPT test provided a robust characterization of VOC concentration and flux distribution at the site. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Shock-and-Release to the Liquid-Vapor Phase Boundary: Experiments and Applications to Planetary Science (United States)

    Stewart, Sarah


    Shock-induced vaporization was a common process during the end stages of terrestrial planet formation and transient features in extra-solar systems are attributed to recent giant impacts. At the Sandia Z Machine, my collaborators and I are conducting experiments to study the shock Hugoniot and release to the liquid-vapor phase boundary of major minerals in rocky planets. Current work on forsterite, enstatite and bronzite and previous results on silica, iron and periclase demonstrate that shock-induced vaporization played a larger role during planet formation than previously thought. I will provide an overview of the experimental results and describe how the data have changed our views of planetary impact events in our solar system and beyond. Sandia National Laboratories is a multiprogram laboratory managed and operated by Sandia Corporation, a wholly owned subsidiary of Lockheed Martin Corporation, for the U.S. Department of Energy's National Nuclear Security Administration under Contract No. DE-AC04-94AL85000. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344. This work is supported by the Z Fundamental Science Program at Sandia National Laboratories, DOE-NNSA Grant DE- NA0002937, NASA Grant # NNX15AH54G, and UC Multicampus-National Lab Collaborative Research and Training Grant #LFR-17-449059.

  6. Investigation of the structural defects in GaN thin films grown by organometallic vapor phase epitaxy (United States)

    Choi, J.-H.; Lim, S.-J.; Cho, M.-S.; Cho, N.-H.; Chung, S.-J.; Sohn, C.-S.


    GaN thin films were prepared on {0001} planes of sapphire substrates by organometallic vapor phase epitaxy (OMVPE) techniques. The crystall orgaphic relation between the film and the substrate as well as the structural features of the defects in the film were investigated by transmission electron microscopy (TEM). Epitaxial relationship was observed in the GaN/sapphire heterostructure prepared in this investigation; (0001) GaN//(0001) sapphire;[ {01bar 10} ] GaN//[ {bar 12bar 10} ] sapphire. Dislocations of Burgers vectorbar b = {1/3} [ {2bar 1bar 10} ] were observed in the film; the propagation behavior of the dislocations exhibits a slip system{ {10bar 10} }< {2bar 1bar 10} rangle is operative in the film. Inversion domain boundary (IDB) facets lying parallel to{ {01bar 10} } and{ {bar 12bar 10} } planes were observed; the type of anti-site bonds (Ga-Ga, N-N) is altemate along these IDB planes, keeping the simple stoichiometry of the compound.

  7. Germanium diffusion with vapor-phase GeAs and oxygen co-incorporation in GaAs

    Directory of Open Access Journals (Sweden)

    Wei-Fu Wang


    Full Text Available Vapor-phase germanium diffusion has been demonstrated in Zn-doped and semi-insulating GaAs in sealed ampoules with GeAs powders and excess arsenic. Secondary-ion-mass spectroscopy (SIMS profiles indicate the presence of unintentional co-incorporation of oxygen in high densities (>1017/cm3 along with diffused germanium donors whose concentration (>>1018/cm3 determined by electro-chemical capacitance-voltage (ECV profiler shows significant compensation near the surface. The source of oxygen mainly originates from the GeAs powder which contains Ge-O surface oxides. Variable-temperature photoluminescence (PL shows that in GeAs-diffused samples, a broad peak ranging from 0.86-1.38 eV with the peak position around 1.1 eV predominates at low temperatures while the near band-edge luminescence quenches. The broad band is attributed to the GeGa-VGa self-activated (SA centers possibly associated with nearby oxygen-related defect complex, and its luminescence persists up to 400 K. The configurational-coordinate modeling finds that the SA defect complex has a thermal activation energy of 150-180 meV and a vibrational energy 26.8 meV. The presence of oxygen does not much affect the SA emission intensity but may have influenced the peak position, vibration frequency and activation energy as compared to other common donor-VGa defects in GaAs.

  8. Detection of vapor-phase organophosphate threats using wearable conformable integrated epidermal and textile wireless biosensor systems. (United States)

    Mishra, Rupesh K; Martín, Aida; Nakagawa, Tatsuo; Barfidokht, Abbas; Lu, Xialong; Sempionatto, Juliane R; Lyu, Kay Mengjia; Karajic, Aleksandar; Musameh, Mustafa M; Kyratzis, Ilias L; Wang, Joseph


    Flexible epidermal tattoo and textile-based electrochemical biosensors have been developed for vapor-phase detection of organophosphorus (OP) nerve agents. These new wearable sensors, based on stretchable organophosphorus hydrolase (OPH) enzyme electrodes, are coupled with a fully integrated conformal flexible electronic interface that offers rapid and selective square-wave voltammetric detection of OP vapor threats and wireless data transmission to a mobile device. The epidermal tattoo and textile sensors display a good reproducibility (with RSD of 2.5% and 4.2%, respectively), along with good discrimination against potential interferences and linearity over the 90-300mg/L range, with a sensitivity of 10.7µA∙cm 3 ∙mg -1 (R 2 = 0.983) and detection limit of 12mg/L in terms of OP air density. Stress-enduring inks, used for printing the electrode transducers, ensure resilience against mechanical deformations associated with textile and skin-based on-body sensing operations. Theoretical simulations are used to estimate the OP air density over the sensor surface. These fully integrated wearable wireless tattoo and textile-based nerve-agent vapor biosensor systems offer considerable promise for rapid warning regarding personal exposure to OP nerve-agent vapors in variety of decentralized security applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Vapor-phase Raman spectra, theoretical calculations, and the vibrational and structural properties of cis- and trans-stilbene. (United States)

    Egawa, Toru; Shinashi, Kiyoaki; Ueda, Toyotoshi; Ocola, Esther J; Chiang, Whe-Yi; Laane, Jaan


    The vapor-phase Raman spectra of cis- and trans-stilbene have been collected at high temperatures and assigned. The low-frequency skeletal modes were of special interest. The molecular structures and vibrational frequencies of both molecules have also been obtained using MP2/cc-pVTZ and B3LYP/cc-pVTZ calculations, respectively. The two-dimensional potential map for the internal rotations around the two Cphenyl-C(═C) bonds of cis-stilbene was generated by using a series of B3LYP/cc-pVTZ calculations. It was confirmed that the molecule has only one conformer with C2 symmetry. The energy level calculation with a two-dimensional Hamiltonian was carried out, and the probability distribution for each level was obtained. The calculation revealed that the "gearing" internal rotation in which the two phenyl rings rotate with opposite directions has a vibrational frequency of 26 cm(-1), whereas that of the "antigearing" internal rotation in which the phenyl rings rotate with the same direction is about 52 cm(-1). In the low vibrational energy region the probability distribution for the gearing internal rotation is similar to that of a one-dimensional harmonic oscillator, and in the higher region the motion behaves like that of a free rotor.

  10. Evaluation of cinnamon essential oil microemulsion and its vapor phase for controlling postharvest gray mold of pears (Pyrus pyrifolia). (United States)

    Wang, Yifei; Zhao, Ruipeng; Yu, Ling; Zhang, Yunbin; He, Yan; Yao, Jie


    Essential oil of cinnamon (CM) is a potential alternative to chemical fungicides. Thus this work aimed to investigate the possible effects of CM microemulsions on decay developments and qualitative properties of pears. The decay incidence of samples treated with 500 µg L⁻¹ microemulsion was significantly reduced by 18.7% in comparison to that of 500 µg L⁻¹ non-microemulsion after 4 days' storage at 20 °C. In the vapor phase, the CM microemulsion with the lowest concentration had the best control for decay incidence and lesion diameter. The interval between inoculations also influenced decay development. Pears treated with Botrytis cinerea and immediately followed by CM microemulsion showed the lowest decay incidence. Moreover, in the natural decay experiment, the percentage of rotted pears was 3.8% in the CM microemulsion treatment and 5.8% in the control. CM microemulsion delayed the loss of ascorbic acid, yet it had no significant influence on pear qualities such as firmness and color. CM microemulsion may be an alternative way to control the gray mold of pears without a negative influence on its qualities. © 2013 Society of Chemical Industry.

  11. Migration of carbon nanotubes from liquid phase to vapor phase in the refrigerant-based nanofluid pool boiling

    Directory of Open Access Journals (Sweden)

    Peng Hao


    Full Text Available Abstract The migration characteristics of carbon nanotubes from liquid phase to vapor phase in the refrigerant-based nanofluid pool boiling were investigated experimentally. Four types of carbon nanotubes with the outside diameters from 15 to 80 nm and the lengths from 1.5 to 10 μm were used in the experiments. The refrigerants include R113, R141b and n-pentane. The oil concentration is from 0 to 10 wt.%, the heat flux is from 10 to 100 kW·m-2, and the initial liquid-level height is from 1.3 to 3.4 cm. The experimental results indicate that the migration ratio of carbon nanotube increases with the increase of the outside diameter or the length of carbon nanotube. For the fixed type of carbon nanotube, the migration ratio decreases with the increase of the oil concentration or the heat flux, and increases with the increase of the initial liquid-level height. The migration ratio of carbon nanotube increases with the decrease of dynamic viscosity of refrigerant or the increase of liquid phase density of refrigerant. A model for predicting the migration ratio of carbon nanotubes in the refrigerant-based nanofluid pool boiling is proposed, and the predictions agree with 92% of the experimental data within a deviation of ±20%.


    National Research Council Canada - National Science Library



    The main aim of this study was to identify the potential use of agar extracted from red seaweed, Gracilaria salicornia, collected from the coastal area of Malaysia as the raw material for synthesis of bioplastic film...

  13. Combustion based technique for synthesis and joining of refractory materials (United States)

    White, Jeremiah David Edward

    Gasless combustion systems offer features that make them attractive tools for a variety of potential applications. Among them are rapid heating rates, high exothermicity, and high maximum temperatures. These characteristics were exploited to accomplish three separate concepts including the joining of refractory materials, synthesis of a pore-free composite, and the study of thermal explosion in mechanically activated powders. Honeywell Aerospace is a leading producer of carbon brakes for commercial aircraft. The manufacturing process involves chemical vapor infiltration (CVI) to form a carbon matrix around a carbon fiber preform. A major disadvantage of this approach is the time required to form a fully dense preform, which is on the order of 140 days. In addition, after the brakes are in service, they have to be discarded while there is a relatively thick amount of friction material still available. There is a profit motive for reusing these discs which are out of spec. One such example would be to perform a refurbishment by bonding a new thin C/C element onto a used "core" to produce a brake that meets performance specifications. Unfortunately, joining C/C composites is not a simple task, as carbon does not lend itself to welding, and other means (e.g. mechanical or adhesives) would not hold up to the harsh operational conditions. A novel apparatus was designed, built, and proven to join C/C using so-called reactive resistance welding (RRW). It is shown that a joint stronger than the original material can be achieved using moderate electrical current and mechanical force. Additionally, joining layers of similar thickness and microstructure were obtained with different reactive media, ranging from pellets of pressed powders (˜1-2 mm) to thin metal foils (˜25 micron). By modifying the schematic of the RRW apparatus, porous C/C was infiltrated with liquid silicon in order to form a new pore-free C/C-SiC composite. It is shown that using such a process, the silicon

  14. Oxide based functional materials through solid state and electrochemical synthesis


    Todorova, Vanya


    The presented dissertation combines synthesis and characterization techniques of solid state chemistry and electrochemistry. The work is organized into two main parts. The first part deals with the synthesis, structural characterization and investigation of the physical properties of new ternary and quaternary transition metal oxides with layered structures. Several compounds of delafossite structure ABO2 with silver on A position and different trivalent cation capable of adopting an octa...

  15. 'Beautiful' unconventional synthesis and processing technologies of superconductors and some other materials. (United States)

    Badica, Petre; Crisan, Adrian; Aldica, Gheorghe; Endo, Kazuhiro; Borodianska, Hanna; Togano, Kazumasa; Awaji, Satoshi; Watanabe, Kazuo; Sakka, Yoshio; Vasylkiv, Oleg


    Superconducting materials have contributed significantly to the development of modern materials science and engineering. Specific technological solutions for their synthesis and processing helped in understanding the principles and approaches to the design, fabrication and application of many other materials. In this review, we explore the bidirectional relationship between the general and particular synthesis concepts. The analysis is mostly based on our studies where some unconventional technologies were applied to different superconductors and some other materials. These technologies include spray-frozen freeze-drying, fast pyrolysis, field-assisted sintering (or spark plasma sintering), nanoblasting, processing in high magnetic fields, methods of control of supersaturation and migration during film growth, and mechanical treatments of composite wires. The analysis provides future research directions and some key elements to define the concept of 'beautiful' technology in materials science. It also reconfirms the key position and importance of superconductors in the development of new materials and unconventional synthesis approaches.

  16. 'Beautiful' unconventional synthesis and processing technologies of superconductors and some other materials

    Directory of Open Access Journals (Sweden)

    Petre Badica, Adrian Crisan, Gheorghe Aldica, Kazuhiro Endo, Hanna Borodianska, Kazumasa Togano, Satoshi Awaji, Kazuo Watanabe, Yoshio Sakka and Oleg Vasylkiv


    Full Text Available Superconducting materials have contributed significantly to the development of modern materials science and engineering. Specific technological solutions for their synthesis and processing helped in understanding the principles and approaches to the design, fabrication and application of many other materials. In this review, we explore the bidirectional relationship between the general and particular synthesis concepts. The analysis is mostly based on our studies where some unconventional technologies were applied to different superconductors and some other materials. These technologies include spray-frozen freeze-drying, fast pyrolysis, field-assisted sintering (or spark plasma sintering, nanoblasting, processing in high magnetic fields, methods of control of supersaturation and migration during film growth, and mechanical treatments of composite wires. The analysis provides future research directions and some key elements to define the concept of 'beautiful' technology in materials science. It also reconfirms the key position and importance of superconductors in the development of new materials and unconventional synthesis approaches.

  17. 'Beautiful' unconventional synthesis and processing technologies of superconductors and some other materials

    Energy Technology Data Exchange (ETDEWEB)

    Badica, Petre; Crisan, Adrian; Aldica, Gheorghe [National Institute of Materials Physics, Atomistilor 105bis, Magurele, Ilfov 077125 (Romania); Endo, Kazuhiro [Research Laboratory for Integrated Technological Systems, Kanazawa Institute of Technology (KIT), 3-1 Yatsukaho, Hakusan, Ishikawa 924-0838 (Japan); Borodianska, Hanna [Institute for Materials Science, NASU, 3, Krzhizhanivsky, Kiev 03680 (Ukraine); Togano, Kazumasa; Sakka, Yoshio; Vasylkiv, Oleg [National Institute for Materials Science, 1-2-1 Sengen, Tsukuba, Ibaraki 305-0047 (Japan); Awaji, Satoshi; Watanabe, Kazuo, E-mail: [Institute for Materials Research, Tohoku University, 2-1-1 Katahira, Aoba, Sendai, Miyagi 980-8577 (Japan)


    Superconducting materials have contributed significantly to the development of modern materials science and engineering. Specific technological solutions for their synthesis and processing helped in understanding the principles and approaches to the design, fabrication and application of many other materials. In this review, we explore the bidirectional relationship between the general and particular synthesis concepts. The analysis is mostly based on our studies where some unconventional technologies were applied to different superconductors and some other materials. These technologies include spray-frozen freeze-drying, fast pyrolysis, field-assisted sintering (or spark plasma sintering), nanoblasting, processing in high magnetic fields, methods of control of supersaturation and migration during film growth, and mechanical treatments of composite wires. The analysis provides future research directions and some key elements to define the concept of 'beautiful' technology in materials science. It also reconfirms the key position and importance of superconductors in the development of new materials and unconventional synthesis approaches. (topical review)

  18. Authorized Limit Evaluation of Spent Granular Activated Carbon Used for Vapor-Phase Remediation at the Lawrence Livermore National Laboratory Livermore, California

    Energy Technology Data Exchange (ETDEWEB)

    Devany, R; Utterback, T


    This report provides a technical basis for establishing radiological release limits for granular activated carbon (GAC) containing very low quantities of tritium and radon daughter products generated during environmental remediation activities at Lawrence Livermore National Laboratory (LLNL). This evaluation was conducted according to the Authorized Limit procedures specified in United States Department of Energy (DOE) Order 5400.5, Radiation Protection of the Public and the Environment (DOE, 1993) and related DOE guidance documents. The GAC waste is currently being managed by LLNL as a Resource Conservation and Recovery Act (RCRA) mixed waste. Significant cost savings can be achieved by developing an Authorized Limit under DOE Order 5400.5 since it would allow the waste to be safely disposed as a hazardous waste at a permitted off-site RCRA treatment and disposal facility. LLNL generates GAC waste during vapor-phase soil remediation in the Trailer 5475 area. While trichloroethylene and other volatile organic compounds (VOCs) are the primary targets of the remedial action, a limited amount of tritium and radon daughter products are contained in the GAC at the time of disposal. As defined in DOE Order 5400.5, an Authorized Limit is a level of residual radioactive material that will result in an annual public dose of 100 milliroentgen-equivalent man per year (mrem/year) or less. In 1995, DOE issued additional release requirements for material sent to a landfill that is not an authorized low-level radioactive waste disposal facility. Per guidance, the disposal site will be selected based on a risk/benefit assessment under the As-Low-As-Reasonably-Achievable (ALARA) process while ensuring that individual doses to the public are less than 25 mrem in a year, ground water is protected, the release would not necessitate further remedial action for the disposal site, and the release is coordinated with all appropriate authorities. The 1995 release requirements also state

  19. Synthesis of Amino- and Nitro-Substituted Heterocycles as Insensitive Energetic Materials

    Energy Technology Data Exchange (ETDEWEB)

    Pagoria, P F; Lee, G S; Mitchell, A R; Schmidt, R D


    In this paper we will describe the synthesis of several amino- and nitro-substituted heterocycles, examples from a continuing research project targeted at the synthesis of new, insensitive energetic materials that possess at least 80% the power of HMX (28% more power than TATB). Recently we reported the synthesis and scale-up of the insensitive energetic material, 2,6-diamino-3,5-dinitropyrazine-1-oxide (LLM-105). The energy content (81% the power of HMX) and thermal stability of LLM-105 make it a viable candidate material for insensitive boosters and deep oil perforation. We will report on recent synthetic improvements and several performance and safety tests performed on LLM-105, including a 1 in. cylinder shot and plate dent. We will also report on the synthesis and characterization of 4-amino-3,5-dinitropyrazole (LLM-116), an interesting new insensitive energetic material with a measured crystal density of 1.90 g/cc, to our knowledge the highest density yet measured for a five-membered heterocycle containing amino- and nitro-substituents. LLM-116 was synthesized by reacting 3,5-dinitropyrazole with 1,1,1-trimethylhydrazinium iodide (TMHI) in DMSO in the presence of base. The synthesis and characterization of 4-amino-5-nitro-1,2,3-triazole (ANTZ) and 43-dinitro-1,2,3-triazole (DNTZ), first described by Baryshnikov and coworkers, will also be presented along with the synthesis of several new energetic materials derived from ANTZ and DNTZ.

  20. Synthesis and morphogenesis of organic and inorganic polymers by means of biominerals and biomimetic materials. (United States)

    Kijima, Misako; Oaki, Yuya; Munekawa, Yurika; Imai, Hiroaki


    We have studied the simultaneous synthesis and morphogenesis of polymer materials with hierarchical structures from nanoscopic to macroscopic scales. The morphologies of the original materials can be replicated to the polymer materials. In general, it is not easy to achieve the simultaneous synthesis and morphogenesis of polymer material even using host materials. In the present work, four biominerals and three biomimetic mesocrystal structures are used as the host materials or templates and polypyrrole, poly(3-hexylthiopehene), and silica were used as the precursors for the simultaneous syntheses and morphogenesis of polymer materials. The host materials with the hierarchical structure possess the nanospace for the incorporation of the monomers. After the incorporation of the monomers, the polymerization reaction proceeds in the nanospace with addition of the initiator agents. Then, the dissolution of the host materials leads to the formation and morphogenesis of the polymer materials. The scheme of the replication can be classified into the three types based on the structures of the host materials (types I-III). The type I template facilitates the hierarchical replication of the whole host material, type II mediates the hierarchical surface replication, and type III induces the formation of the two-dimensional nanosheets. Based on these results, the approach for the coupled synthesis and morphogenesis can be applied to a variety of combinations of the templates and polymer materials. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Control of conductivity type in undoped ZnO thin films grown by metalorganic vapor phase epitaxy (United States)

    Ma, Y.; Du, G. T.; Yang, S. R.; Li, Z. T.; Zhao, B. J.; Yang, X. T.; Yang, T. P.; Zhang, Y. T.; Liu, D. L.


    The properties of the ZnO thin films prepared by metalorganic vapor phase epitaxy under various oxygen partial pressures were thoroughly studied. It was found that the conduction type in undoped ZnO epilayers could be controlled by adjusting the family VI precursor, oxygen partial pressure during growth. The films were characteristic of n-type conductivity under oxygen partial pressure lower than 45 Pa. With the increase of oxygen content, the crystallinity of the ZnO thin films was degraded to polycrystalline with additional (10-12) orientation and the intrinsic p-type ZnO was produced as the oxygen partial pressure was larger than 55 Pa. The hole concentration and mobility could reach to 1.59×1016 cm-3 and 9.23 cm2 V-1 s-1, and the resistivity was 42.7 Ω cm. The near-band-edge emission and the deep level emission in photoluminescence (PL) spectra at room temperature were influenced strongly by the oxygen partial pressure. Temperature-dependent PL spectra in n-type ZnO films showed a dominant neutral-donor bound exciton emission, while p-ZnO was dominated by neutral-acceptor bound exciton emission. Both peaks increased in intensity with the decrease of the temperature and shifted to the short-wavelength side. The band that originated from zinc vacancies emerged at a temperature lower than 155 K only in the p-type films. The origin of intrinsic p-type conductivity in ZnO thin films might be related to zinc vacancy.

  2. Effect of Gold Dispersion on the Photocatalytic Activity of Mesoporous Titania for the Vapor-Phase Oxidation of Acetone

    Directory of Open Access Journals (Sweden)

    S. V. Awate


    Full Text Available Mesostructured titanium dioxide photocatalyst, having uniform crystallite size (6–12 nm and average pore diameter of ∼4.2 nm, was synthesized by using a low-temperature nonsurfactant hydrothermal route, employing tartaric acid as a templating agent. Gold additions from 0.5 to 2 wt% were incorporated, either during the hydrothermal process or by postsynthesis wet impregnation. Compared to the impregnation-prepared samples, the samples synthesized hydrothermally contained smaller-size (≤1 nm gold clusters occluded in the pores of the host matrix. Whereas CO2 and H2O were the main reaction products in UV-assisted vapor-phase oxidation of acetone using these catalysts, C2H6 and HCO2CH3 were also produced for higher acetone concentrations in air. The conversion of acetone was found to increase with decrease in the size of both TiO2 and gold particles. In situ IR spectroscopy revealed that titania and gold particles serve as independent adsorption and reaction sites for acetone and oxygen molecules. Acetone molecules adsorb exclusively at TiO2 surface, giving rise to a strongly adsorbed (condensed state as well as to the formation of formate- and methyl formate-type surface species. Hydroxyl groups at titania surface participate directly in these adsorption steps. Nanosize gold particles, on the other hand, were primarily responsible for the adsorption and activation of oxygen molecules. Mechanistic aspects of the photochemical processes are discussed on the basis of these observations.

  3. Chemical Species in the Vapor Phase of Hanford Double-Shell Tanks: Potential Impacts on Waste Tank Corrosion Processes

    Energy Technology Data Exchange (ETDEWEB)

    Felmy, Andrew R.; Qafoku, Odeta; Arey, Bruce W.; Boomer, Kayle D.


    The presence of corrosive and inhibiting chemicals on the tank walls in the vapor space, arising from the waste supernatant, dictate the type and degree of corrosion that occurs there. An understanding of how waste chemicals are transported to the walls and the affect on vapor species from changing supernatant chemistry (e.g., pH, etc.), are basic to the evaluation of risks and impacts of waste changes on vapor space corrosion (VSC). In order to address these issues the expert panel workshop on double-shell tank (DST) vapor space corrosion testing (RPP-RPT-31129) participants made several recommendations on the future data and modeling needs in the area of DST corrosion. In particular, the drying of vapor phase condensates or supernatants can form salt or other deposits at the carbon steel interface resulting in a chemical composition at the near surface substantially different from that observed directly in the condensates or the supernatants. As a result, over the past three years chemical modeling and experimental studies have been performed on DST supernatants and condensates to predict the changes in chemical composition that might occur as condensates or supernatants equilibrate with the vapor space species and dry at the carbon steel surface. The experimental studies included research on both the chemical changes that occurred as the supernatants dried as well as research on how these chemical changes impact the corrosion of tank steels. The chemical modeling and associated experimental studies were performed at the Pacific Northwest National Laboratory (PNNL) and the research on tank steel corrosion at the Savannah River National Laboratory (SRNL). This report presents a summary of the research conducted at PNNL with special emphasis on the most recent studies conducted in FY10. An overall summary of the project results as well as their broader implications for vapor space corrosion of the DST’s is given at the end of this report.

  4. Position-controlled III-V compound semiconductor nanowire solar cells by selective-area metal-organic vapor phase epitaxy. (United States)

    Fukui, Takashi; Yoshimura, Masatoshi; Nakai, Eiji; Tomioka, Katsuhiro


    We demonstrate position-controlled III-V semiconductor nanowires (NWs) by using selective-area metal-organic vapor phase epitaxy and their application to solar cells. Efficiency of 4.23% is achieved for InP core-shell NW solar cells. We form a 'flexible NW array' without a substrate, which has the advantage of saving natural resources over conventional thin film photovoltaic devices. Four junction NW solar cells with over 50% efficiency are proposed and discussed.

  5. Vapor-phase cristobalite as a durable indicator of magmatic pore structure and halogen degassing: an example from White Island volcano (New Zealand) (United States)

    Ian Schipper, C.; Mandon, Céline; Maksimenko, Anton; Castro, Jonathan M.; Conway, Chris E.; Hauer, Peter; Kirilova, Martina; Kilgour, Geoff


    Vesicles in volcanic rocks are physical records of magmatic degassing; however, the interpretation of their textures is complicated by resorption, coalescence, and collapse. We discuss the textural significance of vesicle-hosted vapor-phase cristobalite (high-T, low-P SiO2 polymorph), and its utility as a complement to textural assessments of magmatic degassing, using a representative dacite bomb erupted from White Island volcano (New Zealand) in 1999. Imaging in 2D (SEM) and 3D (CT) shows the bomb to have 56% bulk porosity, almost all of which is connected ( 99%) and devoid of SiO2 phases. The remaining ( 1%) of porosity is in isolated, sub-spherical vesicles that have corroded walls and contain small (< 30 μm across) prismatic vapor-phase cristobalite crystals (98.4 ± 0.4 wt.% SiO2 with diagnostic laser Raman spectra). Halogen degassing models show vapor-phase cristobalite to be indicative of closed-system chlorine and fluorine partitioning into H2O-rich fluid in isolated pores. At White Island, this occurred during shallow (< 100s of meters) ascent and extensive ( 50%) groundmass crystallization associated with slow cooling in a volcanic plug. Pristine textures in this White Island bomb demonstrate the link between pore isolation and vapor-phase cristobalite deposition. We suggest that because these crystals have higher preservation potential than the bubbles in which they form, they can serve as durable, qualitative textural indicators of halogen degassing and pre-quench bubble morphologies in slowly cooled volcanic rocks (e.g., lava flows and domes), even where emplacement mechanisms have overprinted original bubble textures.

  6. Molecular interactions between organized, surface-confined monolayers and vapor-phase probe molecules. 6. In-situ FTIR external reflectance spectroscopy of monolayer adsorption and reaction chemistry

    Energy Technology Data Exchange (ETDEWEB)

    Xu, C.; Sun, L.; Kepley, L.J.; Crooks, R.M. (Univ. of New Mexico, Albuquerque (United States)); Ricco, A.J. (Sandia National Lab., Albuquerque, NM (United States))


    A new in-situ application of FTIR external reflectance spectroscopy (FTIR-ESR), which is useful for real-time evaluation of monolayer and multilayer adsorption and reaction chemistry at the vapor/solid interface at pressures near 1 atm, is described. The utility and versatility of the method is illustrated by two proof-of-concept experiments. The first experiment involves adsorption of H[sub 2]N(CH[sub 2])[sub 9]CH[sub 3] onto a naked Au substrate from the vapor phase. In-situ FTIR-ERS indicates that the amine forms a stable, ordered monolayer on the Au surface; that is, H[sub 2]N(CH[sub 2])[sub 9]CH[sub 3] self-assembles onto the Au surface from the vapor phase. The second experiment involves vapor-phase adsorption of a HS(C[sub 6]H[sub 5])OH monolayer onto a naked Au surface, followed by an in-situ coupling reaction with [CH[sub 3](CH[sub 2])[sub 7

  7. Application of a Diffusion-denuder Method for the Investigation of the Effects of ‘Smoke pH’ on Vapor-phase Nicotine Yields from Different Types of Cigarettes


    Cochran EW; Joseph MJ; Stinson SS; Summers SS


    The potential effects of smoke pH on vapor-phase nicotine, or unprotonated nicotine, were investigated using a diffusion denuder method selected for its ability to quantitatively monitor vapor-phase nicotine in the presence of smoke particulate. For the purpose of this paper, the pH of the water-soluble fraction of mainstream cigarette smoke will be referred to as ‘smoke pH'. In this study, samples with different construction parameters affecting smoke pH were analyzed for percent vapor-phase...

  8. Synthesis and characterization of mesoporous Si-MCM-41 materials ...

    Indian Academy of Sciences (India)


    synthesis of plasticizers, perfumes, fragrance in cosme- tics, flavours in food, diluents in paints and coatings and intermediates in drugs, dye stuffs and fine chemicals. (Otera 2003). The conventional catalyst used in esterifi- cation reactions is sulphuric acid, methanesulfonic acid or p-toluenesulfonic acid that are cited as ...

  9. Microwave synthesis of electrode materials for lithium batteries

    Indian Academy of Sciences (India)


    Bi4B2O9 have been used as cathodes (Jones and Akridge. 1995). ... reactive, is a superb secondary heater (Vaidhyanathan et al 1997). Researches at our laboratory and elsewhere have demonstrated the use of microwaves in the synthesis of a wide ... 1997a), silicides (Vaidhyanathan and Rao 1997b), borides. (Mingos ...

  10. Scalable synthesis and energy applications of defect engineeered nano materials (United States)

    Karakaya, Mehmet

    Nanomaterials and nanotechnologies have attracted a great deal of attention in a few decades due to their novel physical properties such as, high aspect ratio, surface morphology, impurities, etc. which lead to unique chemical, optical and electronic properties. The awareness of importance of nanomaterials has motivated researchers to develop nanomaterial growth techniques to further control nanostructures properties such as, size, surface morphology, etc. that may alter their fundamental behavior. Carbon nanotubes (CNTs) are one of the most promising materials with their rigidity, strength, elasticity and electric conductivity for future applications. Despite their excellent properties explored by the abundant research works, there is big challenge to introduce them into the macroscopic world for practical applications. This thesis first gives a brief overview of the CNTs, it will then go on mechanical and oil absorption properties of macro-scale CNT assemblies, then following CNT energy storage applications and finally fundamental studies of defect introduced graphene systems. Chapter Two focuses on helically coiled carbon nanotube (HCNT) foams in compression. Similarly to other foams, HCNT foams exhibit preconditioning effects in response to cyclic loading; however, their fundamental deformation mechanisms are unique. Bulk HCNT foams exhibit super-compressibility and recover more than 90% of large compressive strains (up to 80%). When subjected to striker impacts, HCNT foams mitigate impact stresses more effectively compared to other CNT foams comprised of non-helical CNTs (~50% improvement). The unique mechanical properties we revealed demonstrate that the HCNT foams are ideally suited for applications in packaging, impact protection, and vibration mitigation. The third chapter describes a simple method for the scalable synthesis of three-dimensional, elastic, and recyclable multi-walled carbon nanotube (MWCNT) based light weight bucky-aerogels (BAGs) that are

  11. MPA-11: Materials Synthesis and Integrated Devices; Overview of an Applied Energy Group

    Energy Technology Data Exchange (ETDEWEB)

    Dattelbaum, Andrew Martin [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)


    Our mission is to provide innovative and creative chemical synthesis and materials science solutions to solve materials problems across the LANL missions. Our group conducts basic and applied research in areas related to energy security as well as problems relevant to the Weapons Program.

  12. Electrochemical synthesis of nanostructured materials for electrochemical energy conversion and storage. (United States)

    Li, Gao-Ren; Xu, Han; Lu, Xue-Feng; Feng, Jin-Xian; Tong, Ye-Xiang; Su, Cheng-Yong


    Electrochemical synthesis represents a highly efficient method for the fabrication of nanostructured energy materials, and various nanostructures, such as nanorods, nanowires, nanotubes, nanosheets, dendritic nanostructures, and composite nanostructures, can be easily fabricated with advantages of low cost, low synthetic temperature, high purity, simplicity, and environmental friendliness. The electrochemical synthesis, characterization, and application of electrochemical energy nanomaterials have advanced greatly in the past few decades, allowing an increasing understanding of nanostructure-property-performance relationships. Herein, we highlight some recent progress in the electrochemical synthesis of electrochemical energy materials with the assistance of additives and templates in solution or grafted onto metal or conductive polymer supports, with special attention to the effects on surface morphologies, structures and, more importantly, electrochemical performance. The methodology for preparing novel electrochemical energy nanomaterials and their potential applications has been summarized. Finally, we outline our personal perspectives on the electrochemical synthesis and applications of electrochemical energy nanomaterials.

  13. Fundamentals and applications of organic electrochemistry synthesis, materials, devices

    CERN Document Server

    Fuchigami, Toshio; Inagi, Shinsuke


    This textbook is an accessible overview of the broad field of organic electrochemistry, covering the fundamentals and applications of contemporary organic electrochemistry.  The book begins with an introduction to the fundamental aspects of electrode electron transfer and methods for the electrochemical measurement of organic molecules. It then goes on to discuss organic electrosynthesis of molecules and macromolecules, including detailed experimental information for the electrochemical synthesis of organic compounds and conducting polymers. Later chapters highlight new methodology for organic electrochemical synthesis, for example electrolysis in ionic liquids, the application to organic electronic devices such as solar cells and LEDs, and examples of commercialized organic electrode processes. Appendices present useful supplementary information including experimental examples of organic electrosynthesis, and tables of physical data (redox potentials of various organic solvents and organic compounds and phy...

  14. Room-temperature Electrochemical Synthesis of Carbide-derived Carbons and Related Materials

    Energy Technology Data Exchange (ETDEWEB)

    Gogotsi, Yury [Drexel Univ., Philadelphia, PA (United States). Nanomaterials Group. Materials Science and Engineering Dept.


    This project addresses room-temperature electrochemical etching as an energy-efficient route to synthesis of 3D nanoporous carbon networks and layered 2D carbons and related structures, as well as provides fundamental understanding of structure and properties of materials produced by this method. Carbide-derived-carbons (CDCs) are a growing class of nanostructured carbon materials with properties that are desirable for many applications, such as electrical energy and gas storage. The structure of these functional materials is tunable by the choice of the starting carbide precursor, synthesis method, and process parameters. Moving from high-temperature synthesis of CDCs through vacuum decomposition above 1400°C and chlorination above 400°C, our studies under the previous DOE BES support led to identification of precursor materials and processing conditions for CDC synthesis at temperatures as low as 200°C, resulting in amorphous and highly reactive porous carbons. We also investigated synthesis of monolithic CDC films from carbide films at 250-1200°C. The results of our early studies provided new insights into CDC formation, led to development of materials for capacitive energy storage, and enabled fundamental understanding of the electrolyte ions confinement in nanoporous carbons.

  15. Microfluidic synthesis of composite cross-gradient materials for investigating cell-biomaterial interactions. (United States)

    He, Jiankang; Du, Yanan; Guo, Yuqi; Hancock, Matthew J; Wang, Ben; Shin, Hyeongho; Wu, Jinhui; Li, Dichen; Khademhosseini, Ali


    Combinatorial material synthesis is a powerful approach for creating composite material libraries for the high-throughput screening of cell-material interactions. Although current combinatorial screening platforms have been tremendously successful in identifying target (termed "hit") materials from composite material libraries, new material synthesis approaches are needed to further optimize the concentrations and blending ratios of the component materials. Here we employed a microfluidic platform to rapidly synthesize composite materials containing cross-gradients of gelatin and chitosan for investigating cell-biomaterial interactions. The microfluidic synthesis of the cross-gradient was optimized experimentally and theoretically to produce quantitatively controllable variations in the concentrations and blending ratios of the two components. The anisotropic chemical compositions of the gelatin/chitosan cross-gradients were characterized by Fourier transform infrared spectrometry and X-ray photoelectron spectrometry. The three-dimensional (3D) porous gelatin/chitosan cross-gradient materials were shown to regulate the cellular morphology and proliferation of smooth muscle cells (SMCs) in a gradient-dependent manner. We envision that our microfluidic cross-gradient platform may accelerate the material development processes involved in a wide range of biomedical applications. © 2010 Wiley Periodicals, Inc.

  16. Surface modification of aramid fiber by plasma induced vapor phase graft polymerization of acrylic acid. I. Influence of plasma conditions

    Energy Technology Data Exchange (ETDEWEB)

    Wang, C.X., E-mail: [College of Textiles and Clothing, Yancheng Institute of Technology, Jiangsu 224003 (China); School of Textile and Clothing, Nantong University, Jiangsu 226019 (China); Du, M. [College of Textiles and Clothing, Yancheng Institute of Industry Technology, Jiangsu 224000 (China); Lv, J.C.; Zhou, Q.Q. [College of Textiles and Clothing, Yancheng Institute of Technology, Jiangsu 224003 (China); Ren, Y. [School of Textile and Clothing, Nantong University, Jiangsu 226019 (China); Liu, G.L.; Gao, D.W. [College of Textiles and Clothing, Yancheng Institute of Technology, Jiangsu 224003 (China); Jin, L.M. [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201204 (China)


    Highlights: • Aramid fiber surface was modified by PIVPGP of AA to improve wettability, adhesion. • Surface modification effect by PIVPGP of AA increased and then decreased with time. • Surface modification effect increased and then stayed unaltered with output power. • Ar plasma was the most effective in PIVPGP of AA on aramid fiber surface. • In studied range, optimum technology of PIVPGP of AA: Ar plasma, 15 min, 300 W. - Abstract: Plasma induced vapor phase graft polymerization (PIVPGP) method was applied to modify aramid fiber surface. In this study, aramid fibers were pretreated under various plasma conditions such as different treatment times, output powers and working gases to see how these plasma processing parameters influenced the PIVPGP of acrylic acid (AA) on aramid fiber surface and its surface structure and properties. The analysis results of atomic force microscope (AFM) and X-ray photoelectron spectroscope (XPS) showed the increase of surface roughness and the introduction of O=C−OH, which confirmed that the PIVPGP of AA on aramid fiber surface was achieved. The contact angle and interfacial shear strength (IFSS) of the aramid fibers modified by PIVPGP of AA prominently decreased and increased, respectively, indicating the obvious improvements of surface wettability and adhesion between aramid fiber and matrix. The surface modification effects of aramid fiber by PIVPGP of AA firstly increased and then after 15 min slightly decreased with the increasing plasma treatment time, and but firstly increased and then after 300 W nearly remained unchanged with the increasing output power, respectively. Among different working gases, Ar plasma occupied first place, O{sub 2} plasma and N{sub 2} plasma came second and third in the aspect of PIVPGP of AA on aramid fiber surface, respectively. It could be concluded that the PIVPGP of AA on aramid fiber surface could effectively improve surface wettability and adhesion. Plasma conditions had signally

  17. Conventional and pendeo-epitaxial growth of III-nitride thin films by molecular beam and metalorganic vapor phase techniques (United States)

    Linthicum, Kevin James

    Reactive gas-source molecular beam epitaxy was employed for the growth of monocrystalline GaN(0001) thin films. On-surface cracking of ammonia at 800°C was the method of choice for obtaining reactive nitrogen-containing species and growth rates of 2500A/hr were achieved. Pendeo-epitaxy, a general form of selective lateral growth, was developed for the organometallic vapor phase epitaxy growth of GaN and AlGaN thin films on GaN/AlN/6H-SiC(0001) substrates. In this technique, selective lateral growth was forced to initiate from the (1120) sidewalls of etched GaN seed forms by incorporating a silicon nitride seed mask atop the forms and employing the SiC substrate as a pseudo-mask. Coalescence over and between the seed forms was achieved. Transmission electron microscopy revealed that all vertically threading defects stemming from the GaN/AlN and AlN/SiC interfaces were contained within the seed forms and that a substantial reduction in the dislocation density of the laterally grown GaN was achieved. To achieve pendeo-epitaxial growth of monocrystalline GaN films on Si(111) substrates, a series of additional process steps was required, including the formation of a SiC chemical/reaction barrier. Single-crystal beta-SiC(111) thin films were obtained via carburization of the near-surface regions of vicinal Si(111). The thickness of the converted layers was approximately 5nm. Thick (500nm), epitaxial 3C-SiC layers grown via atmospheric pressure chemical vapor deposition were also used in tandem with the carburized silicon substrates. Monocrystalline AlN(0001) layers were grown on the SiC/Si substrates at 1100°C via MOVPE. Single-crystal wurtzitic GaN(0001) seed layers were grown on the AlN(0001) layers. The FWHM of the GaN(0002) x-ray diffraction and the photoluminescence band-edge emission peaks were 1443 arcsec and 19 meV, respectively. Pendeo-epitaxial growth of GaN on GaN/AlN/3C-SiC/Si(111) raised stripes was achieved. Crystallographic tilting of 0.2°(720 arcsec

  18. Fabrication of solid state dye sensitized solar cells utilizing vapor phase polymerized poly(3,4-ethylenedioxythiophene) hole conducting layer (United States)

    Skorenko, Kenneth H.

    There is a need for sustainable and renewable energy sources that can be used in both grid and off-grid structured systems. Photovoltaic devices have been used to generate electrical energy by capturing and converting photons from the sun. Dye sensitized solar cells (DSSC) have gained attention due to their consistent energy generation during indirect sunlight. Furthermore, DSSC can be applied as a flexible device and gain benefits from the low cost roll to roll manufacturing. With this in mind, we have taken steps toward optimizing a DSSC device for use as a solid state solar cell using conducting polymers. Typically DSSC use a liquid electrolyte as a hole conducting layer used to direct the separation of electron -- hole pairs. This liquid electrolyte comes with problems that can be subverted using conducting polymers. Poly(3,4 -- ethylenedioxythiophene) (PEDOT), is a conducting thiophene that is tailored to have enhanced conductivity. We show that a vapor phase polymerization (VPP) of PEDOT can be used as a hole conducting layer in a solid state DSSC device. To this end we have investigated the electrical properties of the VPP PEDOT films in order to understand how the morphology and conductive domains relate to a polymers conductivity. Using 4 point probe we have measure the sheet resistance of the film, as well as how the films resistance is altered during stress tests. Scanning electron microscopy has been utilized to compare morphologies of different PEDOT films and see how surface morphology impacts the conductance measured. Using conductive atomic force microscopy we can look at the conductive domains between VPP PEDOT and PEDOT:PSS films. We saw that conductive domains of the VPP PEDOT are not only more conductive but also much larger in size and widespread throughout the film. We show that there is formation of PEDOT through optical spectroscopy and structural characterization such as UV/Vis and Raman spectroscopy as well as X-ray diffraction. When

  19. Analysis of Acrylonitrile and alpha-Methacrylonitrile in Vapor Phase of Mainstream Cigarette Smoke Using a Charcoal Trap for Collection

    Directory of Open Access Journals (Sweden)

    Moldoveanu SC


    Full Text Available A simple procedure for the collection of vapor phase (VP of mainstream cigarette smoke for analysis has been developed. This procedure consists of collecting the VP on a commercial charcoal trap (ORBO™-32 followed by dissolution in acetone. The acetone extract can be analyzed by a gas chromatography/mass spectrometry (GC/MS technique. A qualitative analysis of the collected VP has been performed for 3R4F Kentucky reference cigarette, allowing the identification of 138 compounds, some compounds being present in both VP and in particulate phase (PP of cigarette smoke. A quantitative analysis method for acrylonitrile and α-methacrylonitrile (2-methyl-2-propenenitrile was also developed, and the level of these compounds in 15 different cigarette brands was measured. Acrylonitrile quantitation was selected since this compound in smoke poses significant health related issues. α-Methacrylonitrile quantitation was selected due to the similar structure of this compound with acrylonitrile. The analyzed cigarettes were several Kentucky reference cigarettes including 1R5F, 2R4F, 3R4F, 2R1F, and 1R3F, several King Size (KS commercial cigarettes from the US market including Basic Non Filter (NF, Basic Ultra Lights (UL, Newport, Marlboro (Red, Marlboro Menthol, Camel Filter, Camel Lights, Camel Ultra Lights, and two herbal cigarettes, Ecstasy and Dreams. The results for acrylonitrile were in very good agreement with data reported in the literature for 2R4F and 1R5F cigarettes. The levels of α-methacrylonitrile were not previously reported. The correlation between the levels of acrylonitrile and of α-methacrylonitrile with the (wet total particulate matter (TPM was evaluated. Although the levels of acrylonitrile and of α-methacrylonitrile in mainstream smoke depend on the TPM values, the correlation is not very strong, indicating that the nature of the cigarette blend and possible other factors in cigarette construction also influence their levels in

  20. Controlled synthesis of the tricontinuous mesoporous material IBN-9 and its carbon and platinum derivatives

    KAUST Repository

    Zhao, Yunfeng


    Controlled synthesis of mesoporous materials with ultracomplicated pore configurations is of great importance for both fundamental research of nanostructures and the development of novel applications. IBN-9, which is the only tricontinuous mesoporous silica with three sets of interpenetrating three-dimensional channel systems, appears to be an excellent model mesophase for such study. The extensive study of synthesis space diagrams proves mesophase transition among the cylindrical MCM-41, tricontinuous IBN-9 and bicontinuous MCM-48, and also allows a more precise control of phase-pure synthesis. On the other hand, rational design of structure-directing agents offers a possibility to extend the synthesis conditions of IBN-9, as well as tailor its pore size. Moreover, an unprecedented helical structure consisting of twisted 3-fold interwoven mesoporous channels is reported here for the first time. The unique tricontinuous mesostructure of IBN-9 has been well-replicated by other functional materials (e.g., carbon and platinum) via a "hard- templating" synthesis route. The obtained carbon material possesses large surface area (∼1900 m2/g), high pore volume (1.56 cm 3/g), and remarkable gas adsorption capability at both cryogenic temperatures and room temperature. The platinum material has an ordered mesostructure composed of highly oriented nanocrystals. © 2011 American Chemical Society.

  1. The Effects of Gravity on Combustion and Structure Formation During Synthesis of Advanced Materials (United States)

    Varma, A.; Pelekh, A.; Mukasyan, A.


    Combustion in a variety of heterogeneous systems, leading to the synthesis of advanced materials, is characterized by high temperatures (2000-3500 K) and heating rates (up to 10(exp 6) K/s) at and ahead of the reaction front. These high temperatures generate liquids and gases which are subject to gravity-driven flow. The removal of such gravitational effects is likely to provide increased control of the reaction front, with a consequent improvement in control of the microstructure of the synthesized products. Thus, microgravity experiments can lead to major advances in the understanding of fundamental aspects of combustion and structure formation under the extreme conditions of the combustion synthesis wave. In addition, the specific features of microgravity environment allow one to produce unique materials, which cannot be obtained under terrestrial conditions. The general goals of the current research are: 1) to improve the understanding of fundamental phenomena taking place during combustion of heterogeneous systems, 2) to use low-gravity experiments for insight into the physics and chemistry of materials synthesis processes, and 3) based on the obtained knowledge, to optimize processing conditions for synthesis of advanced materials with desired microstructures and properties. This research follows logically from the results of investigations we have conducted in the framework of our previous grant on gravity influence on combustion synthesis (CS) of gasless systems. Prior work, by others and by us, has clearly demonstrated that gravity plays an important role during combustion synthesis of materials. The immediate tasks for the future are to quantitatively identify the nature of observed effects, and to create accurate local kinetic models of the processes, which can lead to a control of the microstructure and properties of the synthesized materials. In summary, this is the value of the proposed research. Based on our prior work, we focus on the fundamental

  2. Microwave synthesis of electrode materials for lithium batteries

    Indian Academy of Sciences (India)

    A novel microwave method is described for the preparation of electrode materials required for lithium batteries. The method is simple, fast and carried out in most cases with the same starting material as in conventional methods. Good crystallinity has been noted and lower temperatures of reaction has been inferred in ...

  3. Synthesis and characterization of a new organic semiconductor material

    Energy Technology Data Exchange (ETDEWEB)

    Tiffour, Imane [Laboratoire de Génie Physique, Département de Physique, Université de Tiaret, Tiaret 14000 (Algeria); Faculté des Sciences et Technologies, Université Mustapha Stambouli, Mascara 29000 (Algeria); Dehbi, Abdelkader [Laboratoire de Génie Physique, Département de Physique, Université de Tiaret, Tiaret 14000 (Algeria); Mourad, Abdel-Hamid I., E-mail: [Mechanical Engineering Department, Faculty of Engineering, United Arab Emirates University, Al-Ain, P.O. Box 15551 (United Arab Emirates); Belfedal, Abdelkader [Faculté des Sciences et Technologies, Université Mustapha Stambouli, Mascara 29000 (Algeria); LPCMME, Département de Physique, Université d' Oran Es-sénia, 3100 Oran (Algeria)


    The objective of this study is to create an ideal mixture of Acetaminophen/Curcumin leading to a new and improved semiconductor material, by a study of the electrical, thermal and optical properties. This new material will be compared with existing semiconductor technology to discuss its viability within the industry. The electrical properties were investigated using complex impedance spectroscopy and optical properties were studied by means of UV-Vis spectrophotometry. The electric conductivity σ, the dielectric constant ε{sub r}, the activation energy E{sub a}, the optical transmittance T and the gap energy E{sub g} have been investigated in order to characterize our organic material. The electrical conductivity of the material is approximately 10{sup −5} S/m at room temperature, increasing the temperature causes σ to increase exponentially to approximately 10{sup −4} S/m. The activation energy obtained for the material is equal to 0.49 ± 0.02 ev. The optical absorption spectra show that the investigating material has absorbance in the visible range with a maximum wavelength (λ{sub max}) 424 nm. From analysis, the absorption spectra it was found the optical band gap equal to 2.6 ± 0.02 eV and 2.46 ± 0.02 eV for the direct and indirect transition, respectively. In general, the study shows that the developed material has characteristics of organic semiconductor material that has a promising future in the field of organic electronics and their potential applications, e.g., photovoltaic cells. - Highlights: • Development of a new organic acetaminophen/Curcumin semiconductor material. • The developed material has characteristics of an organic semiconductor. • It has electrical conductivity comparable to available organic semiconductors. • It has high optical transmittance and low permittivity/dielectric constant.

  4. Investigation on Indium-Filled Skutterudite Materials Prepared by Combining Hydrothermal Synthesis and Hot Pressing (United States)

    Du, Y.; Cai, K. F.; Chen, S.; Qin, Z.; Shen, S. Z.


    Indium-filled CoSb3 materials have been investigated by combining hydrothermal synthesis and hot pressing. The materials were prepared as follows. Corresponding nanopowders were synthesized by a hydrothermal synthesis method, in some cases followed by melting at 1373 K, and then hot pressed at 923 K. The phase composition and microstructure of the bulk materials were analyzed by conventional methods, such as x-ray diffraction (XRD), scanning electron microscopy (SEM), and field-emission SEM equipped with energy-dispersive x-ray spectroscopy (EDS). The thermoelectric properties of the bulk materials were measured from room temperature to 773 K. The results reveal that indium can be successfully filled into the voids of the CoSb3 structure when the sample preparation procedure contains melting. The influence of the processing on the thermoelectric properties of the materials is also discussed.

  5. Synthesis of new porphyrinoids for biomedical and materials applications (United States)

    Stewart, Fraser

    The facile synthesis of three non-hydrolysable thioglycosylated porphyrinoids is reported. Starting from meso perfluorophenylporphyrin (TPPF20), the non-hydrolysable thioglycosylated porphyrin (PGlc4), chlorin (CGlc4), isobacteriochlorin (IGlc4), and bacteriochlorin (BGlc4) can be made in 2-3 steps. The ability to append a wide range of targeting agents onto the perfluorophenyl moieties, the chemical stability, and the ability to fine-tune the photophysical properties of the chromophores make this a suitable platform for development of biochemical tags, diagnostics, or as photodynamic therapeutic agents. With reduction of one or two pyrrole double bonds, there is a red shift in the lowest energy absorption band and a significant increase in intensity. The fluorescence of these porphyrinoids is in the order PGlc4 = BGlc4 treatment with these four porphyrinoids indicate they are taken up. The CGlc4 and IGlc4 may be dual function agents that can detect cancer by luminescence, and treat cancer by photodynamic therapy (PDT). Porphyrins appended with four rigid hydrogen bonding motifs on the meso positions were synthesized and self-assembled into a cofacial cage with four complementary bis- (decyl)melamine units in dry solvents, these hydrogen-bonded cages were analysed by diffusion-ordered spectroscopy (DOSY) in solution. The hydrocarbon chains on the melamine mediate the formation of nanofilms on surfaces as the solvent slowly evaporates. A water soluble zinc (II) phthalocyanine symmetrically appended with eight thioglucose units was synthesized from commercially available hexadecafluoro-phthalocyaninato zinc(II) by controlled nucleophilic substitution of the peripheral fluoro groups by thio-sugars. The photophysical properties and cancer cell uptake studies of this nonhydrolyzable thioglycosylated phthalocyanine are reported. The new compound has amphiphilic character, is chemically and photochemically stable, and can potentially be used as a photosensitizer in

  6. Highly Loaded Fe-MCM-41 Materials: Synthesis and Reducibility Studies

    Directory of Open Access Journals (Sweden)

    Malose P. Mokhonoana


    Full Text Available Fe-MCM-41 materials were prepared by different methods. The Fe was both incorporated into the structure and formed crystallites attached to the silica. High Fe content MCM-41 (~16 wt% with retention of mesoporosity and long-range order was achieved by a range of new synthetic methodologies: (i by delaying the addition of Fe3+(aq to the stirred synthesis gel by 2 h, (ii by addition of Fe3+ precursor as a freshlyprecipitated aqueous slurry, (iii by exploiting a secondary synthesis with Si-MCM-41 as SiO2 source. For comparative purposes the MCM-41 was also prepared by incipient wetness impregnation (IWI. Although all these synthesis methods preserved mesoporosity and long-range order of the SiO2 matrix, the hydrothermally-fabricated Fe materials prepared via the secondary synthesis route has the most useful properties for exploitation as a catalyst, in terms of hydrothermal stability of the resulting support. Temperatureprogrammed reduction (TPR studies revealed a three-peak reduction pattern for this material instead of the commonly observed two-peak reduction pattern. The three peaks showed variable intensity that related to the presence of two components: crystalline Fe2O3 and Fe embedded in the SiO2 matrix (on the basis of ESR studies. The role of secondary synthesis of Si-MCM-41 on the iron reducibility was also demonstrated in IWI of sec-Si-MCM-41.

  7. Precursor Mediated Synthesis of Nanostructured Silicas: From Precursor-Surfactant Ion Pairs to Structured Materials

    Directory of Open Access Journals (Sweden)

    Peter Hesemann


    Full Text Available The synthesis of nanostructured anionic-surfactant-templated mesoporous silica (AMS recently appeared as a new strategy for the formation of nanostructured silica based materials. This method is based on the use of anionic surfactants together with a co-structure-directing agent (CSDA, mostly a silylated ammonium precursor. The presence of this CSDA is necessary in order to create ionic interactions between template and silica forming phases and to ensure sufficient affinity between the two phases. This synthetic strategy was for the first time applied in view of the synthesis of surface functionalized silica bearing ammonium groups and was then extended on the formation of materials functionalized with anionic carboxylate and bifunctional amine-carboxylate groups. In the field of silica hybrid materials, the “anionic templating” strategy has recently been applied for the synthesis of silica hybrid materials from cationic precursors. Starting from di- or oligosilylated imidazolium and ammonium precursors, only template directed hydrolysis-polycondensation reactions involving complementary anionic surfactants allowed accessing structured ionosilica hybrid materials. The mechanistic particularity of this approach resides in the formation of precursor-surfactant ion pairs in the hydrolysis-polycondensation mixture. This review gives a systematic overview over the various types of materials accessed from this cooperative ionic templating approach and highlights the high potential of this original strategy for the formation of nanostructured silica based materials which appears as a complementary strategy to conventional soft templating approaches.

  8. Precursor Mediated Synthesis of Nanostructured Silicas: From Precursor-Surfactant Ion Pairs to Structured Materials (United States)

    Hesemann, Peter; Nguyen, Thy Phung; Hankari, Samir El


    The synthesis of nanostructured anionic-surfactant-templated mesoporous silica (AMS) recently appeared as a new strategy for the formation of nanostructured silica based materials. This method is based on the use of anionic surfactants together with a co-structure-directing agent (CSDA), mostly a silylated ammonium precursor. The presence of this CSDA is necessary in order to create ionic interactions between template and silica forming phases and to ensure sufficient affinity between the two phases. This synthetic strategy was for the first time applied in view of the synthesis of surface functionalized silica bearing ammonium groups and was then extended on the formation of materials functionalized with anionic carboxylate and bifunctional amine-carboxylate groups. In the field of silica hybrid materials, the “anionic templating” strategy has recently been applied for the synthesis of silica hybrid materials from cationic precursors. Starting from di- or oligosilylated imidazolium and ammonium precursors, only template directed hydrolysis-polycondensation reactions involving complementary anionic surfactants allowed accessing structured ionosilica hybrid materials. The mechanistic particularity of this approach resides in the formation of precursor-surfactant ion pairs in the hydrolysis-polycondensation mixture. This review gives a systematic overview over the various types of materials accessed from this cooperative ionic templating approach and highlights the high potential of this original strategy for the formation of nanostructured silica based materials which appears as a complementary strategy to conventional soft templating approaches. PMID:28788602

  9. High quality factor whispering gallery modes from self-assembled hexagonal GaN rods grown by metal-organic vapor phase epitaxy. (United States)

    Tessarek, C; Sarau, G; Kiometzis, M; Christiansen, S


    Self-assembled GaN rods were grown on sapphire by metal-organic vapor phase epitaxy using a simple two-step method that relies first on a nitridation step followed by GaN epitaxy. The mask-free rods formed without any additional catalyst. Most of the vertically aligned rods exhibit a regular hexagonal shape with sharp edges and smooth sidewall facets. Cathodo- and microphotoluminescence investigations were carried out on single GaN rods. Whispering gallery modes with quality factors greater than 4000 were measured demonstrating the high morphological and optical quality of the self-assembled GaN rods.

  10. Vapor-phase infrared and Raman spectra and ab-initio calculations of the axial and equatorial forms of cyclohexane-d1 and d11 (United States)

    Chun, Hye Jin; Ocola, Esther J.; Laane, Jaan


    The vapor-phase infrared and Raman spectra of cyclohexane-d11 in the C-H stretching region show two bands at 2891 and 2921 cm-1 corresponding to the axial and equatorial C-H stretching modes respectively. Similarly, cyclohexane-d1 has two C-D stretching modes at 2145 and 2164 cm-1 (Mátrai and Gal, 1984) corresponding to the two forms. Force constants were calculated for these vibrations and these confirm the theoretical calculations, which show the equatorial bonds to be shorter and stronger. The force constant for the equatorial C-H stretching is 2% higher than for the axial.

  11. Synthesis of Helical Carbon Fibers and Related Materials: A Review on the Past and Recent Developments

    Directory of Open Access Journals (Sweden)

    Himanshu Raghubanshi


    Full Text Available Helical carbon fibers (HCFs have been widely studied due to their unique helical morphology and superior properties, which make them efficient materials for several potential applications. This review summarizes the past and current advancement on the synthesis of HCFs. The review focuses and discusses synthesis strategies and effect of experimental parameters on the growth of HCFs. The effect of preparation method of catalyst, catalyst nature, catalyst composition, catalyst size, catalyst initial and final shape, reaction temperature, reaction time, carbon source, impurities, and electromagnetic field on the growth of HCFs is reviewed. We also discuss the growth mechanism for HCFs and the synthesis of HCFs related materials. Finally, we conclude with a brief summary and an outlook on the challenges and future prospects of HCFs.

  12. Synthesis, functionalisation and characterisation of mesoporous materials and sol-gel glasses for applications in catalysis, adsorption and photonics. (United States)

    Øye, Gisle; Glomm, Wilhelm R; Vrålstad, Torbjørn; Volden, Sondre; Magnusson, Heléne; Stöcker, Michael; Sjöblom, Johan


    In this review, synthesis and functionalisation approaches for ordered mesoporous materials and sol-gel glasses are described. Catalytic and adsorption applications are emphasised for the ordered mesoporous materials, while optical applications are the focus for sol-gel glasses.

  13. Synthesis, Properties and Mineralogy of Important Inorganic Materials

    CERN Document Server

    Warner, Terence E


    Intended as a textbook for courses involving preparative solid-state chemistry, this book offers clear and detailed descriptions on how to prepare a selection of inorganic materials that exhibit important optical, magnetic and electrical properties, on a laboratory scale. The text covers a wide range of preparative methods and can be read as separate, independent chapters or as a unified coherent body of work. Discussions of various chemical systems reveal how the properties of a material can often be influenced by modifications to the preparative procedure, and vice versa. References to miner

  14. Production of advanced materials by methods of self-propagating high-temperature synthesis

    CERN Document Server

    Tavadze, Giorgi F


    This translation from the original Russian book outlines the production of a variety of materials by methods of self-propagating high-temperature synthesis (SHS). The types of materials discussed include: hard, refractory, corrosion and wear-resistant materials, as well as other advanced and speciality materials. The authors address the issue of optimal parameters for SHS reactions occurring during processes involving a preliminary metallothermic reduction stage, and they calculate this using thermodynamic approaches. In order to confirm the effectiveness of this approach, the authors describe experiments focussing on the synthesis of elemental crysalline boron, boron carbides and nitrides. Other parts of this brief include theoretical and experimental results on single-stage production of hard alloys on the basis of titanium and zirconium borides, as well as macrokinetics of degassing and compaciton of SHS-products.This brief is suitable for academics, as well as those working in industrial manufacturing com...

  15. S-(+)-Carvone as starting material in the enantioselective synthesis of natural products

    NARCIS (Netherlands)

    Verstegen - Haaksma, A.A.


    In this thesis the applicability of S-(+)-carvone as chiral starting material in the synthesis of biologically active compounds is examined. S-(+)-carvone is the major compound of caraway essential oil. The essential oil content of caraway seed may vary from 2-7% and it contains about

  16. (+)-Aromadendrene as chiral starting material for the synthesis of fragrances and pheromones

    NARCIS (Netherlands)

    Lamers, Y.M.A.W.


    (+)-Aromadendrene ( 1 ) is a sesquiterpene present in the distillation tail of the oil of Eucalyptus globulus . This distillation tail is commercially available in large quantities at low price and is an interesting starting material for the synthesis of other chiral products. A

  17. Exploration of the role of anions in the synthesis of Cr containing mesoporous materials at room temperature

    NARCIS (Netherlands)

    Mahony, L; Wu, C.M.; Kibombo, H.S.; Thiruppathi, E.; Baltrusaitis, Jonas; Rasalingam, S; Koodali, R.T.


    Chromium containing mesoporous silica materials were synthesized via a modified Stöber synthesis at room temperature. The chromium ion loading and the effect of counter ion in the synthesis were studied in detail. The mesoporous materials were extensively characterized by powder X-ray diffraction

  18. Synthesis and characterization of super-microporous material with ...

    Indian Academy of Sciences (India)

    Super-microporouos silicon material with high hydrothermal stability denoted as MCM-41-T has been prepared from mesoporous MCM-41 by high temperature treatment. The structural and chemical property of MCM-41-T has been characterized by X-ray diffraction, transmission electron microscopy, N2 ...

  19. Combustion and Plasma Synthesis of High Temperature Materials (United States)


    cc 0v Table 4. Characteristics of Some Refractory Materials Dolomite and Magnesite-Based Characteristics Dolomite - Magnesite- Based Based...Other routes also exist such as calcination of organo-metallic compounds with a nitriding agent. Recently, thermal plasma processes have been used for

  20. Synthesis of Zeolites from Bolivian Raw Materials for Catalysis and Detergency Applications


    Garcia, Gustavo [UNESP


    Zeolites are very useful in many technological applications such as catalysis, separation and purification of gases and solvents, ion-exchange, etc. The production of zeolites is nowadays carried out with a variety of reagents, such starting materials render large scale production of zeolites expensive. Hence alternative synthesis routes for zeolite production at a lower cost are currently under investigation. One of these routes involves the use of natural aluminosilicate raw materials which...

  1. Synthesis of Hafnium-Based Ceramic Materials for Ultra-High Temperature Aerospace Applications (United States)

    Johnson, Sylvia; Feldman, Jay


    This project involved the synthesis of hafnium (Hf)-based ceramic powders and Hf-based precursor solutions that were suitable for preparation of Hf-based ceramics. The Hf-based ceramic materials of interest in this project were hafnium carbide (with nominal composition HE) and hafnium dioxide (HfO2). The materials were prepared at Georgia Institute of Technology and then supplied to research collaborators Dr. Sylvia Johnson and Dr. Jay Feldman) at NASA Ames Research Center.

  2. Synthesis, characterization and thermal properties of polymers based composites materials for High Power Electronic Packaging Applications


    Spitaleri, Fabiola


    As devices evolve, it s necessary that also interconnections and all hardware circuits evolve, including packaging. Nowadays are required significant improvement in packaging properties: low resistance interconnections, less noise, less parasitic oscillations, increased reliability and improved thermal behaviour. For these purpose has designed a research activity for the synthesis of new composites materials capable to dissipating heat better in relation to the current ones. These material...

  3. Synthesis and Thermodynamic Studies of Physisorptive Energy Storage Materials (United States)

    Stadie, Nicholas

    Physical adsorption of hydrogen or other chemical fuels on the surface of carbonaceous materials offers a promising avenue for energy storage applications. The addition of a well-chosen sorbent material to a compressed gas tank increases the volumetric energy density of the system while still permitting fast refueling, simplicity of design, complete reversibility, high cyclability, and low overall cost of materials. While physical adsorption is most effective at temperatures below ambient, effective storage technologies are possible at room temperature and modestly high pressure. A volumetric Sieverts apparatus was designed, constructed, and commissioned to accurately measure adsorption uptake at high pressures and an appropriate thermodynamic treatment of the experimental data is presented. In Chapter 1, the problem of energy storage is introduced in the context of hydrogen as an ideal alternative fuel for future mobile vehicle applications, and with methane in mind as a near-term solution. The theory of physical adsorption that is relevant to this work is covered in Chapter 2. In-depth studies of two classes of materials are presented in the final chapters. Chapter 3 presents a study of the dissociative "hydrogen spillover" effect in the context of its viability as a practical hydrogen storage solution at room temperature. Chapters 4-5 deal with zeolite-templated carbon, an extremely high surface-area material which shows promise for hydrogen and methane storage applications. Studies of hydrogen adsorption at high pressure (Chapter 4) and anomalous thermodynamic properties of methane adsorption (Chapter 5) on ZTCs are presented. The concluding chapter discusses the impact of and possible future directions for this work.

  4. Synthesis of Two-Dimensional Materials for Capacitive Energy Storage. (United States)

    Mendoza-Sánchez, Beatriz; Gogotsi, Yury


    The unique properties and great variety of two-dimensional (2D) nanomaterials make them highly attractive for energy storage applications. Here, an insight into the progress made towards the application of 2D nanomaterials for capacitive energy storage is provided. Synthesis methods, and electrochemical performance of various classes of 2D nanomaterials, particularly based on graphene, transition metal oxides, dichalcogenides, and carbides, are presented. The factors that directly influence capacitive performance are discussed throughout the text and include nanosheet composition, morphology and texture, electrode architecture, and device configuration. Recent progress in the fabrication of 2D-nanomaterials-based microsupercapacitors and flexible and free-standing supercapacitors is presented. The main electrode manufacturing techniques with emphasis on scalability and cost-effectiveness are discussed, and include laser scribing, printing, and roll-to-roll manufacture. Various issues that prevent the use of the full energy-storage potential of 2D nanomaterials and how they have been tackled are discussed, and include nanosheet aggregation and the low electrical conductivity of some 2D nanomaterials. Particularly, the design of hybrid and hierarchical 2D and 3D structures based on 2D nanomaterials is presented. Other challenges and opportunities are discussed and include: control of nanosheets size and thickness, chemical and electrochemical instability, and scale-up of electrode films. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Simulation, design and proof-of-concept of a two-stage continuous hydrothermal flow synthesis reactor for synthesis of functionalized nano-sized inorganic composite materials

    DEFF Research Database (Denmark)

    Zielke, Philipp; Xu, Yu; Simonsen, Søren Bredmose


    Computational fluid dynamics simulations were employed to evaluate several mixer geometries for a novel two-stage continuous hydrothermal flow synthesis reactor. The addition of a second stage holds the promise of allowing the synthesis of functionalized nano-materials as for example core...

  6. Hydrothermal synthesis and characterization of the semiconductor material Cu2ZnTiS4 (United States)

    Pérez Bustos, H. G.; Patarroyo-Mesa, M.; Gómez-Cuaspud, J. A.; Pineda-Triana, Y.; Vera-López, E.


    This paper describes the results of the synthesis and characterization of a quaternary semiconductor based on Cu2ZnTiS4 (abbreviated CZTiS), using a hydrothermal technique. The results confirm that time (24, 48 and 72 hours) and temperature (250, 275, and 300°C) factors, used in synthesis process, regulate different levels of electrical conductivity in these materials. The results of ultraviolet spectroscopy (UV) analysis, confirm the production of semiconductor solids with Band-gap values around 1.4eV, being coherent with a strong absorption in the ultraviolet region. The X-Ray Diffraction analysis (XRD), confirm that there is an opposite and proportional relationship between the crystal sizes, the reaction times and the synthesis temperature. In all cases, the particle sizes were 50-100nm. The results derived from Scanning Electron Microscopy (SEM), confirm the obtaining of homogenous materials with optimal morphological properties in accordance with synthesis method. Similarly, the composition values derived from the Energy-Dispersion X-ray Spectroscopy analysis (EDS), shown that obtained compositions are in agree with expected values. Finally, the results of electric characterization, confirm that used synthesis parameters show a strong dependence on the conductive behaviour of solids being the most relevant result the shown by the solid obtained at 300°C and 72 hours of reaction in accordance with preliminary works.

  7. Application of a Diffusion-denuder Method for the Investigation of the Effects of ‘Smoke pH’ on Vapor-phase Nicotine Yields from Different Types of Cigarettes

    Directory of Open Access Journals (Sweden)

    Cochran EW


    Full Text Available The potential effects of smoke pH on vapor-phase nicotine, or unprotonated nicotine, were investigated using a diffusion denuder method selected for its ability to quantitatively monitor vapor-phase nicotine in the presence of smoke particulate. For the purpose of this paper, the pH of the water-soluble fraction of mainstream cigarette smoke will be referred to as ‘smoke pH'. In this study, samples with different construction parameters affecting smoke pH were analyzed for percent vapor-phase nicotine. The smoke pH values ranged from 5.87 to 7.79. Percent initial vapor-phase nicotine values ranged from 0.4% to 1.5%. The range of the vapor-phase nicotine values for this study was (a independent of smoke pH and (b potentially dependent upon cigarette construction. In a second experiment, cigarettes with the same construction were used to repeat the analysis, thus eliminating construction as a variable. The tobacco was treated with varying levels of urea to give a range in smoke pH from 6.47 to 7.15. The determined initial vapor-phase nicotine values ranged from 0.4% to 2.1% of the total mainstream smoke nicotine. This variation was independent of smoke pH. It was determined in this study that (a the maximum initial vapor-phase nicotine delivered to mainstream smoke was 2.1% of the total nicotine delivered for our cigarette samples and (b the delivery of the unprotonated nicotine to mainstream smoke was not meaningfully affected by changes in smoke pH within the range studied.


    Energy Technology Data Exchange (ETDEWEB)

    Miller, Joel S. [Univ. of Utah, Salt Lake City, UT (United States)


    We have synthesized and characterized several families of organic-based magnets, a new area showing that organic species can exhibit the technologically important property of magnetic ordering. Thin film magnets with ordering temperatures exceeding room temperature have been exceeded. Hence, organic-based magnets represent a new class of materials that exhibit magnetic ordering and do not require energy-intensive metallurgical processing and are based upon Earth-abundant elements.

  9. Fast Reacting Nano Composite Energetic Materials: Synthesis and Combustion Characterization (United States)


    Office P.O. Box 12211 Research Triangle Park, NC 27709-2211 aluminum combustion; energetic materials; fluorine ; reaction kinetics; fluoropolymers; self...techniques will be examined to quantify combustion performance. All of this information will provide a basis for future research and applications involving... fluorine content in the acids and their structural differences contribute to difference in burn velocity. The mechanisms controlling reactivity will be

  10. Synthesis of Microporous Materials and Their VSC Adsorption Properties (United States)

    Yokogawa, Y.; Morikawa, H.; Sakanishi, M.; Utaka, H.; Nakamura, A.; Kishida, I.


    Oral malodor is caused by volatile sulfur compounds (VSC) such as hydrogen sulfide (H2S), methyl mercaptan and dimethyl sulfide produced in mouth. VSC induces permeability of mucous membrane and oral malodor formation. Thus, the adsorbent which highly adsorbs VSC should be useful for health in mouth and may prevent teeth from decaying. The microporous material, hydrotalcite, was synthesized by a wet method, and the H2S adsorption was studied. The samples, identified by powder X-ray diffraction method, were put into glass flask filled with H2S gas. The initial concentration of H2S was 30 ppm. The change in concentrations of H2S was measured at rt, and the amount of H2S absorbed on the hydrotalcite for 24 h was 300 micro L/g. The samples were taken out from the above glass flask and put into a pyrolysis plant attached to gas chromatography-mass spectrometry to determine the amount of H2S desorbed from samples. Only 3 % of H2S was desorbed when heated at 500 °C. H2S in water was also found to adsorb into hydrotalcite, which was confirmed by the headspace gas chromatography with flame photometric detector. The hydrotalcite material should be expected to be an adsorbent material, useful for health in mouth.

  11. Synthesis of Nano-Crystalline Gamma-TiAl Materials (United States)

    Hales, Stephen J.; Vasquez, Peter


    One of the principal problems with nano-crystalline materials is producing them in quantities and sizes large enough for valid mechanical property evaluation. The purpose of this study was to explore an innovative method for producing nano-crystalline gamma-TiAl bulk materials using high energy ball milling and brief secondary processes. Nano-crystalline powder feedstock was produced using a Fritsch P4(TM) vario-planetary ball mill recently installed at NASA-LaRC. The high energy ball milling process employed tungsten carbide tooling (vials and balls) and no process control agents to minimize contamination. In a collaborative effort, two approaches were investigated, namely mechanical alloying of elemental powders and attrition milling of pre-alloyed powders. The objective was to subsequently use RF plasma spray deposition and short cycle vacuum hot pressing in order to effect consolidation while retaining nano-crystalline structure in bulk material. Results and discussion of the work performed to date are presented.

  12. PDMS based microfluidic chips and their application in material synthesis (United States)

    Gong, Xiuqing

    Microfluidics is a highly interdisciplinary science which is to deal with the behavior, control and manipulation of fluids that are constrained to sub-milimeter scale. It incorporates the knowledge and technique intersecting physics, chemistry, mechanics, nanoscience and biotechnology, with practical applications to the design of systems in which small volumes of fluids will be used. In this thesis, we started our research from GER fluid synthesis which then is applied to designing different functions of microfluidic devices, valve, pump, and mixer. We built a way to correlate mechanical signal with electric signal by soft matter. The mechanical devices based GER fluid had good operating stability and mechanical performance. We studied how to improve the performance of GER fluid by increasing the yield stress while avoiding the sendimentation of nanoparticles in GER suspension. The meaning of this work is to enhance the stability and mechanical strength of GER fluid when it is applyed to the microfluidc channels. We tried different oils and studied the particle size for the GER effect. The largest yield stress which amounts to 300 kPa is achievable compared to previous GER fluid with 100 kPa. Microfluidic reactor, directing the flow of microliter volumes along microscale channels, offers the advantages of precise control of reagent loading, fast mixing and an enhanced reaction rate, cessation of the reaction at specific stages, and more. Basically, there are two microfluidic flow regimes, continuous flow and segmented flow (suspended droplets, channel-spanning slug, and wall-wetting films). Both flow regimes offer chemical reaction applications, e.g., continuous flow formation of polymer nanospheres and inorganic nanoparticles, size- and shape-control synthesis by segmented flow, and precipitate-forming reactions in droplets, wherein the segmented flow has gained more popularity in that area. The compartmentalization of segmented flow offers advantages to chemical

  13. Effect of the Ammonia Flow on the Formation of Microstructure Defects in GaN Layers Grown by High-Temperature Vapor Phase Epitaxy (United States)

    Barchuk, M.; Lukin, G.; Zimmermann, F.; Röder, C.; Motylenko, M.; Pätzold, O.; Heitmann, J.; Kortus, J.; Rafaja, D.


    High-temperature vapor phase epitaxy (HTVPE) is a physical vapor transport technology for a deposition of gallium nitride (GaN) layers. However, little is known about the influence of the deposition parameters on the microstructure of the layers. In order to fill this gap, the influence of the ammonia (NH3) flow applied during the HTVPE growth on the microstructure of the deposited GaN layers is investigated in this work. Although the HTVPE technology is intended to grow GaN layers on foreign substrates, the GaN layers under study were grown on GaN templates produced by metal organic vapor phase epitaxy in order to be able to separate the growth defects from the defects induced by the lattice misfit between the foreign substrate and the GaN layer. The microstructure of the layers is characterized by means of high-resolution x-ray diffraction (XRD), transmission electron microscopy and photoluminescence. In samples deposited at low ammonia flow, planar defects were detected, along which the nitrogen atoms are found to be substituted by impurity atoms. The interplay between these planar defects and the threading dislocations is discussed. A combination of XRD and micro-Raman spectroscopy reveals the presence of compressive residual stress in the samples.

  14. The synthesis and properties of nanoscale ionic materials

    KAUST Repository

    Rodriguez, Robert Salgado


    In this article we discuss the effect of constituents on structure, flow, and thermal properties of nanoscale ionic materials (NIMs). NIMs are a new class of nanohybrids consisting of a nanometer-sized core, a charged corona covalently attached to the core, and an oppositely charged canopy. The hybrid nature of NIMs allows for their properties to be engineered by selectively varying their components. The unique properties associated with these systems can help overcome some of the issues facing the implementation of nanohybrids to various commercial applications, including carbon dioxide capture,water desalinization and as lubricants. Copyright © 2010 John Wiley & Sons, Ltd.

  15. The Synthesis, Characterization and Catalytic Reaction Studies of Monodisperse Platinum Nanoparticles in Mesoporous Oxide Materials

    Energy Technology Data Exchange (ETDEWEB)

    Rioux, Robert M. [Univ. of California, Berkeley, CA (United States)


    A catalyst design program was implemented in which Pt nanoparticles, either of monodisperse size and/or shape were synthesized, characterized and studied in a number of hydrocarbon conversion reactions. The novel preparation of these materials enables exquisite control over their physical and chemical properties that could be controlled (and therefore rationally tuned) during synthesis. The ability to synthesize rather than prepare catalysts followed by thorough characterization enable accurate structure-function relationships to be elucidated. This thesis emphasizes all three aspects of catalyst design: synthesis, characterization and reactivity studies. The precise control of metal nanoparticle size, surface structure and composition may enable the development of highly active and selective heterogeneous catalysts.

  16. New fullerene-based mixed materials: Synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    McBranch, D.; Kohlman, R.; Klimov, V.; Grigorova, M.; Shi, X.; Smilowitz, L.; Mattes, B.R. [Los Alamos National Lab., NM (US); Wang, H.; Wudl, F. [Univ. of California, Santa Barbara, CA (US)


    This is the final report of a three-year, Laboratory Directed Research and Development (LDRD) project at the Los Alamos National Laboratory (LANL). The authors present results of broadband femtosecond transient absorption and broadband nanosecond optical limiting studies of C{sub 60} and derivatized C{sub 60}. They have investigated both solutions and solid-state mixed materials (sol-gel glass hosts doped with fullerene guests). They show that derivatized fullerenes provide enhanced solubility and processability, with a ground-state absorption extended into the infrared compared with C{sub 60}. They have extensively studied both the dynamic optical response and the excited-state absorption cross sections of solutions and solids for multiple wavelengths in the visible to near infrared. Wavelength-dependent studies show that the optical limiting response improves monotonically at longer wavelengths, demonstrating broadband limiting in all 6,6 mono-adducts and neat C{sub 60}. The authors report new approaches to processing sol-gel glass/fullerene composites to improve the optical limiting performance of solid-state materials to approach the response of solution limiters.

  17. Effect of growth conditions on the Al composition and optical properties of Al x Ga 1−x N layers grown by atmospheric-pressure metal organic vapor phase epitaxy

    KAUST Repository

    Soltani, S.


    The effect of growth conditions on the Al composition and optical properties of AlxGa1-xN layers grown by atmospheric-pressure metal organic vapor phase epitaxy is investigated. The Al content of the samples is varied between 3.0% and 9.3% by changing the gas flow rate of either trimethylaluminum (TMA) or trimethylgallium (TMG) while other growth parameters are kept constant. The optical properties of the AlxGa1-xN layers are studied by photoreflectance and time-resolved photoluminescence (TR-PL) spectroscopies. A degeneration in the material quality of the samples is revealed when the Al content is increased by increasing the TMA flow rate. When the TMG flow rate is decreased with a fixed TMA flow rate, the Al content of the AlxGa1-xN layers is increased and, furthermore, an improvement in the optical properties corresponding with an increase in the PL decay time is observed. (C) 2017 Elsevier B.V. All rights reserved.

  18. Synthesis and chemical modification of carbon nanostructures for materials applications (United States)

    Higginbotham, Amanda Lynn

    This dissertation explores the structure, chemical reactivities, electromagnetic response, and materials properties of various carbon nanostructures, including single-walled carbon nanotubes (SWCNTs), multi-walled carbon nanotubes (MWCNTs), graphite, and graphene nanoribbons (GNRs). Efficient production and modification of these unique structures, each with their own distinct properties, will make them more accessible for applications in electronics, materials, and biology. A method is reported for controlling the permittivity from 1--1000 MHz of SWCNT-polymer composites (0.5 wt%) for radio frequency applications including passive RF antenna structures and EMI shielding. The magnitude of the real permittivity varied between 20 and 3.3, decreasing as higher fractions of functionalized-SWCNTs were added. The microwave absorbing properties and subsequent heating of carbon nanotubes were used to rapidly cure ceramic composites. With less than 1 wt% carbon nanotube additives and 30--40 W of directed microwave power (2.45 GHz), bulk composite samples reached temperatures above 500°C within 1 min. Graphite oxide (GO) polymer nanocomposites were developed at 1, 5, and 10 wt% for the purpose of evaluating the flammability reduction and materials properties of the resulting systems. Microscale oxygen consumption calorimetry revealed that addition of GO reduced the total heat release in all systems, and GO-polycarbonate composites demonstrated very fast self-extinguishing times in vertical open flame tests. A simple solution-based oxidative process using potassium permanganate in sulfuric acid was developed for producing nearly 100% yield of graphene nanoribbons (GNRs) by lengthwise cutting and unraveling of MWCNT sidewalls. Subsequent chemical reduction of the GNRs resulted in restoration of electrical conductivity. The GNR synthetic conditions were investigated in further depth, and an improved method which utilized a two-acid reaction medium was found to produce GNRs with

  19. Synthesis and Characterization of Novel Nonlinear Optical Materials (United States)

    Liang, Cheryl Shuang


    Nonlinear optic materials are becoming increasingly important because of their many technological applications, such as second harmonic generation (SHG), optical switching, and waveguides for optical transmission. Currently, there is a demand for crystals transparent in the UV region, which would make the third and higher harmonic generations feasible. Compounds with the general stoichiometry ABCO _4 structural systems have shown to be promising candidates for frequency doubling into the UV region. The stuffed tridymite structure in which these ABCO_4 compounds crystallize is very tolerant to substitution, and over two hundred compounds have been synthesized up to date. While the presently available theories of optical nonlinearity have been applied to many inorganic solids, the threatened structure theory applied for ferroelectric properties can also be used to describe the structure/property relationship in the ABCO_4 structural family. Compounds synthesized for this study, ALiPO_4 (A = Sr, Ba, Pb) have shown that the SHG of these materials can be maximized by bringing each system close to its structural phase transition or by inducing stress in the pure phase structure. Studies have shown that the dielectric coefficients of KNbO_3 increase by more than tenfold with tantalum doping. This prompted the investigation of a mixed niobium/tantalum containing channelled tetrahedra/octahedra open framework, K_{2/3}Li _{1/3}Nb_ {rm 2-x}Ta_{ rm x}PO_8. These compounds are capable of ion exchange, where other cations are used to replace potassium. The cation-framework interaction mimics the guest-host relationship characteristic of many traditional zeolitic materials. This interaction also enables us to determine the role of the cation in framework polarizability, which can be measured by SHG intensities. Through ion exchange, many isostructural compounds can be made at low temperatures. A family of layered rubidium niobium/tantalum oxide compounds have been synthesized in

  20. The DOE Center of Excellence for the Synthesis and Processing of Advanced Materials: Research briefs

    Energy Technology Data Exchange (ETDEWEB)



    This publication is designed to inform present and potential customers and partners of the DOE Center of Excellence for the Synthesis and Processing of Advanced Materials about significant advances resulting from Center-coordinated research. The format is an easy-to-read, not highly technical, concise presentation of the accomplishments. Selected accomplishments from each of the Center`s seven initial focused projects are presented. The seven projects are: (1) conventional and superplastic forming; (2) materials joining; (3) nanoscale materials for energy applications; (4) microstructural engineering with polymers; (5) tailored microstructures in hard magnets; (6) processing for surface hardness; and (7) mechanically reliable surface oxides for high-temperature corrosion resistance.

  1. Combinatorial microfluidic droplet engineering for biomimetic material synthesis (United States)

    Bawazer, Lukmaan A.; McNally, Ciara S.; Empson, Christopher J.; Marchant, William J.; Comyn, Tim P.; Niu, Xize; Cho, Soongwon; McPherson, Michael J.; Binks, Bernard P.; deMello, Andrew; Meldrum, Fiona C.


    Although droplet-based systems are used in a wide range of technologies, opportunities for systematically customizing their interface chemistries remain relatively unexplored. This article describes a new microfluidic strategy for rapidly tailoring emulsion droplet compositions and properties. The approach uses a simple platform for screening arrays of droplet-based microfluidic devices and couples this with combinatorial selection of the droplet compositions. Through the application of genetic algorithms over multiple screening rounds, droplets with target properties can be rapidly generated. The potential of this method is demonstrated by creating droplets with enhanced stability, where this is achieved by selecting carrier fluid chemistries that promote titanium dioxide formation at the droplet interfaces. The interface is a mixture of amorphous and crystalline phases, and the resulting composite droplets are biocompatible, supporting in vitro protein expression in their interiors. This general strategy will find widespread application in advancing emulsion properties for use in chemistry, biology, materials, and medicine. PMID:27730209

  2. Nanostructured carbon materials decorated with organophosphorus moieties: synthesis and application

    Directory of Open Access Journals (Sweden)

    Giacomo Biagiotti


    Full Text Available A new synthetic approach for the production of carbon nanomaterials (CNM decorated with organophosphorus moieties is presented. Three different triphenylphosphine oxide (TPPO derivatives were used to decorate oxidized multiwalled carbon nanotubes (ox-MWCNTs and graphene platelets (GPs. The TPPOs chosen bear functional groups able to react with the CNMs by Tour reaction (an amino group, nitrene cycloaddition (an azido group or CuAAC reaction (one terminal C–C triple bond. All the adducts were characterized by FTIR, Raman spectroscopy, TEM, XPS, elemental analysis and ICP-AES. The cycloaddition of nitrene provided the higher loading on ox-MWCNTs and GPs as well, while the Tour approach gave best results with nanotubes (CNTs. Finally, we investigated the possibility to reduce the TPPO functionalized CNMs to the corresponding phosphine derivatives and applied one of the materials produced as heterogeneous organocatalyst in a Staudinger ligation reaction.

  3. Theoretical Synthesis of Mixed Materials for CO2 Capture Applications

    Energy Technology Data Exchange (ETDEWEB)

    Duan, Yuhua


    These pages provide an example of the layout and style required for the preparation of four-page papers for the TechConnect World 2015 technical proceedings.Documents must be submitted in electronic (Adobe PDFfile) format. Please study the enclosed materials beforebeginning the final preparation of your paper. Proofread your paper carefully before submitting (it will appear in the published volume in exactly the same form). Your PDF manuscript must be uploaded online by April 11th, 2015.You will receive no proofs. Begin your paper with an abstract of no more than 18 lines. Thoroughly summarize your article in this section since this text will be used for on-line listing and classification of the publication.

  4. Synthesis of Titania-Silica Materials by Sol-Gel

    Directory of Open Access Journals (Sweden)

    Rubia F. S. Lenza


    Full Text Available In this work TiO2-SiO2 glasses containing as much as 20 mol % of TiO2 were prepared via sol-gel process using titanium and silicon alkoxides, in the presence of chlorine, in the form of titanium tetrachloride or HCl. The gels were heat-treated until 800 °C. X-ray diffraction and Fourier transform infrared spectroscopy were used to understand the structural properties of TiO2-SiO2 oxides calcined at different temperatures and to evaluate the homogeneity of these materials. The degree of the compactness of the silica network is inferred from the frequency of the asymmetric stretching vibrations of Si-O-Si bonds. Formation of Si-O-Ti bridges, as monitored by the intensity of characteristic 945 cm-1 ¾ 960 cm-1 vibration, is particularly prominent if the method of basic two-step prehydrolysis of silicon alkoxide, addition of titanium alkoxide and completion of hydrolysis was used.

  5. Synthesis of polymer materials for use as cell culture substrates

    Energy Technology Data Exchange (ETDEWEB)

    Lakard, Sophie [Laboratoire de Chimie des Materiaux et Interfaces, University of Franche-Comte, IUT, 30 Avenue de l' Observatoire, 25009 Besancon (France)], E-mail:; Morrand-Villeneuve, Nadege [Laboratoire de Neurosciences, University of Franche-Comte, Place Leclerc, 25030 Besancon (France); Lesniewska, Eric [Laboratoire de Physique de l' Universite de Bourgogne, University of Bourgogne, 9 Avenue Savary, 21078 Dijon (France); Lakard, Boris [Laboratoire de Chimie des Materiaux et Interfaces, University of Franche-Comte, 16 Route de Gray, 25030 Besancon (France); Michel, Germaine [Laboratoire de Neurosciences, University of Franche-Comte, Place Leclerc, 25030 Besancon (France); Herlem, Guillaume [Laboratoire de Chimie des Materiaux et Interfaces, University of Franche-Comte, 16 Route de Gray, 25030 Besancon (France); Gharbi, Tijani [Laboratoire d' Optique P.M. Duffieux, University of Franche-Comte, 16 Route de Gray, 25030 Besancon (France); Fahys, Bernard [Laboratoire de Chimie des Materiaux et Interfaces, University of Franche-Comte, 16 Route de Gray, 25030 Besancon (France)


    Up to today, several techniques have been used to maintain cells in culture for studying many aspects of cell biology and physiology. More often, cell culture is dependent on proper anchorage of cells to the growth surface. Thus, poly-L-lysine, fibronectin or laminin are the most commonly used substrates. In this study, electrosynthesized biocompatible polymer films are proposed as an alternative to these standard substrates. The electrosynthesized polymers tested were polyethylenimine, polypropylenimine and polypyrrole. Then, the adhesion, proliferation and morphology of rat neuronal cell lines were investigated on these polymer substrates in an attempt to develop new and efficient polymer materials for cell culture. During their growth on the polymers, the evolution of the cell morphology was monitored using both confocal microscopy and immunohistochemistry, leading to the conclusion of a normal development. An estimation of the adhesion and proliferation rates of rat neuronal cell cultures indicated that polyethylenimine and polypropylenimine were the best substrates for culturing olfactory neuronal cells. A method to favour the differentiation of the neuronal cells was also developed since the final aim of this work is to develop a biosensor for odour detection using differentiated neuronal cells as transducers. Consequently, a biosensor was microfabricated using silicon technology. This microsystem allowed us to culture the cells on a silicon wafer and to position the cells on certain parts of the silicon wafer.

  6. Multifunctional upconversion-magnetic hybrid nanostructured materials: synthesis and bioapplications. (United States)

    Li, Xiaomin; Zhao, Dongyuan; Zhang, Fan


    The combination of nanotechnology and biology has developed into an emerging research area: nano-biotechnology. Upconversion nanoparticles (UCNPs) have attracted a great deal of attention in bioapplications due to their high chemical stability, low toxicity, and high signal-to-noise ratio. Magnetic nanoparticles (MNPs) are also well-established nanomaterials that offer controlled size, ability to be manipulated externally, and enhancement of contrast in magnetic resonance imaging (MRI). As a result, these nanoparticles could have many applications in biology and medicine, including protein purification, drug delivery, and medical imaging. Because of the potential benefits of multimodal functionality in biomedical applications, researchers would like to design and fabricate multifunctional upconversion-magnetic hybrid nanostructured materials. The hybrid nanostructures, which combine UCNPs with MNPs, exhibit upconversion fluorescence alongside superparamagnetism property. Such structures could provide a platform for enhanced bioimaging and controlled drug delivery. We expect that the combination of unique structural characteristics and integrated functions of multifunctional upconversion-magnetic nanoparticles will attract increasing research interest and could lead to new opportunities in nano-bioapplications.

  7. Synthesis and characterization of luminescent materials for thermal sensing and proton dosimetry (United States)

    Doull, Brandon Arthur

    The work presented in this thesis is the materials synthesis, investigation of synthesis parameters, and basic luminescent characterizations of MgB 4O7, Li2B4O7, and MgO for the applications of thermal sensing using thermoluminescence (TL) and proton dosimetry using optically stimulated luminescence (OSL). The materials were synthesized using solution combustion synthesis and characterized by x-ray diffraction, radioluminescence, thermoluminescence, and optically stimulated luminescence. Based upon the basic characterizations MgB 4O7:Li,Dy and Li2B4O7:Cu,Ag were selected for their potential for use as TL materials for thermal sensing while MgB4O7:Li,Ce and MgO:Li were chosen for use as OSL materials in proton dosimetry. Furthermore, MgB4O7:Li,Ce and MgO:Li were fabricated into detector assemblies and exposed to a clinical proton beam for analysis.

  8. Plasma-Assisted Synthesis and Surface Modification of Electrode Materials for Renewable Energy. (United States)

    Dou, Shuo; Tao, Li; Wang, Ruilun; El Hankari, Samir; Chen, Ru; Wang, Shuangyin


    Renewable energy technology has been considered as a "MUST" option to lower the use of fossil fuels for industry and daily life. Designing critical and sophisticated materials is of great importance in order to realize high-performance energy technology. Typically, efficient synthesis and soft surface modification of nanomaterials are important for energy technology. Therefore, there are increasing demands on the rational design of efficient electrocatalysts or electrode materials, which are the key for scalable and practical electrochemical energy devices. Nevertheless, the development of versatile and cheap strategies is one of the main challenges to achieve the aforementioned goals. Accordingly, plasma technology has recently appeared as an extremely promising alternative for the synthesis and surface modification of nanomaterials for electrochemical devices. Here, the recent progress on the development of nonthermal plasma technology is highlighted for the synthesis and surface modification of advanced electrode materials for renewable energy technology including electrocatalysts for fuel cells, water splitting, metal-air batteries, and electrode materials for batteries and supercapacitors, etc. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Nickel hydroxides and related materials: a review of their structures, synthesis and properties (United States)

    Hall, David S.; Lockwood, David J.; Bock, Christina; MacDougall, Barry R.


    This review article summarizes the last few decades of research on nickel hydroxide, an important material in physics and chemistry, that has many applications in engineering including, significantly, batteries. First, the structures of the two known polymorphs, denoted as α-Ni(OH)2 and β-Ni(OH)2, are described. The various types of disorder, which are frequently present in nickel hydroxide materials, are discussed including hydration, stacking fault disorder, mechanical stresses and the incorporation of ionic impurities. Several related materials are discussed, including intercalated α-derivatives and basic nickel salts. Next, a number of methods to prepare, or synthesize, nickel hydroxides are summarized, including chemical precipitation, electrochemical precipitation, sol–gel synthesis, chemical ageing, hydrothermal and solvothermal synthesis, electrochemical oxidation, microwave-assisted synthesis, and sonochemical methods. Finally, the known physical properties of the nickel hydroxides are reviewed, including their magnetic, vibrational, optical, electrical and mechanical properties. The last section in this paper is intended to serve as a summary of both the potentially useful properties of these materials and the methods for the identification and characterization of ‘unknown’ nickel hydroxide-based samples. PMID:25663812

  10. Synthesis of Inorganic-Organic Hybrid Materials Designed for Radiation Detection, Luminescence, and Gas Storage (United States)

    Vaughn, Shae Anne

    Materials discovery is the driving force behind the research presented herein. Basic research has been conducted in order to obtain a better understanding of coordination chemistry and structural outcomes, particularly within the area of trivalent lanthanides. Discovering new materials is one route to further advancement of technology; another one is the focus on incremental changes to already existing materials. Often the building blocks of a compound are chosen in an effort to synthesize a material that makes use of the properties of each individual component and may result in a better, more robust, applicable material. The combination of organic and inorganic components for the synthesis of novel materials with potential applications such as scintillation photoluminescence, catalysis, and gas storage are the focus of the research presented herein. The first part focuses on lanthanide organic hybrid materials, where the synthesis of a new family of potential scintillating materials was undertaken and yielded improved understanding of the control that can be achieved over the topological structure of these materials by controlling the coordinating crystallization solvents. This research has led to the synthesis of an array of unique motifs, ranging from dimeric complexes, tetrameric complexes, to 1-D chains, and most intriguing of all, catenated tetradecanuclear rings. These rings represent the largest lanthanide rings synthesized to date, the next largest multinuclear rings, until now, were dodecanuclear complexes of alkoxides. From a basic research standpoint this is an exciting new development in lanthanide coordination chemistry and illustrates the importance of steric effects upon a system. These complexes are potential scintillators, supported by their luminescence and measurements of similar compounds that demonstrate surprising scintillation efficiencies. In the second part, other hybrid materials that have also been prepared are discussed, including the

  11. Synthesis, structure and properties of hierarchical nanostructured porous materials studied by molecular dynamics simulations (United States)

    Chae, Kisung

    For applications of porous materials in many fields of technological importance, such as catalysis, filtration, separation, energy storage and conversion, the efficiency is often limited by chemical kinetics, and/or diffusion of reactants and products to and from the active sites. Hierarchical nanostructured porous materials (HNPMs) that possess both mesopores (2 nm gas transport in HNPCs, a computationally efficient reflecting particle method (RPM) together with a perturbation-relaxation loop was developed in this work to make the pressure drop consistent for various structures and transport conditions. The mimetic nanocasting technique and the RPM method can be easily extended to study the synthesis-structure-transport properties relations in many other HNPMs. A complete feedback loop among synthesis, structure and properties will help identify the proper synthesis parameters to design the optimal porous structures for a particular application. This will speed up the applications of HNPMs in many fields, such as electrodes for supercapacitors, lithium ion batteries and fuel cells, catalyst supports, materials for gas sensing and hydrogen storage, etc.

  12. Synthesis and functional properties of nanostructured ceria materials; Synthese und funktionelle Eigenschaften nanostrukturierter Ceroxidmaterialien

    Energy Technology Data Exchange (ETDEWEB)

    Naumann, Meike


    Nanostructured ceria tubes have been synthesised using electro spun polymer fibers as templating material. These polymer mats are produced by electro spinning starting with a polymer solution. In a next step polymer fibers are decorated with cer containing sol, which is then dried. To receive ceria tubes the polymer is removed on the one hand by thermal decomposition of the polymer or on the other hand by oxygen plasma treatment of ceria/polymer hybrid material. The resulting ceria tubes have a specific surface area of 98 m2 g-1. TEM, XRD, SAED and Raman investigations show a fully nanostructured crystallinity with cubic fluorine type structure. This obtained material shows a photo catalytic activity within decomposition of methylene blue in the Vis part of the electromagnetic spectrum. This photo catalytic activity can be increased using doping ions of transition and rare earth elements that are introduced in the sol-gel synthesis. Also here XRD and TEM investigations show a fully nano crystalline structure of ceria. Raman spectroscopy verifies the doping of ceria by transition and rare earth elements up to 22% of doping. No phase separation can be observed. The photo catalytic activity can be increased using these doped materials. Additionally a catalytic activity of pure ceria and mixed ceria/zirconia materials have been investigated synthesis of dimethylcarboxilate without water addition. Here a direct dependence between turn over and doping cannot be detected. The dependence can be deduced to the synthesis process of the catalyst. Terminal sensoric properties of doped and undoped ceria (n-type semiconductor) are investigated. The prepared materials are used as chemiresistors against oxygen at temperatures of 700 C. These investigations show a reversible increase of the electrical resistance against oxygen.

  13. Simplified Application of Material Efficiency Green Metrics to Synthesis Plans: Pedagogical Case Studies Selected from "Organic Syntheses" (United States)

    Andraos, John


    This paper presents a simplified approach for the application of material efficiency metrics to linear and convergent synthesis plans encountered in organic synthesis courses. Computations are facilitated and automated using intuitively designed Microsoft Excel spreadsheets without invoking abstract mathematical formulas. The merits of this…

  14. Influence of the interface on growth rates in AlN/GaN short period superlattices via metal organic vapor phase epitaxy (United States)

    Rodak, L. E.; Korakakis, D.


    AlN/GaN short period superlattices are well suited for a number of applications including, but not limited to, digital alloys, intersubband devices, and emitters. In this work, AlN/GaN superlattices with periodicities ranging from 10 to 20 Å have been grown via metal organic vapor phase epitaxy in order to investigate the influence of the interface on the binary alloy growth rates. The GaN growth rate at the interface was observed to decrease with increasing GaN thickness while the AlN growth rate remained constant. This has been attributed to a decrease in the decomposition rate of GaN at the hetero-interface as seen in other III-V hetero-structures.

  15. Surfactant effects of indium on cracking in AlN/GaN distributed Bragg reflectors grown via metal organic vapor phase epitaxy (United States)

    Rodak, L. E.; Miller, C. M.; Korakakis, D.


    Aluminum Nitride (AlN) and Gallium Nitride (GaN) superlattice structures are often characterized by a network of cracks resulting from the large lattice mismatch and difference in thermal expansion coefficients, especially as the thickness of the layers increases. This work investigates the influence of indium as a surfactant on strain and cracking in AlN/GaN DBRs grown via Metal Organic Vapor Phase Epitaxy (MOVPE). DBRs with peak reflectivities ranging from 465 nm to 540 nm were grown and indium was introduced during the growth of the AlN layer. Image processing techniques were used to quantify the crack length per square millimeter and it was observed that indium has a significant effect on the crack formation and reduced the total crack length in these structures by a factor of two.

  16. Response of Aspergillus niger Inoculated on Tomatoes Exposed to Vapor Phase Mustard Essential Oil for Short or Long Periods and Sensory Evaluation of Treated Tomatoes

    Directory of Open Access Journals (Sweden)

    Ana Elena Aguilar-González


    Full Text Available The inhibitory effect of mustard essential oil (EO in vapor phase against Aspergillus niger was evaluated in vitro and in vivo (in tomatoes. Mold response in tomatoes exposed for short or long periods to selected concentrations of mustard EO was also evaluated. Furthermore, a sensory evaluation was also performed among treated tomatoes and compared with nontreated ones. Minimum inhibitory concentration (MIC for the studied EO was determined by the inverted Petri dish method. MIC for the in vitro and in vivo tests for mustard EO was of 3.08 μL/Lair. In vitro and in vivo results demonstrate the effectiveness of vapors of mustard EO against A. niger. The studied EO contains highly volatile organic compounds with strong inhibitory effects, even when applied for short periods, and can consequently be considered a good alternative to traditional synthetic antimicrobials without detriment of selected sensory attributes.

  17. Structural and electrical properties of InAs/GaSb superlattices grown by metalorganic vapor phase epitaxy for midwavelength infrared detectors

    Energy Technology Data Exchange (ETDEWEB)

    Arikata, Suguru; Kyono, Takashi [Semiconductor Technologies Laboratory, Sumitomo Electric Industries, LTD., Hyogo (Japan); Miura, Kouhei; Balasekaran, Sundararajan; Inada, Hiroshi; Iguchi, Yasuhiro [Transmission Devices Laboratory, Sumitomo Electric Industries, LTD., Yokohama (Japan); Sakai, Michito [Sensor System Research Group, Japan Aerospace Exploration Agency (JAXA), Tsukuba, Ibaraki (Japan); Katayama, Haruyoshi [Space Technology Directorate I, Japan Aerospace Exploration Agency (JAXA), Tsukuba, Ibaraki (Japan); Kimata, Masafumi [College of Science and Engineering, Ritsumeikan University, Shiga (Japan); Akita, Katsushi [Sumiden Semiconductor Materials, LTD., Hyogo (Japan)


    InAs/GaSb superlattice (SL) structures were fabricated on GaSb substrates by metalorganic vapor phase epitaxy (MOVPE) toward midwavelength infrared (MWIR) photodiodes. Almost defect-free 200-period SLs with a strain-compensation interfacial layer were successfully fabricated and demonstrate an intense photoluminescence peak centered at 6.1 μm at 4 K and an external quantum efficiency of 31% at 3.5 μm at 20 K. These results indicate that the high-performance MWIR detectors can be fabricated in application with the InAs/GaSb SLs grown by MOVPE as an attractive method for production. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  18. Bulk GaN substrate with overall dislocation density on the order of 105/cm2 fabricated by hydride vapor phase epitaxy (United States)

    Goubara, Shin; Matsubara, Tohoru; Yukizane, Kota; Arita, Naoki; Fujimoto, Satoru; Ezaki, Tatsuya; Inomoto, Ryo; Yamane, Keisuke; Okada, Narihito; Tadatomo, Kazuyuki


    In this study, a combined facet and flattening (FF) growth technique was implemented to fabricate GaN substrates by hydride vapor phase epitaxy. By changing the growth conditions, i.e., the growth temperature and V/III ratio, it was found that facet growth was promoted with a high V/III ratio and low temperature and planar growth was promoted with low V/III ratios and high temperature. We introduce a FF growth technique involving further reduction of the dislocation density using facet growth as the first step and flattening growth of the GaN layer as the second step. To further reduce dislocation density, we also finally demonstrate a multiple-step growth technique based on FF growth and succeeded in producing GaN substrates with overall dislocation densities on the order of 105 cm-2.

  19. Cross-stacked carbon nanotubes assisted self-separation of free-standing GaN substrates by hydride vapor phase epitaxy (United States)

    Wei, Tongbo; Yang, Jiankun; Wei, Yang; Huo, Ziqiang; Ji, Xiaoli; Zhang, Yun; Wang, Junxi; Li, Jinmin; Fan, Shoushan


    We report a novel method to fabricate high quality 2-inch freestanding GaN substrate grown on cross-stacked carbon nanotubes (CSCNTs) coated sapphire by hydride vapor phase epitaxy (HVPE). As nanoscale masks, these CSCNTs can help weaken the interface connection and release the compressive stress by forming voids during fast coalescence and also block the propagation of threading dislocations (TDs). During the cool-down process, thermal stress-induced cracks are initiated at the CSCNTs interface with the help of air voids and propagated all over the films which leads to full self-separation of FS-GaN substrate. Raman and photoluminescence spectra further reveal the stress relief and crystalline improvement of GaN with CSCNTs. It is expected that the efficient, low cost and mass-producible technique may enable new applications for CNTs in nitride optoelectronic fields.

  20. Halide vapor phase epitaxy of thick GaN films on ScAlMgO4 substrates and their self-separation for fabricating freestanding wafers (United States)

    Ohnishi, Kazuki; Kanoh, Masaya; Tanikawa, Tomoyuki; Kuboya, Shigeyuki; Mukai, Takashi; Matsuoka, Takashi


    Halide vapor phase epitaxy of thick GaN films was demonstrated on ScAlMgO4 (SCAM) substrates, and their self-separation was achieved. The 320-µm-thick GaN film was self-separated from the SCAM substrate during the cooling process after the growth. This separation phenomenon occurred because of both the c-plane cleavability of SCAM and the difference in the thermal-expansion coefficients between GaN and SCAM. The dark-spot densities for the GaN films on the SCAM substrates were approximately 30% lower than those on sapphire substrates. These results indicate that SCAM substrates are promising for fabricating a high-quality freestanding GaN wafer at a low cost.

  1. Occurrence of cubic GaN and strain relaxation in GaN buffer layers grown by low-pressure metalorganic vapor phase epitaxy on (0001) sapphire substrates (United States)

    Cheng, Lisen; Zhou, Kuan; Zhang, Ze; Zhang, Guoyi; Yang, Zhijian; Tong, Yuzhen


    Investigations on GaN buffer layers grown by low-pressure metalorganic vapor phase epitaxy on (0001) sapphire substrates indicated that the mechanisms by way of which GaN buffer layers relax stresses introduced by the lattice mismatch and thermal expansion coefficient difference between GaN epilayer and sapphire substrate are related to both the crystallographic structure of GaN and thickness of the buffer layers. Beside forming misfit dislocations, mismatch-induced stresses can also be relaxed by forming stacking faults and microtwin boundaries parallel to (11-1) of GaN near the interface between GaN and sapphire substrate in cubic GaN buffer layers. It was found that, in cubic GaN buffer layers, there exists a critical thickness within which the stacking faults and/or microtwin boundaries parallel to (11-1) of GaN can be formed. This critical value is determined to be 50 nm.

  2. Synthesis of Chalcone and Flavanone Compound Using Raw Material of Acetophenone and Benzaldehyde Derivative

    Directory of Open Access Journals (Sweden)

    Ismiyarto Ismiyarto


    Full Text Available Synthesis of flavanoid compounds of chalcone and flavanone groups have been conducted. Flavanoid Is one of the group natural products which is mostly found in plants and have been proved to have physiological activity as drug. In this research, chalcone proup compounds that being synthesized are: chalcone, 3,4-dimethoxychalcone, 2'-hidroxy-3,4-dimethoxychalcone where as compound of flavanone group that being synthesized is 3',4'-dimethoxyflavanone. The synthesis of chalcone group are carried out based on Claisen-Schmidt reaction by using raw material of aromatic aldehydes and aromatic ketones. The synthesis in carried out by stirring at the room temperature using alkali solution as catalyst and ethanol as solvent. The synthesis of 3',4'-dimethoxyflanone is made based on the nucleophilic 1,4 addition of the unsaturated α,β ketone. The synthesis is made by refluxing 2'-hydroxy-3,4-dimethoxychalcone in alkali condition for 12 hours. The identification of flavanoid compound is carried out by using spectroscopic IR, GC-MS and 1H-NMR methods. The result of each synthesis chalcone group are follows: chalcone as yellowish solid with m.p= 50 °C and the yield is 83.39%; 3,4-dimethoxychalcone as yellow solid with m.p= 57°C and the yield is 76.00% ; 2'-hydroxy-3,4-dimethoxychalcone as orange solid with m.p= 90 °C and the yield is 74.29%, for 3',4'-dimethoxyflavanone as pale yellow solid with m.p= 80 °C and the yield is 72.00%.

  3. Synthesis, Characterization, and Modeling of Nanotube Materials with Variable Stiffness Tethers (United States)

    Frankland, S. J. V.; Herzog, M. N.; Odegard, G. M.; Gates, T. S.; Fay, C. C.


    Synthesis, mechanical testing, and modeling have been performed for carbon nanotube based materials. Tests using nanoindentation indicated a six-fold enhancement in the storage modulus when comparing the base material (no nanotubes) to the composite that contained 5.3 wt% of nanotubes. To understand how crosslinking the nanotubes may further alter the stiffness, a model of the system was constructed using nanotubes crosslinked with a variable stiffness tether (VST). The model predicted that for a composite with 5 wt% nanotubes at random orientations, crosslinked with the VST, the bulk Young's modulus was reduced by 30% compared to the noncrosslinked equivalent.

  4. Synthesis and Characterization of Fly Ash Geopolymer for Water Absorbent Material


    Anggarini Ufafa; Sukmana Ndaru Candra; Prasetya Fandi Angga


    Geopolymer as a water absorbent material has been synthesized from fly ash. This research aims to determine the ability of geopolymer to save water content with variations of NaOH molar ratio. In this research, the synthesis of geopolymer was conducted by setting NaOH molar ratio at 3, 4, 5, 6 and 7 M. The resulting material characterization was done by using XRD, FTIR and SEM in order to characterize the geopolymer structures. Water absorption capacity was measured by immersing the geopolyme...

  5. Determination of methane concentrations in water in equilibrium with sI methane hydrate in the absence of a vapor phase by in situ Raman spectroscopy (United States)

    Lu, W.; Chou, I.-Ming; Burruss, R.C.


    Most submarine gas hydrates are located within the two-phase equilibrium region of hydrate and interstitial water with pressures (P) ranging from 8 to 60 MPa and temperatures (T) from 275 to 293 K. However, current measurements of solubilities of methane in equilibrium with hydrate in the absence of a vapor phase are limited below 20 MPa and 283.15 K, and the differences among these data are up to 30%. When these data were extrapolated to other P-T conditions, it leads to large and poorly known uncertainties. In this study, in situ Raman spectroscopy was used to measure methane concentrations in pure water in equilibrium with sI (structure one) methane hydrate, in the absence of a vapor phase, at temperatures from 276.6 to 294.6 (??0.3) K and pressures at 10, 20, 30 and 40 (??0.4%) MPa. The relationship among concentration of methane in water in equilibrium with hydrate, in mole fraction [X(CH4)], the temperature in K, and pressure in MPa was derived as: X(CH4) = exp [11.0464 + 0.023267 P - (4886.0 + 8.0158 P)/T]. Both the standard enthalpy and entropy of hydrate dissolution at the studied T-P conditions increase slightly with increasing pressure, ranging from 41.29 to 43.29 kJ/mol and from 0.1272 to 0.1330 kJ/K ?? mol, respectively. When compared with traditional sampling and analytical methods, the advantages of our method include: (1) the use of in situ Raman signals for methane concentration measurements eliminates possible uncertainty caused by sampling and ex situ analysis, (2) it is simple and efficient, and (3) high-pressure data can be obtained safely. ?? 2007 Elsevier Ltd. All rights reserved.

  6. Synthesis of biomass derived carbon materials for environmental engineering and energy storage applications (United States)

    Huggins, Mitchell Tyler

    Biomass derived carbon (BC) can serve as an environmentally and cost effective material for both remediation and energy production/storage applications. The use of locally derived biomass, such as unrefined wood waste, provides a renewable feedstock for carbon material production compared to conventional unrenewable resources like coal. Additionally, energy and capital cost can be reduced through the reduction in transport and processing steps and the use of spent material as a soil amendment. However, little work has been done to evaluate and compare biochar to conventional materials such as granular activated carbon or graphite in advanced applications of Environmental Engineering. In this work I evaluated the synthesis and compared the performance of biochar for different applications in wastewater treatment, nutrient recovery, and energy production and storage. This includes the use of biochar as an electrode and filter media in several bioelectrochemical systems (BES) treating synthetic and industrial wastewater. I also compared the treatment efficiency of granular biochar as a packed bed adsorbent for the primary treatment of high strength brewery wastewater. My studies conclude with the cultivation of fungal biomass to serve as a template for biochar synthesis, controlling the chemical and physical features of the feedstock and avoiding some of the limitations of waste derived materials.

  7. Novel bio-based epoxy-polyurethane materials from modified vegetable oils – synthesis and characterization

    Directory of Open Access Journals (Sweden)

    A. Sienkiewicz


    Full Text Available Presented research shows the results of a study on mechanical properties of materials obtained in the course of innovatory application of epoxidized vegetable oil in the synthesis of new bio-based epoxy resins, crosslinked with curing agents which are not typical for epoxy materials. The product was obtained via modern and pro-ecological modification of a well-known synthesis method of epoxies, namely the epoxy fusion process, then it was crosslinked using polyisocyanates of different structure: toluene-2,4-diisocyanate (TDI, hexamethylene diisocyanate (HDI and 4,4’-methylene diphenyl diisocyanate (MDI. The obtained epoxy-polyurethane materials are characterized by various mechanical properties, which depend on the type of chosen isocyanate. Compositions based on HDI exhibit better mechanical characteristics than elastic polyurethane materials based on hydroxylated soybean oil. Materials cured with aromatic isocyanates MDI and TDI are characterized by higher mechanical resistance comparable with cast polyurethane based on petrochemical resources. Epoxy fusion product cured with toluene-2,4-diisocyanate in a presence of Dabco T9 appears to have the best mechanical properties among all tested compositions.

  8. Solution synthesis of one-dimensional ZnO nanomaterials and their applications. (United States)

    Weintraub, Benjamin; Zhou, Zhengzhi; Li, Yinhua; Deng, Yulin


    Recently, one-dimensional (1D) ZnO nanomaterials (NMs) have been extensively studied because both their functional properties and highly controllable morphology make them important building blocks for understanding nanoscale phenomena and realizing nanoscale devices. Compared with high temperature (>450 degrees C) vapor phase methods, solution-based synthesis methods can be conducted at low temperatures (25-200 degrees C) allowing for compatibility with many organic substrate materials and offer additional advantages such as straightforward processing, low cost, and ease of scale up. Although there exist several review articles in the literature regarding the synthesis and applications of 1D ZnO NMs, those focusing on solution-based synthesis methods are lacking. Thus, this review focuses mainly on 1D ZnO NMs synthesized by solution-based processing. Firstly, 1D ZnO non-patterned, nanoparticle-seeded synthesis and its associated solution growth kinetics are discussed. Next, synthesis of vertically-aligned ZnO nanorod arrays with controlled pattern and density on various substrates is reviewed. Finally, important applications of 1D ZnO NMs are highlighted including sensors, field emission devices, photodetectors, optical switches, and solar cells.

  9. Bioactive Glass Nanoparticles: From Synthesis to Materials Design for Biomedical Applications. (United States)

    Vichery, Charlotte; Nedelec, Jean-Marie


    Thanks to their high biocompatibility and bioactivity, bioactive glasses are very promising materials for soft and hard tissue repair and engineering. Because bioactivity and specific surface area intrinsically linked, the last decade has seen a focus on the development of highly porous and/or nano-sized materials. This review emphasizes the synthesis of bioactive glass nanoparticles and materials design strategies. The first part comprehensively covers mainly soft chemistry processes, which aim to obtain dispersible and monodispersed nanoparticles. The second part discusses the use of bioactive glass nanoparticles for medical applications, highlighting the design of materials. Mesoporous nanoparticles for drug delivery, injectable systems and scaffolds consisting of bioactive glass nanoparticles dispersed in a polymer, implant coatings and particle dispersions will be presented.

  10. Microwave Ignited Combustion Synthesis as a Joining Technique for Dissimilar Materials (United States)

    Rosa, Roberto; Colombini, Elena; Veronesi, Paolo; Poli, Giorgio; Leonelli, Cristina


    Microwave energy has been exploited to ignite combustion synthesis (CS) reactions of properly designed powders mixtures, in order to rapidly reach the joining between different kinds of materials, including metals (Titanium and Inconel) and ceramics (SiC). Beside the great advantage offered by CS itself, i.e., rapid and highly localized heat generation, the microwaves selectivity in being absorbed by micrometric metallic powders and not by bulk metallic components represents a further intriguing aspect in advanced materials joining applications, namely the possibility to avoid the exposition to high temperatures of the entire substrates to be joined. Moreover, in case of microwaves absorbing substrates, the competitive microwaves absorption by both substrates and powdered joining material, leads to the possibility of adhesion, interdiffusion and chemical bonding enhancements. In this study, both experimental and numerical simulation results are used to highlight the great potentialities of microwave ignited CS in the joining of advanced materials.

  11. Biomolecular crystals for material applications and a mechanistic study of an iron oxide nanoparticle synthesis (United States)

    Falkner, Joshua Charles

    The three projects within this work address the difficulties of controlling biomolecular crystal formats (i.e. size and shape), producing 3-D ordered composite materials from biomolecular crystal templates, and understanding the mechanism of a practical iron oxide synthesis. The unifying thread consistent throughout these three topics is the development of methods to manipulate nanomaterials using a bottom-up approach. Biomolecular crystals are nanometer to millimeter sized crystals that have well ordered mesoporous solvent channels. The overall physical dimensions of these crystals are highly dependent on crystallization conditions. The controlled growth of micro- and nanoprotein crystals was studied to provide new pathways for creating smaller crystalline protein materials. This method produced tetragonal hen egg-white lysozyme crystals (250--100,000 nm) with near monodisperse size distributions (membranes or templates. In this work, the porous structure of larger cowpea mosaic virus crystals was used to template metal nanoparticle growth within the body centered cubic crystalline network. The final composite material was found to have long range ordering of palladium and platinum nonocrystal aggregates (10nm) with symmetry consistent to the virus template. Nanoparticle synthesis itself is an immense field of study with an array of diverse applications. The final piece of this work investigates the mechanism behind a previously developed iron oxide synthesis to gain more understanding and direction to future synthesis strategies. The particle growth mechanism was found to proceed by the formation of a solvated iron(III)oleate complex followed by a reduction of iron (III) to iron (II). This unstable iron(II) nucleates to form a wustite (FeO) core which serves as an epitaxial surface for the magnetite (Fe3O4) shell growth. This method produces spherical particles (6-60nm) with relative size distributions of less than 15%.

  12. Controlling Magnetic and Ferroelectric Order Through Geometry: Synthesis, Ab Initio Theory, Characterization of New Multi-Ferric Fluoride Materials

    Energy Technology Data Exchange (ETDEWEB)

    Halasyamani, Shiv [Univ. of Houston, TX (United States); Fennie, Craig [Cornell Univ., Ithaca, NY (United States)


    We have focused on the synthesis, characterization, and ab initio theory on multi-functional mixed-metal fluorides. With funding from the DOE, we have successfully synthesized and characterized a variety of mixed metal fluoride materials.

  13. Design, synthesis, and characterization of materials for controlled line deposition, environmental remediation, and doping of porous manganese oxide material (United States)

    Calvert, Craig A.

    This thesis covers three topics: (1) coatings formed from sol-gel phases, (2) environmental remediation, and (3) doping of a porous manganese oxide. Synthesis, characterization, and application were investigated for each topic. Line-formations were formed spontaneously by self-assembly from vanadium sol-gels and other metal containing solutions on glass substrates. The solutions were prepared by the dissolution of metal oxide or salt in water. A more straightforward method is proposed than used in previous work. Analyses using optical microscopy, atomic force microscopy, scanning electron microscopy, energy-dispersive X-ray analysis, and infrared spectroscopy showed discreet lines whose deposition could be controlled by varying the concentration. A mechanism was developed from the observed results. Microwave heating, the addition of graphite rods, and oxidants, can enhance HCB remediation from soil. To achieve remediation, a TeflonRTM vessel open to the atmosphere along with an oxidant, potassium persulfate (PerS) or potassium hydroxide, along with uncoated or aluminum oxide coated, graphite rods were heated in a research grade microwave oven. Microwave heating was used to decrease the heating time, and graphite rods were used to increase the absorption of the microwave energy by providing thermal centers. The results showed that the percent HCB removed was increased by adding graphite rods and oxidants. Tungsten, silver, and sulfur were investigated as doping agents for K--OMS-2. The synthesis of these materials was carried out with a reflux method. The doping of K--OMS-2 led to changes in the properties of a tungsten doped K--OMS-2 had an increased resistivity, the silver doped material showed improved epoxidation of trans-stilbene, and the addition of sulfur produced a paper-like material. Rietveld refinement of the tungsten doped K--OMS-2 showed that the tungsten was doped into the framework.

  14. Development of a poly(dimethylacrylamide) based matrix material for solid phase high density peptide array synthesis employing a laser based material transfer

    Energy Technology Data Exchange (ETDEWEB)

    Ridder, Barbara [Institute of Microstructure Technology (IMT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Institute of Organic Chemistry (IOC), Karlsruhe Institute of Technology (KIT), Fritz-Haber-Weg 6, 76131 Karlsruhe (Germany); Foertsch, Tobias C. [Institute of Microstructure Technology (IMT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Welle, Alexander [Karlsruhe Nano Micro Facility (KNMF), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Mattes, Daniela S. [Institute of Microstructure Technology (IMT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Institute of Organic Chemistry (IOC), Karlsruhe Institute of Technology (KIT), Fritz-Haber-Weg 6, 76131 Karlsruhe (Germany); Bojnicic-Kninski, Clemens M. von; Loeffler, Felix F.; Nesterov-Mueller, Alexander [Institute of Microstructure Technology (IMT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Meier, Michael A.R., E-mail: [Institute of Organic Chemistry (IOC), Karlsruhe Institute of Technology (KIT), Fritz-Haber-Weg 6, 76131 Karlsruhe (Germany); Breitling, Frank, E-mail: [Institute of Microstructure Technology (IMT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany)


    Highlights: • New matrix material for peptide array synthesis from a ‘solid solvent’. • Resolution was increased with possible spot densities of up to 20.000 spots per cm{sup 2}. • The coupling depth and the effectiveness of washing steps analyzed by ToF-SIMS. • Adaptations and custom changes of the matrix material are possible. - Abstract: Poly(dimethylacrylamide) (PDMA) based matrix materials were developed for laser-based in situ solid phase peptide synthesis to produce high density arrays. In this specific array synthesis approach, amino acid derivatives are embedded into a matrix material, serving as a “solid” solvent material at room temperature. Then, a laser pulse transfers this mixture to the target position on a synthesis slide, where the peptide array is synthesized. Upon heating above the glass transition temperature of the matrix material, it softens, allowing diffusion of the amino acid derivatives to the synthesis surface and serving as a solvent for peptide bond formation. Here, we synthesized PDMA six-arm star polymers, offering the desired matrix material properties, using atom transfer radical polymerization. With the synthesized polymers as matrix material, we structured and synthesized arrays with combinatorial laser transfer. With densities of up to 20,000 peptide spots per cm{sup 2}, the resolution could be increased compared to the commercially available standard matrix material. Time-of-Flight Secondary Ion Mass Spectrometry experiments revealed the penetration behavior of an amino acid derivative into the prepared acceptor synthesis surface and the effectiveness of the washing protocols.

  15. Synthesis of graphene and related two-dimensional materials for bioelectronics devices. (United States)

    Zhang, Tao; Liu, Jilun; Wang, Cheng; Leng, Xuanye; Xiao, Yao; Fu, Lei


    In recent years, graphene and related two-dimensional (2D) materials have emerged as exotic materials in nearly every fields of fundamental science and applied engineering. The latest progress has shown that these 2D materials could have a profound impact on bioelectronics devices. For the construction of these bioelectronics devices, these 2D materials were generally synthesized by the processes of exfoliation and chemical vapor deposition. In particular, the macrostructures of these 2D materials have also been realized by these two processes, which have shown great potentials in the self-supported and special-purpose biosensors. Due to the high specific surface area, subtle electron properties, abundant surface atoms of these 2D materials, the as-constructed bioelectronics devices have exhibited enhanced performance in the sensing of small biomolecules, heavy metals, pH, protein and DNA. The aim of this review article is to provide a comprehensive scientific progress in the synthesis of 2D materials for the construction of five typical bioelectronics devices (electrochemical biosensors, FET-based biosensors, piezoelectric devices, electrochemiluminescence devices and supercapacitors) and to overview the present status and future perspective of the applications of these bioelectronics devices based on 2D materials. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Recent Advances in Two-Dimensional Materials with Charge Density Waves: Synthesis, Characterization and Applications

    Directory of Open Access Journals (Sweden)

    Mongur Hossain


    Full Text Available Recently, two-dimensional (2D charge density wave (CDW materials have attracted extensive interest due to potential applications as high performance functional nanomaterials. As other 2D materials, 2D CDW materials are layered materials with strong in-plane bonding and weak out-of-plane interactions enabling exfoliation into layers of single unit cell thickness. Although bulk CDW materials have been studied for decades, recent developments in nanoscale characterization and device fabrication have opened up new opportunities allowing applications such as oscillators, electrodes in supercapacitors, energy storage and conversion, sensors and spinelectronic devices. In this review, we first outline the synthesis techniques of 2D CDW materials including mechanical exfoliation, liquid exfoliation, chemical vapor transport (CVT, chemical vapor deposition (CVD, molecular beam epitaxy (MBE and electrochemical exfoliation. Then, the characterization procedure of the 2D CDW materials such as temperature-dependent Raman spectroscopy, temperature-dependent resistivity, magnetic susceptibility and scanning tunneling microscopy (STM are reviewed. Finally, applications of 2D CDW materials are reviewed.

  17. Spectroscopic characterizations of a mixed surfactant mesophase and its application in materials synthesis (United States)

    Liu, Limin

    A viscous lyotropic crystalline mesophase containing bis (2-ethylhexyl) sodium sulfosuccinate (AOT), alpha-phosphatidylcholine (lecithin), with comparable volume fractions of isooctane and water was characterized by Fourier-transform 31P and 1H nuclear magnetic resonance (NMR) spectroscopy. Shear alignment on the reverse hexagonal mesophase was reflected through both 31P NMR and 1H NMR spectra. A complicated 31P spectrum was observed as a result of superposition of chemical shifts according to the distribution of crystalline domains prior to shear. The initially disordered samples with polydomain structures became macroscopically aligned after Couette shear and the alignment retained for a long period of time. 31P NMR chemical shift anisotropy characteristics were used to elucidate orientation of the hexagonal phase. Interestingly, 1H NMR of the water, methyl and methylene groups exhibited spectral changes upon shear alignment closely corresponding with that of 31P NMR spectra. A reverse hexagonal to lamellar phase transition was manifested as an expanding of the expressed 31P NMR chemical shift anisotropy and an apparent reversal of the powder pattern with increasing water content and/or temperature. Correspondingly, 1H NMR spectra also experienced a spectral pattern transition as the water content or temperature was increased. These observations complement the findings of mesophase alignment obtained using small angle neutron scattering (SANS) and imply that 31P and 1H NMR spectroscopy can be used as probes to define microstructure and monitor orientation changes in this binary surfactant system. This is especially beneficial if these mesophases are used as templates for materials synthesis. The mesophase retains its alignment for extended periods allowing materials synthesis to be decoupled from the application of shear. Highly aligned string-like silica nanostructures were obtained through templated synthesis in the columnar hexagonal structure of the viscous

  18. Physical-chemical characterization of Tunisian clays for the synthesis of geopolymers materials (United States)

    Selmani, S.; Essaidi, N.; Gouny, F.; Bouaziz, S.; Joussein, E.; Driss, A.; Sdiri, A.; Rossignol, S.


    Natural clay materials from Tunisia were examined as an aluminosilicate source for the synthesis of consolidated materials at low temperatures. Three clay samples were collected from the El Kef, Douiret and Gafsa basins and calcined at different temperatures. All of the samples were characterized using chemical and mineralogical analyses, thermogravimetry, dilatometry, and Fourier transform infrared spectroscopy (FTIR) measurements. The chemical (XRF) and mineralogical analyses (XRD and FTIR) indicated that all of the samples contained various amounts of kaolinite and quartz, followed by calcite, mica, palygorskite and gypsum. Curing produced a binder which did not significantly affect the physic-chemical properties of these clays. The obtained materials heterogeneous did not reach the geopolymerization stage, most likely because of their low kaolinite content. The addition of a suitable aluminosilicate to these clays is therefore recommended to produce homogeneous consolidated geopolymers. The synthesized materials obtained after the addition of metakaolin to the formulation to improve reactivity have interesting properties, thereby providing good potential for Tunisian clays in the synthesis of geopolymers.

  19. Ion beams provided by small accelerators for material synthesis and characterization (United States)

    Mackova, Anna; Havranek, Vladimir


    The compact, multipurpose electrostatic tandem accelerators are extensively used for production of ion beams with energies in the range from 400 keV to 24 MeV of almost all elements of the periodic system for the trace element analysis by means of nuclear analytical methods. The ion beams produced by small accelerators have a broad application, mainly for material characterization (Rutherford Back-Scattering spectrometry, Particle Induced X ray Emission analysis, Nuclear Reaction Analysis and Ion-Microprobe with 1 μm lateral resolution among others) and for high-energy implantation. Material research belongs to traditionally progressive fields of technology. Due to the continuous miniaturization, the underlying structures are far beyond the analytical limits of the most conventional methods. Ion Beam Analysis (IBA) techniques provide this possibility as they use probes of similar or much smaller dimensions (particles, radiation). Ion beams can be used for the synthesis of new progressive functional nanomaterials for optics, electronics and other applications. Ion beams are extensively used in studies of the fundamental energetic ion interaction with matter as well as in the novel nanostructure synthesis using ion beam irradiation in various amorphous and crystalline materials in order to get structures with extraordinary functional properties. IBA methods serve for investigation of materials coming from material research, industry, micro- and nano-technology, electronics, optics and laser technology, chemical, biological and environmental investigation in general. Main research directions in laboratories employing small accelerators are also the preparation and characterization of micro- and nano-structured materials which are of interest for basic and oriented research in material science, and various studies of biological, geological, environmental and cultural heritage artefacts are provided too.

  20. Precision Synthesis of Functional Polysaccharide Materials by Phosphorylase-Catalyzed Enzymatic Reactions

    Directory of Open Access Journals (Sweden)

    Jun-ichi Kadokawa


    Full Text Available In this review article, the precise synthesis of functional polysaccharide materials using phosphorylase-catalyzed enzymatic reactions is presented. This particular enzymatic approach has been identified as a powerful tool in preparing well-defined polysaccharide materials. Phosphorylase is an enzyme that has been employed in the synthesis of pure amylose with a precisely controlled structure. Similarly, using a phosphorylase-catalyzed enzymatic polymerization, the chemoenzymatic synthesis of amylose-grafted heteropolysaccharides containing different main-chain polysaccharide structures (e.g., chitin/chitosan, cellulose, alginate, xanthan gum, and carboxymethyl cellulose was achieved. Amylose-based block, star, and branched polymeric materials have also been prepared using this enzymatic polymerization. Since phosphorylase shows a loose specificity for the recognition of substrates, different sugar residues have been introduced to the non-reducing ends of maltooligosaccharides by phosphorylase-catalyzed glycosylations using analog substrates such as α-d-glucuronic acid and α-d-glucosamine 1-phosphates. By means of such reactions, an amphoteric glycogen and its corresponding hydrogel were successfully prepared. Thermostable phosphorylase was able to tolerate a greater variance in the substrate structures with respect to recognition than potato phosphorylase, and as a result, the enzymatic polymerization of α-d-glucosamine 1-phosphate to produce a chitosan stereoisomer was carried out using this enzyme catalyst, which was then subsequently converted to the chitin stereoisomer by N-acetylation. Amylose supramolecular inclusion complexes with polymeric guests were obtained when the phosphorylase-catalyzed enzymatic polymerization was conducted in the presence of the guest polymers. Since the structure of this polymeric system is similar to the way that a plant vine twines around a rod, this polymerization system has been named

  1. On the chemical synthesis route to bulk-scale skutterudite materials

    DEFF Research Database (Denmark)

    Tafti, Mohsen Y.; Saleemi, Mohsin; Han, Li


    In this article an alternative high yield route for the synthesis of CoSb3-based unfilled skutterudites is presented. Using low-melting temperature salts of the constituents, melting and mixing them homogeneously in a hydrophobic liquid with postprocessing of the powders we achieve a more...... intimately mixed alloy compared to the conventional melting and metallurgical processes. The proposed method consists of a fast and low-temperature processing step followed by a thermochemical post-processing step, compared to the conventional methods of fabricating skutterudites, which require high...... temperatures and long processing times. Several structural characterization techniques were used to assess the mechanism of synthesis, verify the purity of the material as well as the reproducibility of the process. Detailed analysis and results are presented in support of the proposed process. Additionally...

  2. High-Throughput Synthesis of Support Materials for Olefin Polymerization Catalyst. (United States)

    Chammingkwan, Patchanee; Terano, Minoru; Taniike, Toshiaki


    Rational catalyst design necessitates fundamental knowledge on the structure-performance relationship, while the synthetic throughput for heterogeneous Ziegler-Natta olefin polymerization catalysts has long prevented the acquisition of a statistical database. In this contribution, an in-house reactor system was developed to realize the parallel synthesis of support materials for Ziegler-Natta catalysts for the first time. The developed system enabled parallel synthesis of 24 magnesium ethoxide samples with excellent reproducibility and morphological control comparable to a conventional experiment. Our demonstration revealed that the generation of diverse particle characteristics could be achieved through the addition of a third component as a structural modulator, in which the in-house parallel reactor system combined with the first principle component analysis enabled fast screening of effective modulators.

  3. Contingencies and metacontingencies: Toward a synthesis of behavior analysis and cultural materialism (United States)

    Glenn, Sigrid S.


    A synthesis of cultural materialism and behavior analysis might increase the scientific and technological value of both fields. Conceptual and substantive relations between the two fields show important similarities, particularly with regard to the causal role of the environment in behavioral and cultural evolution. Key concepts in Marvin Harris's cultural materialist theories are outlined. A distinction is made between contingencies at the behavioral level of analysis (contingencies of reinforcement) and contingencies at the cultural level of analysis (metacontingencies). Relations between the two kinds of contingencies are explored in cultural practices from paleolithic to industrial sociocultural systems. A synthesis of these two fields may offer the opportunity to resolve serious problems currently facing modern cultures. PMID:22478011

  4. Contingencies and metacontingencies: Toward a synthesis of behavior analysis and cultural materialism. (United States)

    Glenn, S S


    A synthesis of cultural materialism and behavior analysis might increase the scientific and technological value of both fields. Conceptual and substantive relations between the two fields show important similarities, particularly with regard to the causal role of the environment in behavioral and cultural evolution. Key concepts in Marvin Harris's cultural materialist theories are outlined. A distinction is made between contingencies at the behavioral level of analysis (contingencies of reinforcement) and contingencies at the cultural level of analysis (metacontingencies). Relations between the two kinds of contingencies are explored in cultural practices from paleolithic to industrial sociocultural systems. A synthesis of these two fields may offer the opportunity to resolve serious problems currently facing modern cultures.

  5. Ullmann-like reactions for the synthesis of complex two-dimensional materials (United States)

    Quardokus, Rebecca C.; Tewary, V. K.; DelRio, Frank W.


    Engineering two-dimensional materials through surface-confined synthetic techniques is a promising avenue for designing new materials with tailored properties. Developing and understanding reaction mechanisms for surface-confined synthesis of two-dimensional materials requires atomic-level characterization and chemical analysis. Beggan et al (2015 Nanotechnology 26 365602) used scanning tunneling microscopy and x-ray photoelectron spectroscopy to elucidate the formation mechanism of surface-confined Ullmann-like coupling of thiophene substituted porphyrins on Ag(111). Upon surface deposition, bromine is dissociated and the porphyrins couple with surface adatoms to create linear strands and hexagonally packed molecules. Annealing the sample results in covalently-bonded networks of thienylporphyrin derivatives. A deeper understanding of surface-confined Ullmann-like coupling has the potential to lead to precision-engineered nano-structures through synthetic techniques. Contribution of the National Institute of Standards and Technology, not subject to copyright in the United States of America.

  6. One-Step Facile Synthesis of a Simple Hole Transport Material for Efficient Perovskite Solar Cells

    KAUST Repository

    Chen, Hu


    A hole transporting material was designed for use in perovskite solar cells, with a facile one-step synthesis from inexpensive, com-mercially available reagents. The molecule comprises a central fluorinated phenyl core with pendant aryl amines, namely, 3,6-difluoro-N1,N1,N2,N2,N4,N4,N5,N5-octakis(4-methoxyphenyl)benzene-1,2,4,5-tetraamine (DFTAB). A power conversion efficiency of up to 10.4% was achieved in a mesoporous perovskite device architecture. The merits of a simple and potentially low cost syn-thetic route as well as promising performance in perovskite devices, encourages further development of this materials class as new low-cost hole transporting materials for the scale up of perovskite solar cells.

  7. Synthesis of High-Purity alpha-and beta-PbO and Possible Applications to Synthesis and Processing of Other Lead Oxide Materials

    Energy Technology Data Exchange (ETDEWEB)

    Perry, Dale L.; Wilkinson, T. J.


    The red, tetragonal form of lead oxide, alpha-PbO, litharge, and the yellow, orthorhombic form, beta-PbO, massicot, have been synthesized from lead(II) salts in aqueous media at elevated temperature. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) were used to characterize the size, morphology, and crystallographic structural forms of the products. The role of impurities in the experimental synthesis of the materials and microstructural variations in the final products are described, and the implications of these observations with respect to the synthesis of different conducting lead oxides and other related materials are discussed.

  8. Cathode materials produced by spray flame synthesis for lithium ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Hamid, NoorAshrina Binti A.


    Lithium ion batteries are one of the most enthralling rechargeable energy storage systems for portable application due to their high energy density. Nevertheless, with respect to electromobility innovation towards better electrochemical properties such as higher energy and power density is required. Altering the cathode material used in Li-ion batteries is favorable since the mass- and volume performance is closely related to the cathode electrode mass. Instead of using LiCoO{sub 2} as cathode electrode, LiFePO{sub 4} has gained serious attention as this material owns a high theoretical capacity of 170 mAh g{sup -1}. It is non-toxic, cheap and consists of abundant materials but suffers from low electronic and ionic conductivity. Utilization of nanotechnology methods in combination with composite formation is known to cure this problem effectively. In this work, a new combination of techniques using highly scalable gas-phase synthesis namely spray-flame synthesis and subsequent solid-state reaction has been used to synthesize nanocomposite LiFePO{sub 4}/C. At first this work deals with the formation and characterization of nanosize FePO{sub 4} from a solution of iron(III)acetylacetonate and tributyl phosphate in toluene using spray-flame synthesis. It was shown that a subsequent solid state reaction with Li{sub 2}CO{sub 3} and glucose yielded a LiFePO{sub 4}/C nanocomposite with very promising electrochemical properties. Based on these initial findings the influence of two synthesis parameter - carbon content and annealing temperature - was investigated towards the physicochemical properties of LiFePO{sub 4}/C. It was shown that an annealing temperature of 700 C leads to high purity composite materials consisting of crystalline LiFePO{sub 4} with crystallite sizes well below 100 nm and amorphous carbon consisting of disordered and graphite-like carbon. Variation of glucose amount between 10 and 30 wt% resulted in carbon contents between 2.1 and 7.3 wt%. In parallel

  9. Top-down synthesis of versatile polyaspartamide linkers for single-step protein conjugation to materials. (United States)

    Cha, Chaenyung; Jeong, Jae Hyun; Tang, Xin; Zill, Andrew T; Prakash, Y S; Zimmerman, Steven C; Saif, Taher A; Kong, Hyunjoon


    Materials used in various biological applications are often modified with proteins to regulate biomolecular and cellular adhesion. Conventional strategies of protein conjugation accompany monovalent bifunctional protein linkers, which present several limitations in molecular synthesis and protein conjugation. Herein, we present a new strategy of preparing multivalent polyaspartamide linkers in a simple top-down manner, and also demonstrate that the resulting polymer linkers allow us to readily conjugate proteins to both organic and inorganic materials. The top-down synthesis of polyaspartamide linkers was performed by partially opening succinimidyl ring moieties of polysuccinimide (PSI) with the controlled number of nucleophiles reactive to photo-cross-linked hydrogel or gold-coated inorganic materials: (1) Poly(2-hydroxyethyl-co-2-methacryloxyethyl aspartamide) (PHMAA) presenting methacrylate was used to micropattern fibronectin or collagen on a hydrogel in order to regulate cell adhesion and growth area on a micrometer scale. (2) Poly(2-hydroxyethyl-co-2-mercaptoethyl aspartamide) (PHMCA) presenting thiol functional groups was used to link fibronectin to a gold-coated silicon microelectromechanical probe designed to measure cell traction force. Overall, these multivalent polyaspartamide protein linkers will greatly assist efforts to analyze and regulate the cellular adhesion to and phenotypic activities of a wide array of substrates and devices.

  10. Novel LLM series high density energy materials: Synthesis, characterization, and thermal stability (United States)

    Pagoria, Philip; Zhang, Maoxi; Tsyshevskiy, Roman; Kuklja, Maija

    Novel high density energy materials must satisfy specific requirements, such as an increased performance, reliably high stability to external stimuli, cost-efficiency and ease of synthesis, be environmentally benign, and be safe for handling and transportation. During the last decade, the attention of researchers has drifted from widely used nitroester-, nitramine-, and nitroaromatic-based explosives to nitrogen-rich heterocyclic compounds. Good thermal stability, the low melting point, high density, and moderate sensitivity make heterocycle materials attractive candidates for use as oxidizers in rocket propellants and fuels, secondary explosives, and possibly as melt-castable ingredients of high explosive formulations. In this report, the synthesis, characterization, and results of quantum-chemical DFT study of thermal stability of LLM-191, LLM-192 and LLM-200 high density energy materials are presented. Work performed under the auspices of the DOE by the LLNL (Contract DE-AC52-07NA27344). This research is supported in part by ONR (Grant N00014-12-1-0529) and NSF. We used NSF XSEDE (Grant DMR-130077) and DOE NERSC (Contract DE-AC02-05CH11231) resources.

  11. Design, synthesis and polymerization of novel second-order nonlinear optical materials (United States)

    Ghosn, Rima Kamal


    This dissertation focuses on the design, synthesis and nonlinear optical properties of large second-order nonlinearity chromophores. A review of the fundamentals of nonlinear optics and polymeric materials is provided in the first chapter. The second chapter focuses on the optimization of reaction conditions of asymmetric diphenyl diacetylene liquid crystals. The third chapter deals with the design and synthesis of chromophores derived from thiobarbituric acids. Conventional nonlinear optical organic materials employ chromophores possessing a large transition dipole moment between the ground and first excited states. This requirement is fulfilled using conjugated molecules containing optimally balanced electron donor and acceptor moieties. Barbituric acid is a strong electron acceptor that yields molecules with a large first hyperpolarizabilities. There are two classes of chromophores investigated, both capable of covalent polymer incorporation, which include the main chain and double-end crosslinkable chromophores. These chromophores, high in both nonlinearity and thermal stability, are regarded as ideal candidates for electrooptical devices. The fourth chapter investigates polyimides as stable NLO polymeric materials.

  12. Applications of Continuous-Flow Photochemistry in Organic Synthesis, Material Science, and Water Treatment. (United States)

    Cambié, Dario; Bottecchia, Cecilia; Straathof, Natan J W; Hessel, Volker; Noël, Timothy


    Continuous-flow photochemistry in microreactors receives a lot of attention from researchers in academia and industry as this technology provides reduced reaction times, higher selectivities, straightforward scalability, and the possibility to safely use hazardous intermediates and gaseous reactants. In this review, an up-to-date overview is given of photochemical transformations in continuous-flow reactors, including applications in organic synthesis, material science, and water treatment. In addition, the advantages of continuous-flow photochemistry are pointed out and a thorough comparison with batch processing is presented.

  13. Applications of sample-controlled thermal analysis (SCTA) to kinetic analysis and synthesis of materials


    Pérez-Maqueda, Luis A.; Criado Luque, J.M.; Sánchez-Jiménez, P.E.; Diánez, M. J.


    The advantages of the sample-controlled thermal analysis (SCTA) for both the kinetic analysis of solid-state reactions and the synthesis of materials are reviewed. This method implies an intelligent control of the temperature by the solid-state reaction under study in such a way that the reaction rate as a function of the time fits a profile previously defined by the user. It has been shown that SCTA has important advantages for discriminating the kinetic model of solid-state reactions as com...

  14. Interface modification and material synthesis of organic light-emitting diodes using plasma technology (United States)

    Liang, Rongqing; Ou, Qiongrong; Yang, Cheng; He, Kongduo; Yang, Xilu; Zhong, Shaofeng; plasma application Team


    Organic light-emitting diodes (OLEDs), due to their unique properties of solution processability, compatibility with flexible substrates and with large-scale printing technology, attract huge interest in the field of lighting. The integration of plasma technology into OLEDs provides a new route to improve their performance. Here we demonstrate the modification of indium-tin-oxide (ITO) work function by plasma treatment, synthesis of thermally activated delayed fluorescence (TADF) materials using plasma grafting (polymerisation), and multi-layer solution processing achieved by plasma cross-linking.

  15. Mechanistic Studies of Combustion and Structure Formation During Synthesis of Advanced Materials (United States)

    Varma, A.; Lau, C.; Mukasyan, A. S.


    Combustion in a variety of heterogeneous systems, leading to the synthesis of advanced materials, is characterized by high temperatures (2000-3500 K) and heating rates (up to 10(exp 6) K/s) at and ahead of the reaction front. These high temperatures generate liquids and gases which are subject to gravity-driven flow. The removal of such gravitational effects is likely to provide increased control of the reaction front, with a consequent improvement in control of the microstructure of the synthesized products. Thus, microgravity (mu-g) experiments lead to major advances in the understanding of fundamental aspects of combustion and structure formation under the extreme conditions of the combustion synthesis (CS) wave. In addition, the specific features of microgravity environment allow one to produce unique materials, which cannot be obtained under terrestrial conditions. The current research is a logic continuation of our previous work on investigations of the fundamental phenomena of combustion and structure formation that occur at the high temperatures achieved in a CS wave. Our research is being conducted in three main directions: 1) Microstructural Transformations during Combustion Synthesis of Metal-Ceramic Composites. The studies are devoted to the investigation of particle growth during CS of intermetallic-ceramic composites, synthesized from nickel, aluminum, titanium, and boron metal reactants. To determine the mechanisms of particle growth, the investigation varies the relative amount of components in the initial mixture to yield combustion wave products with different ratios of solid and liquid phases, under 1g and mu-g conditions; 2) Mechanisms of Heat Transfer during Reactions in Heterogeneous Media. Specifically, new phenomena of gasless combustion wave propagation in heterogeneous media with porosity higher than that achievable in normal gravity conditions, are being studied. Two types of mixtures are investigated: clad powders, where contact between

  16. Synthesis of functional mesoporous materials and their applications for oil sands

    Energy Technology Data Exchange (ETDEWEB)

    Mutyala, S.; Rahimi, P.; Fairbridge, C.; Alem, T. [National Centre for Upgrading Technology, Devon, AB (Canada); Natural Resources Canada, Devon, AB (Canada). CanmetENERGY


    Athabasca bitumen contains about 1 weight per cent of organic acids. Naphthenic acids (NAs) can cause corrosion in refinery equipment and should therefore be removed. This study focused on converting or removing NAs by using functional mesoporous materials under mild conditions. This poster described the synthesis of functional hybrid mesoporous materials. The materials were characterized by scanning electron microscopy/transmission electron microscopy (SEM/TEM) and Fourier transform infrared (FTIR) analysis. Thiol modified mesoporous materials showed higher activity for adsorption of metals. Alkyl or aryl sulphonic acid-functionalized mesoporous silicas were synthesized using a one-step approach with in-situ oxidation of thiol groups to the sulphonic acid groups. The resulting solid acid materials were tested for their catalytic performance in the esterification of naphthenic acids model compounds with methanol to produce corresponding methyl esters. Well dispersed palladium nanoparticles were identified in the mesoporous materials. High product yields were obtained for naphthenic acids model compounds and isolated NA's by sulphonic acid functionalized catalyst. tabs., figs.

  17. Research Update: Hybrid organic-inorganic perovskite (HOIP thin films and solar cells by vapor phase reaction

    Directory of Open Access Journals (Sweden)

    Po-Shen Shen


    Full Text Available With the rapid progress in deposition techniques for hybrid organic-inorganic perovskite (HOIP thin films, this new class of photovoltaic (PV technology has achieved material quality and power conversion efficiency comparable to those established technologies. Among the various techniques for HOIP thin films preparation, vapor based deposition technique is considered as a promising alternative process to substitute solution spin-coating method for large-area or scale-up preparation. This technique provides some unique benefits for high-quality perovskite crystallization, which are discussed in this research update.

  18. New materials graphyne, graphdiyne, graphone, and graphane: review of properties, synthesis, and application in nanotechnology

    Directory of Open Access Journals (Sweden)

    Peng Q


    Full Text Available Qing Peng,1 Albert K Dearden,2 Jared Crean,1 Liang Han,1 Sheng Liu,3 Xiaodong Wen,4,5 Suvranu De11Department of Mechanical, Aerospace and Nuclear Engineering, Rensselaer Polytechnic Institute, Troy, NY, USA; 2Department of Physics, Applied Physics, and Astronomy, Rensselaer Polytechnic Institute, Troy, NY, USA; 3Institute for Microsystems, School of Mechanical Engineering, Huazhong University of Science and Technology, Wuhan, People's Republic of China; 4State Key Laboratory of Coal Conversion, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan, People's Republic of China; 5Synfuels China Co, Ltd, Huairou, Beijing, People's Republic of ChinaAbstract: Plenty of new two-dimensional materials including graphyne, graphdiyne, graphone, and graphane have been proposed and unveiled after the discovery of the "wonder material" graphene. Graphyne and graphdiyne are two-dimensional carbon allotropes of graphene with honeycomb structures. Graphone and graphane are hydrogenated derivatives of graphene. The advanced and unique properties of these new materials make them highly promising for applications in next generation nanoelectronics. Here, we briefly review their properties, including structural, mechanical, physical, and chemical properties, as well as their synthesis and applications in nanotechnology. Graphyne is better than graphene in directional electronic properties and charge carriers. With a band gap and magnetism, graphone and graphane show important applications in nanoelectronics and spintronics. Because these materials are close to graphene and will play important roles in carbon-based electronic devices, they deserve further, careful, and thorough studies for nanotechnology applications.Keywords: two-dimensional materials, graphene-like structures, properties and synthesis, nanotechnology applications, graphyne, hydrogenation of grapheme

  19. Catalyst-Free Vapor-Phase Method for Direct Integration of Gas Sensing Nanostructures with Polymeric Transducing Platforms

    Directory of Open Access Journals (Sweden)

    Stella Vallejos


    Full Text Available Tungsten oxide nanoneedles (NNs are grown and integrated directly with polymeric transducing platforms for gas sensors via aerosol-assisted chemical vapor deposition (AACVD method. Material analysis shows the feasibility to grow highly crystalline nanomaterials in the form of NNs with aspect ratios between 80 and 200 and with high concentration of oxygen vacancies at the surface, whereas gas testing demonstrates moderate sensing responses to hydrogen at concentrations between 10 ppm and 50 ppm, which are comparable with results for tungsten oxide NNs grown on silicon transducing platforms. This method is demonstrated to be an attractive route to fabricate next generation of gas sensors devices, provided with flexibility and functionality, with great potential in a cost effective production for large-scale applications.

  20. X-ray induced synthesis of a novel material: Stable, doped solid CO at ambient conditions (United States)

    Pravica, Michael; Evlyukhin, Egor; Cifligu, Petrika; Harris, Blake; Jae Koh, Jung; Chen, Ning; Wang, Yonggang


    We report a novel synthesis of stable doped solid carbon monoxide (p-CO) via hard X-ray irradiation of strontium oxalate at ambient conditions and high pressure. We also show via mid- and far- infrared (IR) techniques that CO2 produced via X-ray photochemistry remained trapped within the recovered sample for many months in contrast to pure p-CO which decomposes in days. Our results demonstrate that p-CO doped with carbonates (as verified with IR and Extended X-ray Absorption Fine Structure spectroscopies) is relatively stable, enabling longer term and practical use of this novel material for CO2 storage or as a novel electrical/optical material.

  1. Preparing compound heterozygous reference material using gene synthesis technology: a model of thrombophilic mutations. (United States)

    Beranek, Martin; Drastikova, Monika; Dulicek, Petr; Palicka, Vladimir


    The aim of our study is to present a novel approach for preparing a compound heterozygous reference material (hetRM) using gene synthesis technology with inverted insertion of wild-type and mutant fragments into a single cloning vector. Factor II (G20210A) and Factor V (G1691A Leiden) gene mutations were used as an experimental model. During the gene synthesis, DNA fragments were aligned in the following order: G1691 FV wild-type forward strain, G20210 FII wild-type forward strain, 1691A FV mutant reverse strain, 20210A FII mutant reverse strain. The complete chain was inserted into a pIDT SMART cloning vector and amplified in an E. coli competent strain. For assessing hetRM characteristics and commutability, we used real-time PCR with subsequent melting curve analysis, real-time PCR with hydrolysis probes, allele-specific amplification, reverse hybridization, and dideoxynucleotide DNA sequencing. All five methods yielded concordant results of DNA analysis of the hetRM. Differences in real-time PCR cycle threshold values after six-months of storage at -80 °C were not statistically significant from those obtained from freshly prepared hetRM aliquots, which is a good indication of their stability. By applying the procedures of gene synthesis and cloning technology, we prepared and verified a model genetic reference material for FII G20210A and FV G1691A testing with a compound heterozygous genotype. The hetRM was stable, commutable, and available in large quantities and in a wide concentration range.

  2. Synthesis and Characterization of High Aluminum Zeolite X from Technical Grade Materials

    Directory of Open Access Journals (Sweden)

    Seyed Kamal Masoudian


    Full Text Available Zeolites are widely used as ion exchangers, adsorbents, separation materials and catalyst due to their well-tailored and highly-reproducible structures; therefore, the synthesis of zeolite from low grade resources can be interested. In the present work, high aluminum zeolite X was prepared from mixing technical grade sodium aluminate and sodium silicate solutions at temperatures between 70°C and 100°C. The synthesized zeolite X was characterized by SEM and X-ray methods according to ASTM standard procedures. The results showed that aging of the synthesis medium at the room temperature considerably increased the selectivity of zeolite X formation. On the other hand, high temperature of reaction mixture during crystallization formed zeolite A in the product; therefore, it decreased the purity of zeolite X. In addition, it was found that increasing H2O/Na2O and decreasing Na2O/SiO2 molar ratios in the reaction mixture resulted product with higher purity. © 2013 BCREC UNDIP. All rights reservedReceived: 7th January 2013; Revised: 7th April 2013; Accepted: 19th April 2013[How to Cite: Masoudian, S. K., Sadighi, S., Abbasi, A. (2013. Synthesis and Characterization of High Alu-minum Zeolite X from Technical Grade Materials. Bulletin of Chemical Reaction Engineering & Catalysis, 8 (1: 54-60. (doi:10.9767/bcrec.8.1.4321.54-60][Permalink/DOI:] | View in  |


    Directory of Open Access Journals (Sweden)

    Suyanta Suyanta


    Full Text Available The research about synthesis and characterization of MCM-41 from rice husk has been done. Silica (SiO2 was extracted from rice husk by refluxing with 3M hydrochloric solution at 80 °C for 3 h. The acid-leached rice husk was filtered, washed, dried and calcined at 650 °C for 6 h lead the rough powder of rice husk silica with light brown in color. Characterization was carried out by X-ray diffraction (XRD and FTIR spectroscopy method. Rice husk silica was dissolved into the sodium hydroxide solution leading to the solution of sodium silicate, and used as silica source for the synthesis of MCM-41. MCM-41 was synthesized by hydrothermal process to the mixture prepared from 29 g of distilled water, 8.67 g of cetyltrimethyl ammonium bromide (CTMAB, 9.31 g of sodium silicate solution, and amount mL of 1 M H2SO4. Hydrothermal process was carried out at 100 °C in a teflon-lined stainless steel autoclave heated in the oven for 36 h. The solid phase was filtered, then washed with deionised water, and dried in the oven at 100 °C for 2 h. The surfactant CTMAB was removed by calcination at 550 °C for 10 h with heating rate 2 °C/min. The as-synthesized and calcined crystals were characterized by using FTIR spectroscopy, X-ray diffraction and N2 physisorption methods. In order to investigate the effect of silica source, the same procedure was carried out by using pure sodium silicate as silica source. It was concluded that silica extracted from rice husk can be used as raw materials in the synthesis of MCM-41, there is no significant difference in crystallinity and pore properties when was compared to material produced from commercial sodium silicate.

  4. Design and synthesis of polyoxometalate-framework materials from cluster precursors (United States)

    Vilà-Nadal, Laia; Cronin, Leroy


    Inorganic oxide materials are used in semiconductor electronics, ion exchange, catalysis, coatings, gas sensors and as separation materials. Although their synthesis is well understood, the scope for new materials is reduced because of the stability limits imposed by high-temperature processing and top-down synthetic approaches. In this Review, we describe the derivatization of polyoxometalate (POM) clusters, which enables their assembly into a range of frameworks by use of organic or inorganic linkers. Additionally, bottom-up synthetic approaches can be used to make metal oxide framework materials, and the features of the molecular POM precursors are retained in these structures. Highly robust all-inorganic frameworks can be made using metal-ion linkers, which combine molecular synthetic control without the need for organic components. The resulting frameworks have high stability, and high catalytic, photochemical and electrochemical activity. Conceptually, these inorganic oxide materials bridge the gap between zeolites and metal-organic frameworks (MOFs) and establish a new class of all-inorganic POM frameworks that can be designed using topological and reactivity principles similar to MOFs.

  5. Synthesis, microstructure and properties of BiFeO{sub 3}-based multiferroic materials: A review

    Energy Technology Data Exchange (ETDEWEB)

    Bernardo, M. S.


    BiFeO{sub 3}-based materials are currently one of the most studied multiferroics due to their possible applications at room temperature. However, among the large number of published papers there is much controversy. For example, possibility of synthesizing a pure BiFeO{sub 3} phase is still source of discussion in literature. Not even the nature of the binary Bi{sub 2}O{sub 3}-Fe{sub 2}O{sub 3} diagram has been clarified yet. The difficulty in controlling the formation of parasite phases reaches the consolidation step. Accordingly, the sintering conditions must be carefully determined both to get dense materials and to avoid bismuth ferrite decomposition. However, the precise conditions to attain dense bismuth ferrite materials are frequently contradictory among different works. As a consequence, the reported properties habitually result opposed and highly irreproducible hampering the preparation of BiFeO{sub 3} materials suitable for practical applications. In this context, the purpose of the present review is to summarize the main researches regarding BiFeO{sub 3} synthesis, microstructure and properties in order to provide an easier understanding of these materials. (Author)

  6. Soft-Templating Synthesis of Mesoporous Silica-Based Materials for Environmental Applications (United States)

    Gunathilake, Chamila Asanka

    Dissertation research is mainly focus on: 1) the development of mesoporous silica materials with organic pendant and bridging groups (isocyanurate, amidoxime, benzene) and incorporated metal (aluminum, zirconium, calcium, and magnesium) species for high temperature carbon dioxide (CO2) sorption, 2) phosphorous-hydroxy functionalized mesoporous silica materials for water treatment, and 3) amidoxime-modified ordered mesoporous silica materials for uranium sorption under seawater conditions. The goal is to design composite materials for environmental applications with desired porosity, surface area, and functionality by selecting proper metal oxide precursors, organosilanes, tetraethylorthosilicate, (TEOS), and block copolymer templates and by adjusting synthesis conditions. The first part of dissertation presents experimental studies on the merge of aluminum, zirconium, calcium, and magnesium oxides with mesoporous silica materials containing organic pendant (amidoxime) and bridging groups (isocyanurate, benzene) to obtain composite sorbents for CO2 sorption at ambient (0-25 °C) and elevated (60-120 °C) temperatures. These studies indicate that the aforementioned composite sorbents are fairly good for CO2 capture at 25 °C via physisorption mechanism and show a remarkably high affinity toward CO2 chemisorption at 60-120 °C. The second part of dissertation is devoted to silica-based materials with organic functionalities for removal of heavy metal ions such as lead from contaminated water and for recovery of metal ions such as uranium from seawater. First, ordered mesoporous organosilica (OMO) materials with diethylphosphatoethyl and hydroxyphosphatoethyl surface groups were examined for Pb2+ adsorption and showed unprecedented adsorption capacities up to 272 mg/g and 202 mg/g, respectively However, the amidoxime-modified OMO materials were explored for uranium extraction under seawater conditions and showed remarkable capacities reaching 57 mg of uranium per gram

  7. Applications of Click Chemistry Reactions to the Synthesis of Functional Materials (United States)

    Accurso, Adrian A.

    This body of work focuses on the production of functional materials using the most reliable carbon-hetoratom bond-forming processes available, which are widely termed "click chemistry" reactions in the literature. This focus on function is enabled by a basis in synthetic chemistry, and where appropriate, brings in techniques from the related fields of materials science and biology to address current needs in those areas. Chapter 1 concerns the in situ production of azide and alkyne-based click chemistry adhesive polymers. Screening of a library of multivalent azides and alkynes was accomplished on a custom-built highthroughput instrument and followed up on a lap-shear testing apparatus. The conductivity of composites made of the adhesive was also explored according to standard methods. The second and third chapters explore the synthesis and function of a family of related [3.3.1]-bicyclononane dichlorides, which we have termed "WCL" electrophiles, and their potential applications for surface functionalization, the synthesis of polycations, and candidate membrane disruptive compounds. The rates of consumption of dichlorides and hydrolysis of model compounds were also explored using NMR, GC-MS, and HPLC-based methods.

  8. Synthesis and comparison of the activities of a catalyst supported on two silicate materials

    Energy Technology Data Exchange (ETDEWEB)

    Vieira, Eduardo G., E-mail: [Departamento de Física e Química, Unesp-Univ Estadual Paulista, Av. Brasil, 56-Centro, Caixa Postal 31, CEP 15385-000, Ilha Solteira, São Paulo (Brazil); Silva, Rafael O.; Carmo, Devaney R. do [Departamento de Física e Química, Unesp-Univ Estadual Paulista, Av. Brasil, 56-Centro, Caixa Postal 31, CEP 15385-000, Ilha Solteira, São Paulo (Brazil); Junior, Enes F. [Departamento de Fitotecnia, Tecnologia de Alimentos e Sócio Economia, Faculdade de Engenharia de Ilha Solteira, Universidade Estadual Paulista, Ilha Solteira, São Paulo (Brazil); Dias Filho, Newton L., E-mail: [Departamento de Física e Química, Unesp-Univ Estadual Paulista, Av. Brasil, 56-Centro, Caixa Postal 31, CEP 15385-000, Ilha Solteira, São Paulo (Brazil); Universidade do Extremo Sul Catarinense, Av. Universitaria, 1105, CP 3167, CEP 88806-000, Criciúma, SC (Brazil)


    The focus of this work is inspecting the synthesis and comparison of the activities of a catalyst supported on two silicate materials in the epoxidation of 1-octene. The two new catalyst materials were characterized by infrared spectroscopy, elemental analysis, solid-state {sup 29}Si and {sup 13}C nuclear magnetic resonance, scanning electronic microscope (SEM) and analysis of nitrogen. Lastly, the two new catalysts, Silsesq-TCA-[(W(CO){sub 3}I{sub 2}){sub 3}] and Silica-TCA-[W(CO){sub 3}I{sub 2}] were tested as catalysts in reactions of epoxidation of 1-octene and compared with their analogue not supported [W(CO){sub 3}I{sub 2}(thiocarbamide)]. After an extensive literature search, we verified that our work is the first that has reported the immobilization process of [W(CO){sub 3}I{sub 2}(NCCH{sub 3}){sub 2}] on silsesquioxane and silica gel functionalized with propyl-thiocarbamide groups and their applications as catalysts of reactions of catalytic epoxidation of 1-octene. - Highlights: • Immobilization of [W(CO){sub 3}I{sub 2}(NCCH{sub 3}){sub 2}] complex onto mesoporous supports. • Synthesis and characterization of new mesoporous catalysts. • The new catalysts exhibit great catalytic activity in the epoxidation of 1-octene. • Recyclable catalysts with excellent reusability and stability.

  9. Solution Synthesis and Processing of PZT Materials for Neutron Generator Applications

    Energy Technology Data Exchange (ETDEWEB)

    Anderson, M.A.; Ewsuk, K.G.; Montoya, T.V.; Moore, R.H.; Sipola, D.L.; Tuttle, B.A.; Voigt, J.A.


    A new solution synthesis route has been developed for the preparation of lead-based ferroelectric materials (patent filed). The process produces controlled stoichiometry precursor powders by non-aqueous precipitation. For a given ferroelectric material to be prepared, a metal acetate/alkoxide solution containing constituent metal species in the appropriate ratio is mixed with an oxalic acid/n-propanol precipitant solution. An oxalate coprecipitate is instantly fonned upon mixing that quantitatively removes the metals from solution. Most of the process development was focused on the synthesis and processing of niobium-substituted lead zirconate titanate with a Zr-to-Ti ratio of 95:5 (PNZT 95/5) that has an application in neutron generator power supplies. The process was scaled to produce 1.6 kg of the PNZT 95/5 powder using either a sen-ii-batch or a continuous precipitation scheme. Several of the PNZT 95/5 powder lots were processed into ceramic slug form. The slugs in turn were processed into components and characterized. The physical properties and electrical performance (including explosive functional testing of the components met the requirements set for the neutron generator application. Also, it has been demonstrated that the process is highly reproducible with respect to the properties of the powders it produces and the properties of the ceramics prepared from its powders. The work described in this report was funded by Sandia's Laboratory Directed Research and Development Program.

  10. Design, Synthesis and Characterization of Functional Metal-Organic Framework Materials

    KAUST Repository

    Alamer, Badriah


    Over the past few decades, vast majority of industrial and academic research throughout the world has witnessed the emergence of materials that can serve as ideal candidates for potential utility in desired applications, and these materials are known as Metal Organic Framework (MOFs). This exceptional new family of porous materials is fabricated by linkage of metal ions or clusters and organic linkers via strong bonds. MOFs have been awarded with remarkable interest and widely studied due to their inherent structural methodology (e.g. use of various metals, expanded library of organic building blocks with different geometry and functionality particularly frameworks designed from carboxylate organic linkers) and unquestionably unique structural and chemical features for many practical applications. (i.e. gas storage/separation, catalysis, drug delivery etc). Simply, metal organic frameworks epitomize the beauty of porous chemical structures. From a design perspective, the introduction of the Molecular Building Block (MBB) approach is actively being pursued pathway by researchers toward the construction of MOFs by employing inorganic building blocks and organic linkers and taking advantage of not only their multiple coordination modes and geometries but also the way in which they are reticulated to generate final framework. In this thesis, research studies will be directed toward (i) the investigation of the relationship between experimental parameters and synthesis of well-known fcu –MOF, (ii) rational design and synthesis of new rare earth (RE) based MOFs, (ii) isoreticular materials based on particular MBB ([M3O(RCO2)6]), M= p-and d-block metals, and (iv) zeolite- like metal organic framework assembled from single-metal ion based MBB ([MN2(CO2)4]) via 2-, 3-,and 4-connected organic linkers. Consequently, the porosity, chemical and thermal stability, and gas sorption properties will be evaluated and detailed.

  11. Nanoselective area growth of GaN by metalorganic vapor phase epitaxy on 4H-SiC using epitaxial graphene as a mask

    Energy Technology Data Exchange (ETDEWEB)

    Puybaret, Renaud; Jordan, Matthew B.; Voss, Paul L.; Ougazzaden, Abdallah, E-mail: [School of Electrical and Computer Engineering, Georgia Institute of Technology, Atlanta, Georgia 30332 (United States); CNRS UMI 2958, Georgia Institute of Technology, 2 Rue Marconi, 57070 Metz (France); Patriarche, Gilles [CNRS, Laboratoire de Photonique et de Nanostructures, Route de Nozay, 91460 Marcoussis (France); Sundaram, Suresh; El Gmili, Youssef [CNRS UMI 2958, Georgia Institute of Technology, 2 Rue Marconi, 57070 Metz (France); Salvestrini, Jean-Paul [Université de Lorraine, CentraleSupélec, LMOPS, EA4423, 57070 Metz (France); Heer, Walt A. de [School of Physics, Georgia Institute of Technology, Atlanta, Georgia 30332 (United States); Berger, Claire [School of Physics, Georgia Institute of Technology, Atlanta, Georgia 30332 (United States); CNRS, Institut Néel, BP166, 38042 Grenoble Cedex 9 (France)


    We report the growth of high-quality triangular GaN nanomesas, 30-nm thick, on the C-face of 4H-SiC using nanoselective area growth (NSAG) with patterned epitaxial graphene grown on SiC as an embedded mask. NSAG alleviates the problems of defects in heteroepitaxy, and the high mobility graphene film could readily provide the back low-dissipative electrode in GaN-based optoelectronic devices. A 5–8 graphene-layer film is first grown on the C-face of 4H-SiC by confinement-controlled sublimation of silicon carbide. Graphene is then patterned and arrays of 75-nm-wide openings are etched in graphene revealing the SiC substrate. A 30-nm-thick GaN is subsequently grown by metal organic vapor phase epitaxy. GaN nanomesas grow epitaxially with perfect selectivity on SiC, in the openings patterned through graphene. The up-or-down orientation of the mesas on SiC, their triangular faceting, and cross-sectional scanning transmission electron microscopy show that they are biphasic. The core is a zinc blende monocrystal surrounded with single-crystal wurtzite. The GaN crystalline nanomesas have no threading dislocations or V-pits. This NSAG process potentially leads to integration of high-quality III-nitrides on the wafer scalable epitaxial graphene/silicon carbide platform.

  12. High growth rate GaN on 200 mm silicon by metal-organic vapor phase epitaxy for high electron mobility transistors (United States)

    Charles, M.; Baines, Y.; Bavard, A.; Bouveyron, R.


    It is increasingly important to reduce the cycle time of epitaxial growth, in order to reduce the costs of device fabrication, especially for GaN based structures which typically have growth cycles of several hours. We have performed a comprehensive study using metal-organic vapor phase epitaxy (MOVPE) investigating the effects of changing GaN growth rates from 0.9 to 14.5 μm/h. Although there is no significant effect on the strain incorporated in the layers, we have seen changes in the surface morphology which can be related to the change in dislocation behaviour and surface diffusion effects. At the small scale, as seen by AFM, increased dislocation density for higher growth rates leads to increased pinning of growth terraces, resulting in more closely spaced terraces. At a larger scale of hundreds of μm observed by optical profiling, we have related the formation of grains to the rate of surface diffusion of adatoms using a random walk model, implying diffusion distances from 30 μm for the highest growth rates up to 100 μm for the lowest. The increased growth rate also increases the intrinsic carbon incorporation which can increase the breakdown voltage of GaN films. Despite an increased threading dislocation density, these very high growth rates of 14.5 μm/hr by MOVPE have been shown to be appealing for reducing epitaxial growth cycle times and therefore costs in High Electron Mobility Transistor (HEMT) structures.

  13. Defect structure of high temperature hydride vapor phase epitaxy-grown epitaxial (0 0 0 1) AlN/sapphire using growth mode modification process (United States)

    Su, Xujun; Zhang, Jicai; Huang, Jun; Zhang, Jinping; Wang, Jianfeng; Xu, Ke


    Defect structures were investigated by transmission electron microscopy for AlN/sapphire (0 0 0 1) epilayers grown by high temperature hydride vapor phase epitaxy using a growth mode modification process. The defect structures, including threading dislocations, inversion domains, and voids, were analyzed by diffraction contrast, high-resolution imaging, and convergent beam diffraction. AlN film growth was initiated at 1450 °C with high V/III ratio for 8 min. This was followed by low V/III ratio growth for 12 min. The near-interfacial region shows a high density of threading dislocations and inversion domains. Most of these dislocations have Burgers vector b = 1/3〈1 1 2 0〉 and were reduced with the formation of dislocation loops. In the middle range 400 nm < h < 2 μm, dislocations gradually aggregated and reduced to ∼109 cm-2. The inversion domains have a shuttle-like shape with staggered boundaries that deviate by ∼ ±5° from the c axis. Above 2 μm thickness, the film consists of isolated threading dislocations with a total density of 8 × 108 cm-2. Most of threading dislocations are either pure edge or mixed dislocations. The threading dislocation reduction in these films is associated with dislocation loops formation and dislocation aggregation-interaction during island growth with high V/III ratio.

  14. Electron mobility enhancement in metalorganic-vapor-phase-epitaxy-grown InAlN high-electron-mobility transistors by control of surface morphology of spacer layer (United States)

    Yamada, Atsushi; Ishiguro, Tetsuro; Kotani, Junji; Nakamura, Norikazu


    We demonstrated low-sheet-resistance metalorganic-vapor-phase-epitaxy-grown InAlN high-electron-mobility transistors using AlGaN spacers with excellent surface morphology. We systematically investigated the effects of AlGaN spacer growth conditions on surface morphology and electron mobility. We found that the surface morphology of InAlN barriers depends on that of AlGaN spacers. Ga desorption from AlGaN spacers was suppressed by increasing the trimethylaluminum (TMA) supply rate, resulting in the small surface roughnesses of InAlN barriers and AlGaN spacers. Moreover, we found that an increase in the NH3 supply rate also improved the surface morphologies of InAlN barriers and AlGaN spacers as long as the TMA supply rate was high enough to suppress the degradation of GaN channels. Finally, we realized a low sheet resistance of 185.5 Ω/sq with a high electron mobility of 1210 cm2 V‑1 s‑1 by improving the surface morphologies of AlGaN spacers and InAlN barriers.

  15. High-quality AlN film grown on a nanosized concave-convex surface sapphire substrate by metalorganic vapor phase epitaxy (United States)

    Yoshikawa, Akira; Nagatomi, Takaharu; Morishita, Tomohiro; Iwaya, Motoaki; Takeuchi, Tetsuya; Kamiyama, Satoshi; Akasaki, Isamu


    We developed a method for fabricating high-crystal-quality AlN films by combining a randomly distributed nanosized concavo-convex sapphire substrate (NCC-SS) and a three-step growth method optimized for NCC-SS, i.e., a 3-nm-thick nucleation layer (870 °C), a 150-nm-thick high-temperature layer (1250 °C), and a 3.2-μm-thick medium-temperature layer (1110 °C). The NCC-SS is easily fabricated using a conventional metalorganic vapor phase epitaxy reactor equipped with a showerhead plate. The resultant AlN film has a crack-free and single-step surface with a root-mean-square roughness of 0.5 nm. The full-widths at half-maxima of the X-ray rocking curve were 50/250 arcsec for the (0002)/(10-12) planes, revealing that the NCC surface is critical for achieving such a high-quality film. Hexagonal-pyramid-shaped voids at the AlN/NCC-SS interface and confinement of dislocations within the 150-nm-thick high-temperature layer were confirmed. The NCC surface feature and resultant faceted voids play an important role in the growth of high-crystal-quality AlN films, likely via localized and/or disordered growth of AlN at the initial stage, contributing to the alignment of high-crystal-quality nuclei and dislocations.

  16. Nanoselective area growth of GaN by metalorganic vapor phase epitaxy on 4H-SiC using epitaxial graphene as a mask (United States)

    Puybaret, Renaud; Patriarche, Gilles; Jordan, Matthew B.; Sundaram, Suresh; El Gmili, Youssef; Salvestrini, Jean-Paul; Voss, Paul L.; de Heer, Walt A.; Berger, Claire; Ougazzaden, Abdallah


    We report the growth of high-quality triangular GaN nanomesas, 30-nm thick, on the C-face of 4H-SiC using nanoselective area growth (NSAG) with patterned epitaxial graphene grown on SiC as an embedded mask. NSAG alleviates the problems of defects in heteroepitaxy, and the high mobility graphene film could readily provide the back low-dissipative electrode in GaN-based optoelectronic devices. A 5-8 graphene-layer film is first grown on the C-face of 4H-SiC by confinement-controlled sublimation of silicon carbide. Graphene is then patterned and arrays of 75-nm-wide openings are etched in graphene revealing the SiC substrate. A 30-nm-thick GaN is subsequently grown by metal organic vapor phase epitaxy. GaN nanomesas grow epitaxially with perfect selectivity on SiC, in the openings patterned through graphene. The up-or-down orientation of the mesas on SiC, their triangular faceting, and cross-sectional scanning transmission electron microscopy show that they are biphasic. The core is a zinc blende monocrystal surrounded with single-crystal wurtzite. The GaN crystalline nanomesas have no threading dislocations or V-pits. This NSAG process potentially leads to integration of high-quality III-nitrides on the wafer scalable epitaxial graphene/silicon carbide platform.

  17. Interruption-free growth of 10 μm-thick GaN film prepared on sputtered AlN/PSS template by hydride vapor phase epitaxy (United States)

    Chen, Y. A.; Kuo, C. H.; Wu, J. P.; Chang, C. W.


    GaN films (10 μm-thick) of high crystalline quality were prepared on sputtered AlN/PSS template by hydride vapor phase epitaxy (HVPE). By introducing the two-step growth method into HVPE, one can reduce the steps in the procedure, realize uninterrupted growth, and improve the crystal quality of the films. The effects of initial GaN growth on the AlN/PSS template by HVPE were also investigated. In this study, 10 μm-thick GaN films prepared on sputtered AlN/PSS template by HVPE showed improved crystal quality using X-ray diffraction and etching pits density. Compared with conventional undoped GaN film grown by metal organic chemical vapor deposition, the full width at half maximum of the (0 0 2) and (1 0 2) peaks of GaN decreased from 450 arcsec to 290 arcsec and from 376 arcsec to 344 arcsec, respectively. Transmission electron microscopy results showed that the gaps observed between the convex regions would eventually turn into dislocations during coalescence, because the number of dislocations increased with the number of gaps observed between the convex regions after step-1 growth.

  18. Low-temperature growth of AlN and GaN by metal organic vapor phase epitaxy for polarization engineered water splitting photocathode (United States)

    Nakamura, Akihiro; Suzuki, Michihiro; Fujii, Katsushi; Nakano, Yoshiaki; Sugiyama, Masakazu


    Crystal properties of low-temperature grown AlN (LT-AlN) combined with low temperature GaN (LT-GaN) grown by metal organic vapor phase epitaxy (MOVPE) were investigated to obtain a high quality GaN/AlN/GaN structure with a few-nm-thick AlN layer. LT-AlN suppresses unintentional Ga incorporation and can be pseudomorphically grown on GaN with a relatively smooth surface morphology. The lattice of LT-AlN coherent to GaN, however, was found to relax after reactor conditions were changed to grow the subsequent GaN layer at higher temperature. The top GaN layer grown on the relaxed LT-AlN, thus, exhibited a rough surface morphology and a threading dislocation density (TDD) higher than 109 cm-2 estimated from an X-ray diffraction measurement. An LT-GaN capping layer was found to be highly effective for avoiding such lattice relaxation of LT-AlN. The combination of LT-AlN and LT-GaN enables us to obtain a GaN/AlN/GaN junction with high Al content, a low TDD, and abrupt interfaces. As a result, introducing an LT-GaN layer improved the photoelectrochemical (PEC) property of a polarization engineered un-doped GaN/AlN/n-type GaN (u-GaN/AlN/n-GaN) photocathode for water splitting.

  19. Highly c-axis-oriented one-inch square freestanding GaN grown by hydride vapor-phase epitaxy using an AIN deposited on Si

    CERN Document Server

    Lee, M H; Chung, S H; Moon, D C


    In this letter, we report on the growth and the properties of freestanding GaN substrates. Large areas of one-inch square with a thickness of a 0.5 mm were grown by the hydride vapor-phase epitaxy (HVPE) method after a thick film of GaN was grown on an AIN buffer layer deposited on a sacrificial Si substrate which was subsequently chemically removed. The GaN substrate showed intensified X-ray diffraction from the (00.2) and the (00.4) planes, and the full width at half maximum of the double-crystal X-ray diffraction curve was as large as 4.2 degrees. The photoluminescence spectra measured at 10 K and at 300 K exhibited a sharp and strong excitonic emission without deep-level emission. They also showed n-type conduction with an electron concentration of approx 1x10 sup 1 sup 8 cm sup - sup 3 and a Hall mobility of 50 cm sup 2 / Vsec. The highly c-axis oriented large-area freestanding GaN prepared using a Si sacrificial substrate by HVPE through this work can be used for homoepitaxial growth of GaN-based optoel...

  20. Influence of incoherent twin boundaries on the electrical properties of β-Ga2O3 layers homoepitaxially grown by metal-organic vapor phase epitaxy (United States)

    Fiedler, A.; Schewski, R.; Baldini, M.; Galazka, Z.; Wagner, G.; Albrecht, M.; Irmscher, K.


    We present a quantitative model that addresses the influence of incoherent twin boundaries on the electrical properties in β-Ga2O3. This model can explain the mobility collapse below a threshold electron concentration of 1 × 1018 cm-3 as well as partly the low doping efficiency in β-Ga2O3 layers grown homoepitaxially by metal-organic vapor phase epitaxy on (100) substrates of only slight off-orientation. A structural analysis by transmission electron microscopy (TEM) reveals a high density of twin lamellae in these layers. In contrast to the coherent twin boundaries parallel to the (100) plane, the lateral incoherent twin boundaries exhibit one dangling bond per unit cell that acts as an acceptor-like electron trap. Since the twin lamellae are thin, we consider the incoherent twin boundaries to be line defects with a density of 1011-1012 cm-2 as determined by TEM. We estimate the influence of the incoherent twin boundaries on the electrical transport properties by adapting Read's model of charged dislocations. Our calculations quantitatively confirm that the mobility reduction and collapse as well as partly the compensation are due to the presence of twin lamellae.

  1. High-pressure vapor-phase hydrodeoxygenation of lignin-derived oxygenates to hydrocarbons by a PtMo bimetallic catalyst: Product selectivity, reaction pathway, and structural characterization

    Energy Technology Data Exchange (ETDEWEB)

    Yohe, Sara L.; Choudhari, Harshavardhan J.; Mehta, Dhairya D.; Dietrich, Paul J.; Detwiler, Michael D.; Akatay, Cem M.; Stach, Eric A.; Miller, Jeffrey T.; Delgass, W. Nicholas; Agrawal, Rakesh; Ribeiro, Fabio H.


    High-pressure, vapor-phase, hydrodeoxygenation (HDO) reactions of dihydroeugenol (2-methoxy-4-propylphenol), as well as other phenolic, lignin-derived compounds, were investigated over a bimetallic platinum and molybdenum catalyst supported on multi-walled carbon nanotubes (5%Pt2.5%Mo/MWCNT). Hydrocarbons were obtained in 100% yield from dihydroeugenol, including 98% yield of the hydrocarbon propylcyclohexane. The final hydrocarbon distribution was shown to be a strong function of hydrogen partial pressure. Kinetic analysis showed three main dihydroeugenol reaction pathways: HDO, hydrogenation, and alkylation. The major pathway occurred via Pt catalyzed hydrogenation of the aromatic ring and methoxy group cleavage to form 4-propylcyclohexanol, then Mo catalyzed removal of the hydroxyl group by dehydration to form propylcyclohexene, followed by hydrogenation of propylcyclohexene on either the Pt or Mo to form the propylcyclohexane. Transalkylation by the methoxy group occurred as a minor side reaction. Catalyst characterization techniques including chemisorption, scanning transmission electron microscopy, X-ray absorption spectroscopy, and X-ray photoelectron spectroscopy were employed to characterize the catalyst structure. Catalyst components identified were Pt particles, bimetallic PtMo particles, a Mo carbide-like phase, and Mo oxide phases.

  2. Modelling and numerical simulation of liquid-vapor phase transitions; Modelisation et simulation numerique des transitions de phase liquide-vapeur

    Energy Technology Data Exchange (ETDEWEB)

    Caro, F


    This work deals with the modelling and numerical simulation of liquid-vapor phase transition phenomena. The study is divided into two part: first we investigate phase transition phenomena with a Van Der Waals equation of state (non monotonic equation of state), then we adopt an alternative approach with two equations of state. In the first part, we study the classical viscous criteria for selecting weak solutions of the system used when the equation of state is non monotonic. Those criteria do not select physical solutions and therefore we focus a more recent criterion: the visco-capillary criterion. We use this criterion to exactly solve the Riemann problem (which imposes solving an algebraic scalar non linear equation). Unfortunately, this step is quite costly in term of CPU which prevent from using this method as a ground for building Godunov solvers. That is why we propose an alternative approach two equations of state. Using the least action principle, we propose a phase changing two-phase flow model which is based on the second thermodynamic principle. We shall then describe two equilibrium submodels issued from the relaxations processes when instantaneous equilibrium is assumed. Despite the weak hyperbolicity of the last sub-model, we propose stable numerical schemes based on a two-step strategy involving a convective step followed by a relaxation step. We show the ability of the system to simulate vapor bubbles nucleation. (author)

  3. Growth of InGaAs nanowires on Ge(111) by selective-area metal-organic vapor-phase epitaxy (United States)

    Yoshida, Akinobu; Tomioka, Katsuhiro; Ishizaka, Fumiya; Motohisa, Junichi


    We report the growth of InGaAs nanowires (NWs) on Ge(111) substrates using selective-area metal-organic vapor-phase epitaxy (SA-MOVPE) for novel InGaAs/Ge hybrid complementary metal-oxide-semiconductor (CMOS) applications. Ge(111) substrates with periodic arrays of mask opening were prepared, and InGaAs was selectively grown on the opening region of Ge(111). A uniform array of InGaAs NWs with a diameter around 100 nm was successfully grown using appropriate preparation of the initial surfaces with an AsH3 thermal treatment and flow-rate modulation epitaxy (FME). We found that optimizing partial pressure of AsH3 and the number of FME cycles improved the yield of vertical InGaAs NWs. Line-scan profile analysis of energy dispersive X-ray (EDX) spectrometry showed that the In composition in the InGaAs NW was almost constant from the bottom to the top. Transmission electron microscope (TEM) analysis revealed that the interface between InGaAs NW and Ge had misfit dislocations, but their distance was longer than that expected from the difference in their lattice constants.

  4. Hall-effect measurements of metalorganic vapor-phase epitaxy-grown p-type homoepitaxial GaN layers with various Mg concentrations (United States)

    Horita, Masahiro; Takashima, Shinya; Tanaka, Ryo; Matsuyama, Hideaki; Ueno, Katsunori; Edo, Masaharu; Takahashi, Tokio; Shimizu, Mitsuaki; Suda, Jun


    Mg-doped p-type gallium nitride (GaN) layers with doping concentrations in the range from 6.5 × 1016 cm-3 (lightly doped) to 3.8 × 1019 cm-3 (heavily doped) were investigated by Hall-effect measurement for the analysis of hole concentration and mobility. p-GaN was homoepitaxially grown on a GaN free-standing substrate by metalorganic vapor-phase epitaxy. The threading dislocation density of p-GaN was 4 × 106 cm-2 measured by cathodoluminescence mapping. Hall-effect measurements of p-GaN were carried out at a temperature in the range from 130 to 450 K. For the lightly doped p-GaN, the acceptor concentration of 7.0 × 1016 cm-3 and the donor concentration of 3.2 × 1016 cm-3 were obtained, where the compensation ratio was 46%. We also obtained the depth of the Mg acceptor level to be 220 meV. The hole mobilities of 86, 31, 14 cm2 V-1 s-1 at 200, 300, 400 K, respectively, were observed in the lightly doped p-GaN.

  5. Synthesis of magnetic and multiferroic materials from polyvinyl alcohol-based gels

    Energy Technology Data Exchange (ETDEWEB)

    Lisnevskaya, I.V.; Bobrova, I.A.; Lupeiko, T.G.


    This review article summarizes results on the synthesis of the magnetic materials including modified nickel ferrite (Ni{sub 0.9}Co{sub 0.1}Cu{sub 0.1}Fe{sub 1.9}O{sub 4−δ}), yttrium iron garnet (Y{sub 3}Fe{sub 5}O{sub 12}), lanthanum-containing manganites (M{sub x}La{sub 1−x}MnO{sub 3} (M=Pb, Ba or Sr; x=0.3−0.35)), and multiferroics (BiFeO{sub 3} and BiFe{sub 0.5}Mn{sub 0.5}O{sub 3}) from polyvinyl alcohol-based gels. It is shown that the ammonium nitrate accelerates destruction of organic components of xerogels and thus Ni{sub 0.9}Co{sub 0.1}Cu{sub 0.1}Fe{sub 1.9}O{sub 4−δ} and BiFeO{sub 3} can be prepared at record low temperatures (100 and 250 °C, respectively) which are 200–300 °C lower compared to the process where air is used as an oxidizing agent. As for the synthesis of Y{sub 3}Fe{sub 5}O{sub 12}, M{sub x}La{sub 1−x}MnO{sub 3} and BiFe{sub 0.5}Mn{sub 0.5}O{sub 3}, the presence of NH{sub 4}NO{sub 3} favors formation of foreign phases, which ultimately complicate reaction mechanisms and lead to the higher temperature to synthesize target products. Developed methods provide nanoscale magnetic and multiferroic materials with an average particle size of ∼20–50 nm. - Highlights: • This review summarizes results on the synthesis of the magnetic materials and multiferroics. • Ammonium nitrate accelerates destruction of organic components of xerogels. • Ni{sub 0.9}Co{sub 0.1}Cu{sub 0.1}Fe{sub 1.9}O{sub 4−δ} and BiFeO{sub 3} can be prepared at record low temperatures. • Developed methods provide nanoscale magnetic and multiferroic materials.

  6. Continuous-Flow Synthesis and Materials Interface Engineering of Lead Sulfide Quantum Dots for Photovoltaic Applications

    KAUST Repository

    El-Ballouli, Ala’a O.


    Harnessing the Sun’s energy via the conversion of solar photons to electricity has emerged as a sustainable energy source to fulfill our future demands. In this regard, solution-processable, size-tunable PbS quantum dots (QDs) have been identified as a promising active materials for photovoltaics (PVs). Yet, there are still serious challenges that hinder the full exploitation of QD materials in PVs. This dissertation addresses two main challenges to aid these QDs in fulfilling their tremendous potential in PV applications. First, it is essential to establish a large-scale synthetic technique which maintains control over the reaction parameters to yield QDs with well-defined shape, size, and composition. Rigorous protocols for cost-effective production on a scale are still missing from literature. Particularly, previous reports of record-performance QD-PVs have been based on small-scale, manual, batch syntheses. One way to achieve a controlled large-scale synthesis is by reducing the reaction volume to ensure uniformity. Accordingly, we design a droplet-based continuous-flow synthesis of PbS QDs. Only upon separating the nucleation and growth phases, via a dual-temperature-stage reactor, it was possible to achieve high-quality QDs with high photoluminescence quantum yield (50%) in large-scale. The performance of these QDs in a PV device was comparable to batch-synthesized QDs, thus providing a promise in utilizing automated synthesis of QDs for PV applications. Second, it is crucial to study and control the charge transfer (CT) dynamics at QD interfaces in order to optimize their PV performance. Yet, the CT investigations based on PbS QDs are limited in literature. Here, we investigate the CT and charge separation (CS) at size-tunable PbS QDs and organic acceptor interfaces using a combination of femtosecond broadband transient spectroscopic techniques and steady-state measurements. The results reveal that the energy band alignment, tuned by the quantum

  7. Synthesis and characterization of hydroxyapatite-gelatine composite materials for orthopaedic application

    Energy Technology Data Exchange (ETDEWEB)

    Yanovska, A., E-mail: [Institute of Applied Physics, National Academy of Sciences of Ukraine, 58 Petropavlovskaya Str., 40000, Sumy (Ukraine); Sumy State University, Ministry of Education and Science of Ukraine, 2 R. Korsakova Str., 40007, Sumy (Ukraine); Kuznetsov, V. [Institute of Applied Physics, National Academy of Sciences of Ukraine, 58 Petropavlovskaya Str., 40000, Sumy (Ukraine); Sumy State University, Ministry of Education and Science of Ukraine, 2 R. Korsakova Str., 40007, Sumy (Ukraine); Stanislavov, A. [Institute of Applied Physics, National Academy of Sciences of Ukraine, 58 Petropavlovskaya Str., 40000, Sumy (Ukraine); Husak, E. [Institute of Applied Physics, National Academy of Sciences of Ukraine, 58 Petropavlovskaya Str., 40000, Sumy (Ukraine); Sumy State University, Ministry of Education and Science of Ukraine, 2 R. Korsakova Str., 40007, Sumy (Ukraine); Pogorielov, M. [Sumy State University, Ministry of Education and Science of Ukraine, 2 R. Korsakova Str., 40007, Sumy (Ukraine); Starikov, V. [National Technical University ”Kharkov Polytechnic Institute”, 21 Frunze Str., 61002, Kharkov (Ukraine); Bolshanina, S. [Sumy State University, Ministry of Education and Science of Ukraine, 2 R. Korsakova Str., 40007, Sumy (Ukraine); Danilchenko, S. [Institute of Applied Physics, National Academy of Sciences of Ukraine, 58 Petropavlovskaya Str., 40000, Sumy (Ukraine)


    The composite materials based on hydroxyapatite (HA) and gelatine (Gel) with addition of silver and zirconium oxide were obtained. The study investigates a combination of low powered ultrasonic irradiation and low concentration of gelatine in the co-precipitation synthesis. These composites have different weight ratios of organic/inorganic components and may be synthesized in two ways: simple mixing and co-precipitation. Both of which were compared. The estimation of porosity, in vivo testing, surface morphology and phase composition as well as the IR-analysis were provided. Hydroxyapatite was the main crystalline phase in obtained composites. While around powdered HA-Gel composite the connective tissue capsule is formed without bone tissue formation, HA-Gel-Ag porous composite implantation leads to formation of new bone tissue and activation of cell proliferation. Addition of silver ions into composite material allows decreasing inflammation on the first stage of implantation and has positive effect on bone tissue formation. Some of the obtained composite materials containing silver or ZrO{sub 2} are biocompatible. bio-resorbable and osteoconductive with high level of porosity (75–85%). - Highlights: • Hydroxyapatite-gelatine composites with addition of Ag{sup +} and ZrO{sub 2} were obtained. • Composites were synthesized in two ways: simple mixing and co-precipitation. • Co-precipitation synthesis combined ultrasonic treatment and low concentration of gelatine. • Obtained composites have different weight ratios of organic/inorganic components. • Some composites are osteoconductive and all of them have high level of porosity (75–85%).

  8. Optimization on electrochemical synthesis of HKUST-1 as candidate catalytic material for Green diesel production (United States)

    Lestari, W. W.; Nugraha, R. E.; Winarni, I. D.; Adreane, M.; Rahmawati, F.


    In the effort to support the discovery of new renewable energy sources in Indonesia, biofuel is one of promising options. The conversion of vegetable oil into ready-biofuel, especially green diesel, needs several steps, one of which is a hydrogenation or hydro-deoxygenation reaction. In this case, the catalyst plays a very important role regarding to its activity and selectivity, and Metal-Organic Frameworks (MOFs) becoming a new generation of heterogeneous catalyst in this area. In this research, a preliminary study to optimize electrochemical synthesis of the catalytic material based on MOFs, namely HKUST-1 [Cu3(BTC)2], has been conducted. Some electrochemical reaction parameters were tested, for example by modifying the electrochemical synthetic conditions, i.e. by performing variation of voltages (12, 13, 14, and 15 Volt), temperatures (RT, 40, 60, and 80 °C) and solvents (ethanol, water, methanol and dimethyl-formamide (DMF)). Material characterization was carried out by XRD, SEM, FTIR, DTA/TG and SAA. The results showed that the optimum synthetic conditions of HKUST-1 are performed at room temperature in a solvent combination of water: ethanol (1: 1) and a voltage of 15 Volt for 2 hours. The XRD-analysis revealed that the resulted peaks are identical to the simulated powder pattern generated from single crystal data and comparable to the peaks of solvothermal method. However, the porosity of the resulting material through electrochemical method is still in the range of micro-pore according to IUPAC and 50% smaller than the porosity resulted from solvothermal synthesis. The corresponding compounds are thermally stable until 300 °C according to TG/DTA.

  9. Synthesis of nanodispersed filler for polymer composite materials of thermostatic purpose

    Directory of Open Access Journals (Sweden)

    PAVLENKO Vyacheslav Ivanovich


    Full Text Available The paper presents data on the synthesis of nanosized filler for nonpolar polymer matrix. Aqueous solution of sodium methylsiliconate with empirical formula CH3–Si(OH2ONa was used as the base component for the synthesis of nanosized filler. The production process of filler consists of several stages, these are the main ones: synthesizing of gel that was obtained in gel formation from sol colloidal solution – transformation of free-dispersed system (sol into connected-dispersed one; gel precipitation by centrifugation and washing from ion Na+; gel drying at temperature of 100оC to obtain a powder filler; dispersion in the mill to the particle size of 0,1–1 microns. To destroy globules and diminish particle size to nanoscale level the obtained material was exposed to dispersion in planetary mill with further sonication (22 Hz. To study the obtained filler X-ray, differential thermal and microscopic methods have been used. For quantification of colloidal component (nanoparticles in the suspension the centrifugation method was used at high speeds. It has been determined that the content of nanoparticles (up to 200 nm in the obtained substance is about 10%. Damping edge angle of the obtained material is 110–120оC, that shows high hydrophobic properties of the synthesized powder. The obtained material possesses high dispersiveness, hydrophobicity and silicone frame resistant to the temperature range up to 531оC (there are no significant chemical transformations except dealkylation and dehydration reactions. Thermal degradation of the synthesized filler distinctly observed at the temperaturemore than 531оC.

  10. Synthesis of Disentangled Ultra-High Molecular Weight Polyethylene: Influence of Reaction Medium on Material Properties

    Directory of Open Access Journals (Sweden)

    Giuseppe Forte


    Full Text Available The polymerization of ethylene to Ultra-High Molecular Weight Polyethylene (UHMWPE in certain reaction conditions allows synthesis of nascent powders with a considerably lower amount of entanglements: the material obtained is of great interest from both academic and industrial viewpoints. From an academic point of view, it is interesting to follow the evolution of the metastable melt state with the progressive entanglements formation. Industrially, it is valuable to have a solvent-free processing route for the production of high modulus, high strength tapes. Since the polymer synthesis is performed in the presence of a solvent, it is interesting to investigate the influence that the reaction medium can have on the catalyst activity, resultant molecular characteristics, and polymer morphology at the macroscopic as wells as microscopic level. In this paper, we present the effect that two typical polymerization solvents, toluene and heptane, and mixtures of them, have on the catalytic performance and on the polymer properties. The observations are that an unexpected increase of catalyst activity, accompanied by a significant improvement in mechanical properties, is found when using a carefully chosen mixture of solvents. A tentative explanation is given on the basis of the presented results.

  11. Plasmachemical Synthesis of Nanopowders in the System Ti(O,C,N for Material Structure Modification

    Directory of Open Access Journals (Sweden)

    Michael Filkov


    Full Text Available Refractory nanoparticles are finding broad application in manufacturing of materials with enhanced physical properties. Production of carbide, nitride, and carbonitride nanopowders in high volumes is possible in the multijet plasmachemical reactor, where temperature and velocity distributions in reaction zone can be controlled by plasma jet collision angle and mixing chamber geometry. A chemical reactor with three Direct Current (DC arc plasma jets intersecting at one point was applied for titanium carbonitride synthesis from titanium dioxide, propane-butane mixture, and nitrogen. The influence of process operational parameters on the product chemical and phase composition was investigated. Mixing conditions in the plasma jet collision zone, particles residence time, and temperatures were evaluated with the help of Computational Fluid Dynamics (CFD simulations. The synthesized nanoparticles have predominantly cubic shape and dimensions in the range 10–200 nm. Phase compositions were represented by oxycarbonitride phases. The amount of free (not chemically bonded carbon in the product varied in the range 3–12% mass, depending on synthesis conditions.

  12. Controlled gas–liquid interfacial plasmas for synthesis of nano-bio-carbon conjugate materials (United States)

    Kaneko, Toshiro; Hatakeyama, Rikizo


    Plasmas generated in contact with a liquid have been recognized to be a novel reactive field in nano-bio-carbon conjugate creation because several new chemical reactions have been yielded at the gas–liquid interface, which were induced by the physical dynamics of non-equilibrium plasmas. One is the ion irradiation to a liquid, which caused the spatially selective dissociation of the liquid and the generation of additive reducing and oxidizing agents, resulting in the spatially controlled synthesis of nanostructures. The other is the electron irradiation to a liquid, which directly enhanced the reduction action at the plasma–liquid interface, resulting in temporally controlled nanomaterial synthesis. Using this novel reaction field, gold nanoparticles with controlled interparticle distance were synthesized using carbon nanotubes as a template. Furthermore, nanoparticle–biomolecule conjugates and nanocarbon–biomolecule conjugates were successfully synthesized by an aqueous-solution contact plasma and an electrolyte plasma, respectively, which were rapid and low-damage processes suitable for nano-bio-carbon conjugate materials.

  13. High pressure synthesis of novel, zeolite based nano-composite materials (United States)

    Santoro, Mario


    Meso/micro-porous solids such as zeolites are complex materials exhibiting an impressive range of applications, including molecular sieve, gas storage, catalysis, electronics and photonics. We used these materials, particularly non catalytic zeolites in an entirely different fashion. In fact, we performed high pressure (0.5-30 GPa) chemical reactions of simple molecules on a sub-nanometer scale in the channels of a pure SiO2 zeolite, silicalite to obtain unique nano-composite materials with drastically modified physical and chemical properties. Our material investigations are based on a combination of X-ray diffraction and optical spectroscopy techniques in the diamond anvil cell. I will first briefly show how silicalite can be easily filled by simple molecules such as Ar, CO2 and C2H4 among others from the fluid phase at high pressures, and how this efficient filling removes the well known pressure induced amorphization of the silica framework (Haines et al., JACS 2010). I will then present on a silicon carbonate crystalline phase synthesized by reacting silicalite and molecular CO2 that fills the nano-pores, at 18-26 GPa and 600-980 K; after the synthesis the compound is temperature quenched and it results to be slightly metastable at room conditions (Santoro et al., PNAS 2011). On the other hand, a stable at room condition spectacular crystalline nano-composite is obtained by photo-polymerizing ethylene at 0.5-1.5 GPa under UV (351-364 nm) irradiation in the channels of silicalite (Santoro et al., Nat. Commun, in press 2013). For this composite we obtained a structure with single polyethylene chains adapting very well to the confining channels, which results in significant increases in bulk modulus and density, and the thermal expansion coefficient changes sign from negative to positive with respect to the original silicalite host. Mechanical properties may thus be tuned by varying the amount of polymerized ethylene. We then think our findings could allow the

  14. Maximizing hysteretic losses in magnetic ferrite nanoparticles via model-driven synthesis and materials optimization. (United States)

    Chen, Ritchie; Christiansen, Michael G; Anikeeva, Polina


    This article develops a set of design guidelines for maximizing heat dissipation characteristics of magnetic ferrite MFe2O4 (M = Mn, Fe, Co) nanoparticles in alternating magnetic fields. Using magnetic and structural nanoparticle characterization, we identify key synthetic parameters in the thermal decomposition of organometallic precursors that yield optimized magnetic nanoparticles over a wide range of sizes and compositions. The developed synthetic procedures allow for gram-scale production of magnetic nanoparticles stable in physiological buffer for several months. Our magnetic nanoparticles display some of the highest heat dissipation rates, which are in qualitative agreement with the trends predicted by a dynamic hysteresis model of coherent magnetization reversal in single domain magnetic particles. By combining physical simulations with robust scalable synthesis and materials characterization techniques, this work provides a pathway to a model-driven design of magnetic nanoparticles tailored to a variety of biomedical applications ranging from cancer hyperthermia to remote control of gene expression.

  15. Nanocomposite materials based on hydroxyapatite and sodium alginate: synthesis and characteristics

    Directory of Open Access Journals (Sweden)

    О. О. Мартинюк


    Full Text Available This work is devoted to the development and optimization of the synthesis methodof nanostructured biopolymer-apatite composite materials for medical applications with different ratios of polymer (sodium alginate, SA and inorganic (hydroxyapatite, HA phases and research their properties. Composition, structure and morphology of the samples by FTIR spectroscopy, X-ray diffraction and transmission electron microscopy (TEM were characterized. Porosity, degree of swelling and in vitro response on bioactivity in physiological solution obtained compositesweredetermined. The formation in the presence of sodium alginate hydroxyapatite phase with needle structure and average crystallite size 23 nm with simultaneous formation biopolymer matrix due to the interaction of positively charged calcium ions (Ca2+ and negatively charged carboxyl groups (COO- by instrumental methodswasconfirmed. The pH changing of physiological solution in the presence of samples testifies their bioactivit

  16. Rare earth based nanostructured materials: synthesis, functionalization, properties and bioimaging and biosensing applications

    Directory of Open Access Journals (Sweden)

    Escudero Alberto


    Full Text Available Rare earth based nanostructures constitute a type of functional materials widely used and studied in the recent literature. The purpose of this review is to provide a general and comprehensive overview of the current state of the art, with special focus on the commonly employed synthesis methods and functionalization strategies of rare earth based nanoparticles and on their different bioimaging and biosensing applications. The luminescent (including downconversion, upconversion and permanent luminescence and magnetic properties of rare earth based nanoparticles, as well as their ability to absorb X-rays, will also be explained and connected with their luminescent, magnetic resonance and X-ray computed tomography bioimaging applications, respectively. This review is not only restricted to nanoparticles, and recent advances reported for in other nanostructures containing rare earths, such as metal organic frameworks and lanthanide complexes conjugated with biological structures, will also be commented on.

  17. Rare earth based nanostructured materials: synthesis, functionalization, properties and bioimaging and biosensing applications (United States)

    Escudero, Alberto; Becerro, Ana I.; Carrillo-Carrión, Carolina; Núñez, Nuria O.; Zyuzin, Mikhail V.; Laguna, Mariano; González-Mancebo, Daniel; Ocaña, Manuel; Parak, Wolfgang J.


    Rare earth based nanostructures constitute a type of functional materials widely used and studied in the recent literature. The purpose of this review is to provide a general and comprehensive overview of the current state of the art, with special focus on the commonly employed synthesis methods and functionalization strategies of rare earth based nanoparticles and on their different bioimaging and biosensing applications. The luminescent (including downconversion, upconversion and permanent luminescence) and magnetic properties of rare earth based nanoparticles, as well as their ability to absorb X-rays, will also be explained and connected with their luminescent, magnetic resonance and X-ray computed tomography bioimaging applications, respectively. This review is not only restricted to nanoparticles, and recent advances reported for in other nanostructures containing rare earths, such as metal organic frameworks and lanthanide complexes conjugated with biological structures, will also be commented on.

  18. Recent progress in layered double hydroxide based materials for electrochemical capacitors: design, synthesis and performance. (United States)

    Zhao, Mingming; Zhao, Qunxing; Li, Bing; Xue, Huaiguo; Pang, Huan; Chen, Changyun


    As representative two-dimensional (2D) materials, layered double hydroxides (LDHs) have received increasing attention in electrochemical energy storage and conversion because of the facile tunability between their composition and morphology. The high dispersion of active species in layered arrays, the simple exfoliation into monolayer nanosheets and chemical modification offer the LDHs an opportunity as active electrode materials in electrochemical capacitors (ECs). LDHs are favourable in providing large specific surface areas, good transport features as well as attractive physicochemical properties. In this review, our purpose is to provide a detailed summary of recent developments in the synthesis and electrochemical performance of the LDHs. Their composites with carbon (carbon quantum dots, carbon black, carbon nanotubes/nanofibers, graphene/graphene oxides), metals (nickel, platinum, silver), metal oxides (TiO2, Co3O4, CuO, MnO2, Fe3O4), metal sulfides/phosphides (CoS, NiCo2S4, NiP), MOFs (MOF derivatives) and polymers (PEDOT:PSS, PPy (polypyrrole), P(NIPAM-co-SPMA) and PET) are also discussed in this review. The relationship between structures and electrochemical properties as well as the associated charge-storage mechanisms is discussed. Moreover, challenges and prospects of the LDHs for high-performance ECs are presented. This review sheds light on the sustainable development of ECs with LDH based electrode materials.

  19. Coordination Covalent Frameworks: A New Route for Synthesis and Expansion of Functional Porous Materials

    Energy Technology Data Exchange (ETDEWEB)

    Elsaidi, Sameh K.; Mohamed, Mona H.; Loring, John S.; McGrail, Bernard. Pete; Thallapally, Praveen K.


    The synthetic approaches for fine-tuning the structural properties of coordination polymers or metal organic frameworks have exponentially grown during the last decade. This is due to the control over the properties of the resulting structures such as stability, pore size, pore chemis-try and surface area for myriad possible applications. Herein, we present a new class of porous materials called Covalent Coordination Frameworks (CCFs) that were designed and effectively synthesized using a two-step reticular chemistry approach. During the first step, trigonal prismatic molecular building block was isolated using 4-aminobenazoic acid and Cr (III) salt, subsequently in the second step the polymerization of the isolated molecular building blocks (MBBs) takes place by the formation of strong covalent bonds where small organic molecules can connect the MBBs forming extended porous CCF materials. All the isolated CCFs were found to be permanently porous while the discrete MBB were non-porous. This approach would inevitably open a feasible path for the applications of reticular chemistry and the synthesis of novel porous materials with various topologies under ambient conditions using simple organic molecules and versatile MBBs with different functionalities which would not be possible using the traditional one step approach

  20. Properties and potential applications of zeolitic materials produced from fly ash using simple method of synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Arkadiusz Derkowski; Wojciech Franus; Elzbieta Beran; Adriana Czimerova [Polish Academy of Sciences, Krakow (Poland). Institute of Geological Sciences


    Very low energy-consuming procedure is proposed for synthesis of zeolitic materials from fly ash. Three different zeolite materials (X, P and S), rich in zeolite phases, Na-X (FAU), NaP1 (GIS) and sodalite (SOD) were produced from F-class fly ash, using NaOH and NaCl solutions under atmospheric pressure at temperature below 110{sup o}C. Obtained zeolitic products were analysed for their composition and physicochemical properties then compared to the raw fly ash and commercial adsorbents. The zeolitization results in a significant increase of CEC (from 5.5 up to 239 meq 100 g{sup -1}), and the high ability to adsorb heavy metal ions (over 40 mg g{sup -1}) and retain complex and organic molecules (EGME), mostly evident for material X. Adsorptive purification of waste and working lubricating oils using zeolitic products allow to provide their commercial applications in petroleum industry. Leachability of toxic elements after standard post-reaction washing is environmentally safe.

  1. Geometric Shape Regulation and Noncovalent Synthesis of One-Dimensional Organic Luminescent Nano-/Micro-Materials. (United States)

    Song, Xiaoxian; Zhang, Zuolun; Zhang, Shoufeng; Wei, Jinbei; Ye, Kaiqi; Liu, Yu; Marder, Todd B; Wang, Yue


    Noncovalent synthesis of one-dimensional (1D) organic nano-/micro-materials with controllable geometric shapes or morphologies and special luminescent and electronic properties is one of the greatest challenges in modern chemistry and material science. Control of noncovalent interactions is fundamental for realizing desired 1D structures and crucial for understanding the functions of these interactions. Here, a series of thiophene-fused phenazines composed of a halogen-substituted π-conjugated plate and a pair of flexible side chains is presented, which displays halogen-dependent 1D self-assemblies. Luminescent 1D twisted wires, straight rods, and zigzag wires, respectively, can be generated in sequence when the halogen atoms are varied from the lightest F to the heaviest I. It was demonstrated that halogen-dependent anisotropic noncovalent interactions and mirror-symmetrical crystallization dominated the 1D-assembly behaviors of this class of molecules. The methodology developed in this study provides a potential strategy for constructing 1D organic materials with unique optoelectronic functions.

  2. Low-reactive circulating fluidized bed combustion (CFBC) fly ashes as source material for geopolymer synthesis. (United States)

    Xu, Hui; Li, Qin; Shen, Lifeng; Zhang, Mengqun; Zhai, Jianping


    In this contribution, low-reactive circulating fluidized bed combustion (CFBC) fly ashes (CFAs) have firstly been utilized as a source material for geopolymer synthesis. An alkali fusion process was employed to promote the dissolution of Si and Al species from the CFAs, and thus to enhance the reactivity of the ashes. A high-reactive metakaolin (MK) was also used to consume the excess alkali needed for the fusion. Reactivities of the CFAs and MK were examined by a series of dissolution tests in sodium hydroxide solutions. Geopolymer samples were prepared by alkali activation of the source materials using a sodium silicate solution as the activator. The synthesized products were characterized by mechanical testing, scanning electron microscopy (SEM), X-ray diffractography (XRD), as well as Fourier transform infrared spectroscopy (FTIR). The results of this study indicate that, via enhancing the reactivity by alkali fusion and balancing the Na/Al ratio by additional aluminosilicate source, low-reactive CFAs could also be recycled as an alternative source material for geopolymer production.

  3. Synthesis and gas adsorption study of porous metal-organic framework materials (United States)

    Mu, Bin

    Metal-organic frameworks (MOFs) or porous coordination polymers (PCPs) have become the focus of intense study over the past decade due to their potential for advancing a variety of applications including air purification, gas storage, adsorption separations, catalysis, gas sensing, drug delivery, and so on. These materials have some distinct advantages over traditional porous materials such as the well-defined structures, uniform pore sizes, chemically functionalized sorption sites, and potential for postsynthetic modification, etc. Thus, synthesis and adsorption studies of porous MOFs have increased substantially in recent years. Among various prospective applications, air purification is one of the most immediate concerns, which has urgent requirements to improve current nuclear, biological, and chemical (NBC) filters involving commercial and military purposes. Thus, the major goal of this funded project is to search, synthesize, and test these novel hybrid porous materials for adsorptive removal of toxic industrial chemicals (TICs) and chemical warfare agents (CWAs), and to install the benchmark for new-generation NBC filters. The objective of this study is three-fold: (i) Advance our understanding of coordination chemistry by synthesizing novel MOFs and characterizing these porous coordination polymers; (ii) Evaluate porous MOF materials for gasadsorption applications including CO2 capture, CH4 storage, other light gas adsorption and separations, and examine the chemical and physical properties of these solid adsorbents including thermal stability and heat capacity of MOFs; (iii) Evaluate porous MOF materials for next-generation NBC filter media by adsorption breakthrough measurements of TICs on MOFs, and advance our understanding about structureproperty relationships of these novel adsorbents.

  4. Transmission Electron Microscope Observation of Cubic GaN Grown by Metalorganic Vapor Phase Epitaxy with Dimethylhydrazine on (001) GaAs (United States)

    Kuwano, Noriyuki; Nagatomo, Yoshiyuki; Kobayashi, Kenki; Oki, Kensuke; Miyoshi, Seiro; Yaguchi, Hiroyuki; Onabe, Kentaro; Shiraki, Yasuhiro


    Cross-sectional transmission electron microscope observation has been performed on the microstructure of GaN films grown on a (001) GaAs substrate by metalorgahic vapor phase epitaxy (MOVPE) using 1,1-dimethylhydrazine (DMHy) and trimethylgallium (TMG) as the sources of nitrogen and gallium, respectively. Before the deposition, the surface of the substrate was nitrided with DMHy. High-resolution images and electron diffraction patterns confirmed that the GaN films have a zincblende structure (β-GaN) with the lattice constant of a GaN=0.454 nm, and contain bands of stacking faults parallel to {111} planes. The interface between GaN and GaAs is made of {111} facets with no interlayer. Misfit dislocations are found to be inserted on the interface approximately every five atomic planes of GaAs. The nitridation treatment with only DMHy for 130 min is found to form a thick layer of β-GaN on the (001) GaAs substrate. Nuclei of β-GaN formed by the pretreatment of surface nitridation play an important role in growing GaN in a zincblende structure during the supply of DMHy and TMG. The formation of facets on the top surface of GaN and on the interface of GaN/GaAs is explained in terms of the diffusion of arsenic in β-GaN. The characteristics of the structure of GaN films grown at 600 and 650° C are also presented.

  5. Synthesis of partial stabilized cement-gypsum as new dental retrograde filling material

    Energy Technology Data Exchange (ETDEWEB)

    Sadhasivam, S. [Institute of Biomedical Engineering, National Taiwan University, Taipei, Taiwan (China); Division of Medical Engineering Research, National Health Research Institute, Zhunan, Miaoli County, Taiwan (China); Chen, Jung-Chih [Institute of Biomedical Engineering, National Taiwan University, Taipei, Taiwan (China); Medical Device Innovation Center, National Cheng Kung University, Tainan,Taiwan (China); Savitha, S. [Institute of Biomedical Engineering, National Taiwan University, Taipei, Taiwan (China); Hsu, Ming-Xiang; Hsu, Chung-King [Institute of Materials Science and Engineering, National Taipei University of Technology, Taipei, Taiwan (China); Lin, Chun-Pin [School of Dentistry and Graduate Institute of Clinical Dentistry, College of Medicine, National Taiwan University and National Taiwan University Hospital, Taipei, Taiwan (China); Lin, Feng-Huei, E-mail: [Institute of Biomedical Engineering, National Taiwan University, Taipei, Taiwan (China); Division of Medical Engineering Research, National Health Research Institute, Zhunan, Miaoli County, Taiwan (China)


    The study describes the sol-gel synthesis of a new dental retrograde filling material partial stabilized cement (PSC)-gypsum by adding different weight percentage of gypsum (25% PSC + 75% gypsum, 50% PSC + 50% gypsum and 75% PSC + 25% gypsum) to the PSC. The crystalline phase and hydration products of PSC-gypsum were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) analysis. The handling properties such as setting time, viscosity, tensile strength, porosity and pH, were also studied. The XRD and microstructure analysis demonstrated the formation of hydroxyapatite and removal of calcium dihydrate during its immersion in simulated body fluid (SBF) on day 10 for 75% PSC + 25% gypsum. The developed PSC-gypsum not only improved the setting time but also greatly reduced the viscosity, which is very essential for endodontic surgery. The cytotoxic and cell proliferation studies indicated that the synthesized material is highly biocompatible. The increased alkaline pH of the PSC-gypsum also had a remarkable antibacterial activity. - Highlights: Black-Right-Pointing-Pointer A new dental retrograde filling material PSC-gypsum was developed. Black-Right-Pointing-Pointer PSC-gypsum cement has shown excellent initial and final setting time as 15-35 min. Black-Right-Pointing-Pointer It not only improved the setting time but also retain the viscosity, 2 Pa{center_dot}s. Black-Right-Pointing-Pointer High alkaline pH of the cement had a remarkable antibacterial activity. Black-Right-Pointing-Pointer Cytotoxicity studies revealed that the synthesized material is highly biocompatible.

  6. Synthesis of NiMnO3/C nano-composite electrode materials for electrochemical capacitors. (United States)

    Kakvand, Pejman; Rahmanifar, Mohammad Safi; El-Kady, Maher F; Pendashteh, Afshin; Kiani, Mohammad Ali; Hashami, Masumeh; Najafi, Mohsen; Abbasi, Ali; Mousavi, Mir F; Kaner, Richard B


    Demand for high-performance energy storage materials has motivated research activities to develop nano-engineered composites that benefit from both high-rate and high-capacitance materials. Herein, NiMnO3 (NMO) nanoparticles have been synthesized through a facile co-precipitation method. As-prepared NMO samples are then employed for the synthesis of nano-composites with graphite (Gr) and reduced graphene oxide (RGO). Various samples, including pure NMO, NMO-graphite blend, as well as NMO/Gr and NMO/RGO nano-composites have been electrochemically investigated as active materials in supercapacitors. The NMO/RGO sample exhibited a high specific capacitance of 285 F g(-1) at a current density of 1 A g(-1), much higher than the other samples (237 F g(-1) for NMO/Gr, 170 F g(-1) for NMO-Gr and 70 F g(-1) for NMO). Moreover, the NMO/RGO nano-composite has shown excellent cycle stability with a 93.5% capacitance retention over 1000 cycles at 2 A g(-1) and still delivered around 87% of its initial capacitance after cycling for 4000 cycles. An NMO/RGO composite was assessed in practical applications by assembling NMO/RGO//NMO/RGO symmetric devices, exhibiting high specific energy (27.3 Wh kg(-1)), high specific power (7.5 kW kg(-1)), and good cycle stability over a broad working voltage of 1.5 V. All the obtained results demonstrate the promise of NMO/RGO nano-composite as a high-performance electrode material for supercapacitors.

  7. Sol–gel one-pot synthesis in soft conditions of mesoporous silica materials ready for drug delivery system

    NARCIS (Netherlands)

    Tourne-Peteilh, C.; Begu, S.; Lerner, D.A.; Galarneau, A.; Lafont, U.; Devoiselle, J.M.


    The present work reveals a new and simple strategy, a one-step sol–gel procedure, to encapsulate a low water-soluble drug in silica mesostructured microparticles and to improve its release in physiological media. The synthesis of these new materials is based on the efficient solubilisation of a

  8. Human neutrophil elastase peptide sensors conjugated to cellulosic and nanocellulosic materials: part I, synthesis and characterization of fluorescent analogs (United States)

    Here we describe the synthesis and characterization of peptide conjugated cellulose and nanocellulose materials as sensors for fluorescent detection of human neutrophil elastase (HNE). The cellulose sensor surfaces selected are filter paper (FP) and print cloth (PC) fabric, which are composed of pro...

  9. Material Transport and Synthesis by Cantilever-free Scanning Probe Lithography (United States)

    Liao, Xing

    Reliably synthesizing and transporting materials in nanoscale is the key question in many fields of nanotechnology. Cantilever-free scanning probe lithography, by replacing fragile and costly cantilevers with a robust and low cost elastomeric structure, fundamentally solved the low-throughput nature of scanning probe lithography, which has great potential to be a powerful and point-of-use tool for high throughput synthesis of various kinds of nanomaterials. Two nanolithographic methods, polymer pen lithography (PPL) and beam pen lithography (BPL), have been developed based on the cantilever-free architecture to directly deliver materials and transfer energy to substrates, respectively. The first portion of my thesis, including chapter two and chapter three, addresses major challenges remaining in the cantilever-free scanning probe lithographic techniques. Chapter two details the role of contact force in polymer pen lithography. A geometric model was developed to quantitatively explain the relationship between the z-piezo extension, the contact force and the resulted feature size. With such a model, force can be used as the in-situ feedback during the patterning and a new method for leveling the pen arrays was developed, which utilizes the total force between the pen arrays and the surface to achieve leveling with a tilt of less than 0.004°. In chapter three, massively multiplexed near-field photolithography has been demonstrated by combining BPL with a batch method to fabricate nanometer scale apertures in parallel fashion and a strategy to individually actuation of each pen in the pen array are discussed. This transformative combination enables one to writing arbitrary patterns composed of diffraction-unlimited features over square centimeter areas that are in registry with existing patterns and nanostructures, creating a unified tool for constructing and studying nanomaterials. The second portion of this thesis focuses on applications of cantilever-free scanning

  10. Laser-induced chemistry: an advanced tool for micro structuring, synthesis, and modification of materials (United States)

    Metev, Simeon; Stephen, Andreas; Schwarz, Joerg; Wochnowski, Carsten


    Laser-induced technological chemical processes can significantly contribute to the development of new methods for micro treatment of materials and hence to the broadening of the application spectrum of laser microtechnology. In this paper three typical laser-activated chemical technological methods in liquids, gases and solids and their possible applications are presented and discussed: (1) Laser-induced liquid-phase jet-chemical etching of metals. In this method, laser radiation which is guided from a coaxially expanding liquid jet-stream initiates locally on a metal surface a thermochemical etching reaction, which leads to a selective material removal at high resolution (thermochemical CVD processes taking place in a photon-initiated stationary plasma maintained in the electromagnetic optical field of a high-power cw-CO2 laser radiation. This method allows synthesis of thin-film coatings in the open-air atmosphere without using vacuum or reaction chamber; (3) Laser-induced photochemical modification of the optical properties of polymers. This method is based on the local controllable change of the polymer structure leading to modification of the refractive index in the treated area. By numerous independently adjustable laser radiation parameters, for instance wavelength and irradiation dose, the modification process can be controllably driven in order to generate desired functional properties.

  11. Synthesis and Characterization of Bio-Oil Phenol Formaldehyde Resin Used to Fabricate Phenolic Based Materials

    Directory of Open Access Journals (Sweden)

    Yong Cui


    Full Text Available In this study, bio-oil from the fast pyrolysis of renewable biomass was used as the raw material to synthesize bio-oil phenol formaldehyde (BPF resin—a desirable resin for fabricating phenolic-based material. During the synthesis process, paraformaldehyde was used to achieve the requirement of high solid content and low viscosity. The properties of BPF resins were tested. Results indicated that BPF resin with the bio-oil addition of 20% had good performance on oxygen index and bending strength, indicating that adding bio-oil could modify the fire resistance and brittleness of PF resin. The thermal curing behavior and heat resistance of BPF resins were investigated by differential scanning calorimetry (DSC and thermal gravimetric analysis (TGA. Results showed that adding bio-oil had an impact on curing characteristics and thermal degradation process of PF resin, but the influence was insignificant when the addition was relatively low. The chemical structure and surface characteristics of BPF resins were determined by Fourier transform infrared (FTIR spectroscopy and scanning electron microscopy (SEM. The analysis demonstrated that adding bio-oil in the amount of 20% was able to improve the crosslinking degree and form more hydrocarbon chains in PF resin.

  12. Bottom-up synthesis of vertically oriented two-dimensional materials (United States)

    Vilá, R. A.; Momeni, K.; Wang, Q.; Bersch, B. M.; Lu, N.; Kim, M. J.; Chen, L. Q.; Robinson, J. A.


    Understanding nucleation and growth of two-dimensional (2D) and layered materials is a challenging topic due to the complex van der Waals interactions between layers and substrate. The morphology of 2D materials is known vary depending on experimental conditions. For the case of MoS2, the morphology has been shown to vary from rounded (molybdenum rich) domains to equilateral triangular (sulfur rich) domains. These different morphologies can result in drastically different properties, which can be exploited for applications in catalytic reactions, digital electronics, optoelectronics, and energy storage. Powder vaporization (PV) synthesis of molybdenum disulfide (MoS2) can yield vertical domains, however, these domains are often ignored when the morphology evolution of MoS2 is discussed, thereby completely omitting a major part of the impact of the Mo:S ratio to the growth mode of MoS2 during PV. Combining experimental and numerical simulation methods, we reveal a vertical-to-horizontal growth mode transition for MoS2 that occurs in the presence of a molybdenum oxide partial pressure gradient. Transmission electron microscopy reveals that the growth of vertical MoS2 results from initial seeding of single crystalline molybdenum dioxide, followed by sulfurization from the substrate upward to form vertically oriented MoS2 domains.

  13. Grafting materials for alveolar cleft reconstruction: a systematic review and best-evidence synthesis. (United States)

    Wu, C; Pan, W; Feng, C; Su, Z; Duan, Z; Zheng, Q; Hua, C; Li, C


    The purpose of this study was to compare the efficacy of alveolar bone reconstruction for alveolar cleft patients performed with the traditional iliac graft or alternative/supplementary bone grafting materials. Electronic databases, relevant journals, and reference lists of the included studies were searched to the end of June 2016. A best-evidence synthesis was performed to draw conclusions. A total of 38 studies were included, which provided 25 pieces of evidence: seven of moderate evidence and 18 of insufficient evidence. The seven pieces of moderate evidence indicated that (1) bone morphogenetic protein 2 bound to absorbable collagen sponge shares similar cleft repair efficacy to the iliac graft; (2) covering the iliac graft with an acellular dermis matrix membrane may increase bone retention for unilateral cleft patients; (3) mixing iliac graft with platelet-rich plasma may increase bone retention for skeletally mature patients, but (4) does not achieve the same result for younger patients; and compared with the iliac graft, (5) the mandible graft is more effective, whereas (6) the cranium graft and (7) rib graft are less effective for alveolar cleft reconstruction. The efficacy of the remaining grafting materials was supported by insufficient evidence. More well-designed controlled studies are needed to ascertain the long-term clinical results of alveolar cleft reconstruction. Copyright © 2017 International Association of Oral and Maxillofacial Surgeons. Published by Elsevier Ltd. All rights reserved.

  14. Synthesis and Characterization of Bio-Oil Phenol Formaldehyde Resin Used to Fabricate Phenolic Based Materials. (United States)

    Cui, Yong; Hou, Xiaopeng; Wang, Wenliang; Chang, Jianmin


    In this study, bio-oil from the fast pyrolysis of renewable biomass was used as the raw material to synthesize bio-oil phenol formaldehyde (BPF) resin-a desirable resin for fabricating phenolic-based material. During the synthesis process, paraformaldehyde was used to achieve the requirement of high solid content and low viscosity. The properties of BPF resins were tested. Results indicated that BPF resin with the bio-oil addition of 20% had good performance on oxygen index and bending strength, indicating that adding bio-oil could modify the fire resistance and brittleness of PF resin. The thermal curing behavior and heat resistance of BPF resins were investigated by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). Results showed that adding bio-oil had an impact on curing characteristics and thermal degradation process of PF resin, but the influence was insignificant when the addition was relatively low. The chemical structure and surface characteristics of BPF resins were determined by Fourier transform infrared (FTIR) spectroscopy and scanning electron microscopy (SEM). The analysis demonstrated that adding bio-oil in the amount of 20% was able to improve the crosslinking degree and form more hydrocarbon chains in PF resin.

  15. Synthesis by plasma of polymer-metal materials; Sintesis por plasma de materiales polimero-metal

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez R, G


    The objective of this work is the design of an experimental set-up to synthesize polymer- metal composites by plasma with versatility in the conditions of synthesis. The main components are a vacuum system capable to reach up to 10{sup -2} mbar and valves and accessories to control the pressure in the system. In order to generate the electrical discharges and the plasma, an electrical circuit with an inductive connection at 13.56 MHz of frequency was constructed. The electric field partially ionizes the reactor atmosphere where the polymer-metal composites were synthesized. The reactor has two metallic electrodes, one in front of the other, where the particles electrically charged collide against the electrodes producing ablation on them. The polymer-metal composites were synthesized by means of an inductive connection at 13.56 MHz. Aniline, 3-chlorine-ethylene and electrodes of silver (Ag) and copper (Cu) were used in a cylindrical reactor coupled with an external coil to generate glow discharges. The average pressures were 6.15 X 10{sup -1} and 5.2 X 10{sup -1} mbar for the synthesis of Poly aniline (P An) and Poly chloroethylene (PE-CI), respectively. The synthesis was performed during 60 and 180 minutes for P An and PE-CI, respectively. The polymers were formed, as films, with an average thickness of 6.42 {mu}m for P An and, in the case of PE-CI, with an approximately growing rate of 14 {eta}m/W. The power in the syntheses was 30, 50, 70 and 90 W for P An and 50, 100, 120, 140 170, and 200 W for PE-CI. The characterization of the polymer-metal composites was done by energy dispersive spectroscopy to study the composition and the relation of the elements involved in the synthesis. The morphology of the films was studied by means of scanning electron microscopy. The infrared analysis (IR) was done to study the chemicals bonds and the structure of these polymers. Another important study in these materials was the behavior of the electrical conductivity ({sigma

  16. Investigating the Heavy Metal Adsorption of Mesoporous Silica Materials Prepared by Microwave Synthesis (United States)

    Zhu, Wenjie; Wang, Jingxuan; Wu, Di; Li, Xitong; Luo, Yongming; Han, Caiyun; Ma, Wenhui; He, Sufang


    Mesoporous silica materials (MSMs) of the MCM-41 type were rapidly synthesized by microwave heating using silica fume as silica source and evaluated as adsorbents for the removal of Cu2+, Pb2+, and Cd2+ from aqueous solutions. The effects of microwave heating times on the pore structure of the resulting MSMs were investigated as well as the effects of different acids which were employed to adjust the solution pH during the synthesis. The obtained MCM-41 samples were characterized by nitrogen adsorption-desorption analyses, X-ray powder diffraction, and transmission electron microscopy. The results indicated that microwave heating method can significantly reduce the synthesis time of MCM-41 to 40 min. The MCM-41 prepared using citric acid (c-MCM-41(40)) possessed more ordered hexagonal mesostructure, higher pore volume, and pore diameter. We also explored the ability of c-MCM-41(40) for removing heavy metal ions (Cu2+, Pb2+, and Cd2+) from aqueous solution and evaluated the influence of pH on its adsorption capacity. In addition, the adsorption isotherms were fitted by Langmuir and Freundlich models, and the adsorption kinetics were assessed using pseudo-first-order and pseudo-second-order models. The intraparticle diffusion model was studied to understand the adsorption process and mechanism. The results confirmed that the as-synthesized adsorbent could efficiently remove the heavy metal ions from aqueous solution at pH range of 5-7. The adsorption isotherms obeyed the Langmuir model, and the maximum adsorption capacities of the adsorbent for Cu2+, Pb2+, and Cd2+ were 36.3, 58.5, and 32.3 mg/g, respectively. The kinetic data were well fitted to the pseudo-second-order model, and the results of intraparticle diffusion model showed complex chemical reaction might be involved during adsorption process.

  17. Electrochemical synthesis and characterisation of hybrid materials polypyrrole/dodecatungstophosphate as protective agents against steel corrosion (United States)

    Bonastre Cano, Jose Antonio

    hand, this pretreatment should guarantee appropriate conditions in order to obtain a coating with high adhesion on carbon steel. Once studied the better parameters for the synthesis of the hybrid material by cyclic voltammetry, hybrid material is morphological, chemical and electrochemical characterised by the following techniques: Cyclic Voltammetry, Scanning Electron Microscopy, Energy Dispersive X Ray, X Ray Photoelectron Spectroscopy and Electrochemical Impedance Spectroscopy. The hybrid material polypyrrole/PW 12O403-. chemical structure presents Fe oxides and hydroxide within the polypyrrole polycationic matrix. Hybrid material polypyrrol/PW12O403- diminishes the corrosion of carbon steel in NaOH and Porland cement filtering solutions. These cement solutions simulate the pore fluid conditions existing in cured mortar or concrete elements. Fe ion concentration data were determinated in corrosion tests. Voltammetric response of polymeric coatings was evaluated by cyclic voltammetry. Finally, the protection provided by hybrid material polypyrrole/PW 12O403, in oxidised and reduced state, was evaluated on carbon steel electrodes embedded in Portland cement mortars immersed in seawater and submitted to an accelerated carbonation process for 265 days. Polymeric material covered carbon steel electrodes in reduced state suffer a Fe gravimetric loss 15 times lower than the ones of bare electrodes against chlorides attack, due to the effect of physical barrier. Hybrid material covered electrodes in oxidised state after being submitted to a carbonation process suffer a Fe gravimetric loss 2.5 times lower than the ones of bare electrodes, due to galvanic protection provided by hybrid material polypyrrole/PW 12O403- on carbon steel.

  18. Casting a Wider Net: Rational Synthesis Design of Low-Dimensional Bulk Materials. (United States)

    Benavides, Katherine A; Oswald, Iain W H; Chan, Julia Y


    The discovery of novel magnetic and electronic properties in low-dimensional materials has led to the pursuit of hierarchical materials with specific substructures. Low-dimensional solids are highly anisotropic by nature and show promise in new quantum materials leading to exotic physical properties not realized in three-dimensional materials. We have the opportunity to extend our synthetic strategy of the flux-growth method to designing single crystalline low-dimensional materials in bulk. The goal of this Account is to highlight the synthesis and physical properties of several low-dimensional intermetallic compounds containing specific structural motifs that are linked to desirable magnetic and electrical properties. We turned our efforts toward intermetallic compounds consisting of antimony nets because they are closely linked to properties such as high carrier mobility (the velocity of an electron moving through a material under a magnetic field) and large magnetoresistance (the change in resistivity with an applied magnetic field), both of which are desirable properties for technological applications. The SmSb 2 structure type is of particular interest because it is comprised of rectangular antimony nets and rare earth ions stacked between the antimony nets in a square antiprismatic environment. LnSb 2 (Ln = La-Nd, Sm) have been shown to be highly anisotropic with SmSb 2 exhibiting magnetoresistance of over 50000% for H∥c axis and ∼2400% for H∥ab. Using this structure type as an initial building block, we envision the insertion of transition metal substructures into the SmSb 2 structure type to produce ternary materials. We describe compounds adopting the HfCuSi 2 structure type as an insertion of a tetrahedral transition metal-antimony subunit into the LnSb 2 host structure. We studied LnNi 1-x Sb 2 (Ln = Y, Gd-Er), where positive magnetoresistance reaching above 100% was found for the Y, Gd, and Ho analogues. We investigated the influence of the

  19. On the suppression of superconducting phase formation in YBCO materials by templated synthesis in the presence of a sulfated biopolymer

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Elliott; Schnepp, Zoe [Centre for Organized Matter Chemistry, School of Chemistry, University of Bristol, Cantock' s Close, Bristol BS8 1TS (United Kingdom); Wimbush, Stuart C. [Department of Materials Science and Metallurgy, University of Cambridge, Pembroke Street, Cambridge CB2 3QZ (United Kingdom); Hall, Simon R. [Centre for Organized Matter Chemistry, School of Chemistry, University of Bristol, Cantock' s Close, Bristol BS8 1TS (United Kingdom)], E-mail:


    The use of biopolymers as templates to control superconductor crystallization is a recent phenomenon and is generating a lot of interest both from the superconductor community and in materials chemistry circles. This work represents a critical finding in the use of such biopolymers, in particular the contraindicatory nature of sulfur when attempting to affect a morphologically controlled synthesis. Synthesis of superconducting nanoparticles was attempted using carrageenan as a morphological template. Reactive sulfate groups on the biopolymer prevent this, producing instead significant quantities of barium sulfate nanotapes. By substituting the biopolymer for structurally analogous, non-sulfated agar, we show that superconducting nanoparticles could be successfully synthesized.

  20. Growth of gallium nitride based devices on silicon(001) substrates by metalorganic vapor phase epitaxy; Wachstum von Galliumnitrid-basierten Bauelementen auf Silizium(001)-Substraten mittels metallorganischer Gasphasenepitaxie

    Energy Technology Data Exchange (ETDEWEB)

    Reiher, Fabian


    The main topic of this thesis is to investigate GaN-based layer systems grown by metalorganic vapor phase epitaxy on Si(001) substrates. A temperature shift up to 45 K is measured for a complete device structure on a 2-inch silicon substrate. By using a 40 nm thin LT-AlN-seed layer (680 C), the GaN crystallites on Si(001) substrates are almost oriented with their GaN(10 anti 12)-planes parallel to the Si(001)-plane. A four-fold azimuthal symmetry occurs for these layers, with the GaN[10 anti 11]-direction is aligned parallel to one of the four equivalent left angle 110 right angle -directions, respectively. However, a mono-crystalline and fully coalesced GaN-layer with this crystallographic orientation could not yet been obtained. If a deposition temperature of more than 1100 C is used for the AlN-seed layer, solely the GaN[0001]- growth direction of crystallites occurs in the main GaN layer on Si(001) substrates. These c-axis oriented GaN columns feature two opposite azimuthal alignments that are rotated by 90 with respect to each other and with GaN[11 anti 20] parallel Si[110] and GaN[10 anti 10] parallel Si[110], respectively. By using 4 off-oriented substrates towards the Si[110]-direction, one certain azimuthal texture component can be selected. The critical value of the miscut angle corresponds to theoretical calculations predicting the occurrence of atomic double steps on the Si(001) surface. The achieved crystallographic quality of the GaN layers on Si(001) is characterized by having a tilt of FWHM=0.27 and a twist of FWHM=0.8 of the crystallites, determined by X-ray diffraction. A completely crack-free, up to 2.5 {mu}m thick, and mono-crystalline GaN-template can be realized on Si(001), integrating 4 or 5 LT-AlN-interlayers in the GaN buffer structure. Based on this structure, the first successful implementation of an (InGaN/GaN)-LED on Si(001) is achieved. Furthermore, the possible fabrication of GaN-based FET-structures is demonstrated with a fully

  1. Structural properties of ZnSy Se1-yZnSe/GaAs (001) heterostructures grown by photoassisted metalorganic vapor phase epitaxy (United States)

    Zhang, X. G.; Kalisetty, S.; Robinson, J.; Zhao, G.; Parent, D. W.; Ayers, J. E.; Jain, F. C.


    ZnSySe1-yZnSe/GaAs (001) heterostructures have been grown by photoassisted metalorganic vapor phase epitaxy, using the sources dimethylzinc, dimethylselenium, diethylsulfur, and irradiation by a Hg arc lamp. The solid phase composition vs gas phase composition characteristics have been determined for ZnSyySe1-y grown with different mole fractions of dimethylselenium and different temperatures. Although the growth is not mass-transport controlled with respect to the column VI precursors, the solid phase composition vs gas phase composition characteristics are sufficiently gradual so that good compositional control and lattice matching to GaAs substrates can be readily achieved by photoassisted growth in the temperature range 360°C ≤ T ≤ 400°C. ZnSe/GaAs (001) single heterostructures were grown by a two-step process with ZnSe thicknesses in the range from 54 nm to 776 nm. Based on 004 x-ray rocking curve full width at half maximums (FWHMs), we have determined that the critical layer thickness is hc ≤200 nm. Using the classical method involving strain, lattice relaxation is undetectable in layers thinner than 270 nm for the growth conditions used here. Therefore, the rocking curve FWHM is a more sensitive indicator of lattice relaxation than the residual strain. For ZnSySe1-y layers grown on ZnSe buffers at 400°C, the measured dislocation density-thickness product Dh increases monotonically with the room temperature mismatch. Lower values of the Dh product are obtained for epitaxy on 135 nm buffers compared to the case of 270 nm buffers. This difference is due to the fact that the 135 nm ZnSe buffers are pseudomorphic as deposited. For ZnSySe1-y layers grown on 135 nm ZnSe buffers at 360°C, the minimum dislocation density corresponds approximately to room-temperature lattice matching (y ˜ 5.9%), rather than growth temperature lattice matching (y ˜ 7.6%). Epitaxial layers with lower dislocation densities demonstrated superior optical quality, as judged by

  2. Synthesis, microstructure and properties of BiFeO3-based multiferroic materials: A review

    Directory of Open Access Journals (Sweden)

    Bernardo, M. S.


    Full Text Available BiFeO3-based materials are currently one of the most studied multiferroics due to their possible applications at room temperature. However, among the large number of published papers there is much controversy. For example, possibility of synthesizing a pure BiFeO3 phase is still source of discussion in literature. Not even the nature of the binary Bi2O3-Fe2O3 diagram has been clarified yet. The difficulty in controlling the formation of parasite phases reaches the consolidation step. Accordingly, the sintering conditions must be carefully determined both to get dense materials and to avoid bismuth ferrite decomposition. However, the precise conditions to attain dense bismuth ferrite materials are frequently contradictory among different works. As a consequence, the reported properties habitually result opposed and highly irreproducible hampering the preparation of BiFeO3 materials suitable for practical applications. In this context, the purpose of the present review is to summarize the main researches regarding BiFeO3 synthesis, microstructure and properties in order to provide an easier understanding of these materials.Los materiales basados en BiFeO3 son en la actualidad uno de los multiferroicos más estudiados debido a sus posibles aplicaciones a temperatura ambiente. Sin embargo, entre la multitud de trabajos publicados referentes a estos materiales existe mucha controversia. Por ejemplo, la posibilidad de sintetizar una fase BiFeO3 pura es aún objeto de discusión en la bibliografía y la naturaleza de los diagramas de fases del sistema Bi2O3-Fe2O3 aún no está clara. La dificultad para controlar las fases parásitas se extiende al proceso de consolidación por lo que las condiciones de sinterización deben ser cuidadosamente controladas para obtener materiales densos y al mismo tiempo evitar la descomposición de la ferrita. No obstante, las condiciones precisas para obtener materiales densos de BiFeO3 son frecuentemente

  3. Preparation, characterization and catalytic properties of MCM-48 supported tungstophosphoric acid mesoporous materials for green synthesis of benzoic acid

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Hai-Yan; Zhang, Xiao-Li; Chen, Xi; Chen, Ya; Zheng, Xiu-Cheng, E-mail:


    MCM-48 and tungstophosphoric acid (HPW) were prepared and applied for the synthesis of HPW/MCM-48 mesoporous materials. The characterization results showed that HPW/MCM-48 obtained retained the typical mesopore structure of MCM-48, and the textural parameters decreased with the increase loading of HPW. The catalytic oxidation results of benzyl alcohol and benzaldehyde with 30% H{sub 2}O{sub 2} indicated that HPW/MCM-48 was an efficient catalyst for the green synthesis of benzoic acid. Furthermore, 35 wt% HPW/MCM-48 sample showed the highest activity under the reaction conditions. Highlights: • 5–45 wt% HPW/MCM-48 mesoporous catalysts were prepared and characterized. • Their catalytic activities for the green synthesis of benzoic acid were investigated. • HPW/MCM-48 was approved to be an efficient catalyst. • 5 wt% HPW/MCM-48 exhibited the highest catalytic activity.

  4. Novel approaches to the synthesis and cooperative assembly of inorganic materials utilizing block copolypeptides (United States)

    Euliss, Larken E.

    Biominerals and biocomposites are highly ornate and functional materials. Nature controls the properties of these materials by organizing their organic and inorganic constituents on the atomic, molecular, nano, and micron scales. The remarkable precision and complexity of this organization is accomplished using a combination of electrostatics, hydrogen bonding, disulfide bonding, and other molecular-level interactions. The goal of the work described in this dissertation was to use the principles employed by Nature in the biological assembly of biomaterials as inspiration for developing (1) completely synthetic and novel composite materials, and (2) new general methods for the synthesis of composite materials. Specifically, block copolypeptides were used as structure-directing agents in several successful applications of this approach. One application involves the rational design of an organic polymer molecule to direct the crystallization of calcium carbonate into microspheres. I have shown that the doubly-hydrophilic block copolypeptide poly{Nepsilon-2[2-(2 methoxy-ethoxy)ethoxy]acetyl-L-lysine}100-block-poly(L-aspartate sodium salt)30 can act as the structure-directing agent in this process. In addition, control over the morphology of calcium carbonate crystals can be exerted using anionic, amphiphilic block copolypeptides, such as poly(L-aspartate sodium salt)100-block-poly(L-phenylalanine- random-L-leucine)50 and poly(L-glutamate sodium salt) 100-block-poly(L-phenylalanine-random-L-leucine) 50. I have demonstrated that microspheres of calcium carbonate can be prepared by introducing the polymer additive during crystallization. These self-assembling polymers control the precipitation of the microspheres by acting as templates for sphere formation. Another application involves the organization of magnetic nanoparticles into well-defined, soluble nanoclusters. First, I have demonstrated that highly crystalline, monodisperse maghemite (gamma-Fe2O3) nanoparticles

  5. Multifunctional iron-based metal oxide nanostructured materials: Synthesis, characterization, and properties (United States)

    Park, Tae-Jin

    Iron-based metal oxides, such as iron oxides, iron-containing perovskites, and iron-containing perovskite composites or solid solutions, are promising materials for the design and synthesis of technologically important multifunctional materials. They are noteworthy for their unique and diverse properties including electronic, magnetic, and elastic ones. Stimulated by interest in the bulk properties of these materials as well as scientific potential and applications at the nanoscale, iron-based metal oxide nanostructured (FeMONS) materials are being considered as an interesting model system to investigate fundamental properties and for a host of potential applications as diverse as additives, catalysts, electronic devices, magnetic recording media, information storage, spintronics, and sensors. Recent research on a multiferroic system, such as BiFeO3, reveals that there are unique couplings among the independent physical properties including ferroelectricity, ferromagnetism, and ferroelasticity. Developing approaches to designing as well as investigating properties of new synthetic formulations of these transition metal oxide nanomaterials has been the recent focus of much of our efforts in this group. Multiferroic bismuth ferrite (BiFeO 3) nanoparticles have been synthesized employing a facile sol-gel method and their size-dependent magnetic properties have been studied and correlated with: (i) increased suppression of the known spiral spin structure (period length of ˜62 nm) with decreasing nanoparticle size and (ii) uncompensated spins and strain anisotropies at the surface. Moreover, BiFeO 3 nanotubes have been generated using a modified template methodology and extensively characterized. Furthermore, solid solutions of BiFeO 3 and typical perovskites, such as BaTiO3 and SrTiO 3, have been prepared employing a molten salt method and the study has been extended to properties associated with their inherent compositions. Single-crystalline Bi2Fe4O9 nanocubes have

  6. Policaprolactone/polyvinylpyrrolidone/siloxane hybrid materials: Synthesis and in vitro delivery of diclofenac and biocompatibility with periodontal ligament fibroblasts

    Energy Technology Data Exchange (ETDEWEB)

    Peña, José A. [Departamento de Química, Pontificia Universidad Javeriana, Bogotá D.C. (Colombia); Gutiérrez, Sandra J., E-mail: [Centro de investigaciones Odontológicas, Facultad de Odontología, Pontificia Universidad Javeriana, Bogotá (Colombia); Villamil, Jean C. [Centro de investigaciones Odontológicas, Facultad de Odontología, Pontificia Universidad Javeriana, Bogotá (Colombia); Agudelo, Natalia A. [Instituto de Química, Universidad de Antioquia, Medellin (Colombia); Pérez, León D., E-mail: [Grupo de Macromoléculas, Departamento de Química, Universidad Nacional de Colombia, Carrera 45 No 26–85, edificio 451 of. 449, Bogotá D.C. Colombia (Colombia)


    In this paper, we report the synthesis of polycaprolactone (PCL) based hybrid materials containing hydrophilic domains composed of N-vinylpyrrolidone (VP), and γ-methacryloxypropyltrimethoxysilane (MPS). The hybrid materials were obtained by RAFT copolymerization of N-vinylpyrrolidone and MPS using a pre-formed dixanthate-end-functionalized PCL as macro-chain transfer agent, followed by a post-reaction crosslinking step. The composition of the samples was determined by elemental and thermogravimetric analyses. Differential scanning calorimetry and X-ray diffraction indicated that the crystallinity of PCL decreases in the presence of the hydrophilic domains. Scanning electron microscopy images revealed that the samples present an interconnected porous structure on the swelling. Compared to PCL, the hybrid materials presented low water contact angle values and higher elastic modulus. These materials showed controlled release of diclofenac, and biocompatibility with human periodontal ligament fibroblasts. - Highlights: • Synthesis of Policaprolactone/polyvinylpyrrolidone/siloxane hybrid materials • Moderated hydrophilic materials with high swelling resistance • Organic–inorganic hybrid materials were biocompatible.

  7. Organic luminescent materials. First results on synthesis and characterization of Alq{sub 3} thin films

    Energy Technology Data Exchange (ETDEWEB)

    Baldacchini, G.; Gagliardi, S.; Montereali, R.M.; Pace, A. [ENEA, Centro Ricerche Frascati, Frascati, RM (Italy). Div. Fisica Applicata; Balaji Pode, R. [Nagpur University, Nagpur (India). Dept. of Physics


    Inorganic semiconductor diodes brought a technological revolution in the field of efficient light and laser sources in the last 20 years. New development in this field are expected from organic compounds, thanks to their low cost of synthesis and the relative easiness of growth as thin films. In particular, electrically pumped luminescent devices based on organic thin layers are among the most promising systems for next generation flat panel displays and semiconductor lasers. The tris - (8-hydroxy quinoline)-aluminium complex-Alq{sub 3} - is one of the most studied electro luminescent materials. In this paper, after a short introduction regarding historical development in the field, are reported preliminary results on the growth of Alq{sub 3} films and on their optical and spectroscopic characterization. [Italian] Negli ultimi 20 anni i diodi semiconduttori hanno portato una rivoluzione tecnologica nel campo delle sorgenti luminose e laser. Un nuovo sviluppo possibile in questo campo sono i composti organici, grazie al basso costo di sintesi e la relativa facilita' di crescerli in forma di film sottile. In particolare, dispositivi luminescenti pompati elettricamente basati su film sottili di materiali organici sono promettenti per una nuova generazione di display per schermi piatti e laser a Alq{sub 3} e' uno dei materiali elettroluminescenti piu' studiati. In questo rapporto, dopo una breve introduzione sullo sviluppo storico in questo campo, presentiamo i nostri primi risultati sulla crescita e caratterizzazione ottica di film di Alq{sub 3}.

  8. Co-implantation of carbon and nitrogen into silicon dioxide for synthesis of carbon nitride materials

    CERN Document Server

    Huang, M B; Nuesca, G; Moore, R


    Materials synthesis of carbon nitride has been attempted with co-implantation of carbon and nitrogen into thermally grown SiO sub 2. Following implantation of C and N ions to doses of 10 sup 1 sup 7 cm sup - sup 2 , thermal annealing of the implanted SiO sub 2 sample was conducted at 1000 degree sign C in an N sub 2 ambient. As evidenced in Fourier transform infrared measurements and X-ray photoelectron spectroscopy, different bonding configurations between C and N, including C-N single bonds, C=N double bonds and C=N triple bonds, were found to develop in the SiO sub 2 film after annealing. Chemical composition profiles obtained with secondary ion mass spectroscopy were correlated with the depth information of the chemical shifts of N 1s core-level electrons, allowing us to examine the formation of C-N bonding for different atomic concentration ratios between N and C. X-ray diffraction and transmission electron microscopy showed no sign of the formation of crystalline C sub 3 N sub 4 precipitates in the SiO ...

  9. Synthesis of ultra high molecular weight polyethylene: A differentiate material for specialty applications

    Energy Technology Data Exchange (ETDEWEB)

    Padmanabhan, Sudhakar, E-mail: [Research Centre, Vadodara Manufacturing Division, Reliance Industries Limited, Vadodara, 391 346, Gujarat (India); Sarma, Krishna R.; Rupak, Kishor; Sharma, Shashikant [Research Centre, Vadodara Manufacturing Division, Reliance Industries Limited, Vadodara, 391 346, Gujarat (India)


    Tailoring the synthesis of a suitable Ziegler-Natta (ZN) catalyst coupled with optimized polymerization conditions using a suitable activator holds the key for an array of differentiated polymers with diverse and unique properties. Ultra high molecular weight polyethylene (UHMWPE) is one such polymer which we have synthesized using TiCl{sub 4} anchored on MgCl{sub 2} as the support and activated using AlRR'{sub 2} (where R, R' = iso-prenyl or isobutyl) under specific conditions. Here in we have accomplished a process for synthesizing UHMWPE in hydrocarbon as the medium with molecular weights ranging from 5 to 10 million g/mole. The differentiated polymers exhibited the desired properties such as particle size distribution (PSD), average particle size (APS), bulk density (BD) and molecular weight (MW) with controlled amount of fine and coarse particles. Scanning electron micrographs (SEM) reflected the material to have uniform particle size distribution with a spherical morphology. The extent of entanglement was determined from thermal studies and it was found to be highly entangled.

  10. Synthesis of Hydrophobic Mesoporous Material MFS and Its Adsorption Properties of Water Vapor

    Directory of Open Access Journals (Sweden)

    Guotao Zhao


    Full Text Available Fluorine-containing hydrophobic mesoporous material (MFS with high surface area is successfully synthesized with hydrothermal synthesis method by using a perfluorinated surfactant SURFLON S-386 template. The adsorption properties of water vapor on the synthesized MFS are also investigated by using gravimetric method. Results show that SEM image of the MFS depicted roundish morphology with the average crystal size of 1-2 μm. The BET surface area and total pore volume of the MFS are 865.4 m2 g−1 and 0.74 cm3 g−1 with a narrow pore size distribution at 4.9 nm. The amount of water vapor on the MFS is about 0.41 mmol g−1 at 303 K, which is only 52.6% and 55.4% of MCM-41 and SBA-15 under the similar conditions, separately. The isosteric adsorption heat of water on the MFS is gradually about 27.0–19.8 kJ mol−1, which decreases as the absorbed water vapor amount increases. The value is much smaller than that on MCM-41 and SBA-15. Therefore, the MFS shows more hydrophobic surface properties than the MCM-41 and SBA-15. It may be a kind of good candidate for adsorption of large molecule and catalyst carrier with high moisture resistance.

  11. New anthracene-based-phtalocyanine semi-conducting materials: Synthesis and optoelectronic properties

    Energy Technology Data Exchange (ETDEWEB)

    Kahouech, M.S. [Laboratoire de Chimie Organique et Analytique, Institut Supérieur de l' Education et de la Formation Continue (Université El Manar), Bardo 2000 (Tunisia); Hriz, K., E-mail: [Laboratoire des Interfaces et Matériaux Avancés (LIMA), Faculté des Sciences de Monastir (Université de Monastir), Bd. de l' Environnement, Monastir 5019 (Tunisia); Touaiti, S.; Bassem, J. [Laboratoire de Chimie Organique et Analytique, Institut Supérieur de l' Education et de la Formation Continue (Université El Manar), Bardo 2000 (Tunisia)


    Highlights: • Synthesis of tow phtalocyanines based on the anthracene and tetrazole. • Semi-conducting supramolecular material. • Good PL quantum yield. • The film morphology of the phtalocynine containing tetrazole group enhanced the carrier mobility. - Abstract: A new anthracene-based semi-conducting phtalocyanines AnPc and AnPc-Tr were synthesized in solvent-free conditions. The supramolecular structure of these compounds was confirmed by NMR and FT-IR spectroscopies. Their optical properties were investigated by UV–vis and photoluminescence spectroscopies. The optical gaps were estimated from the absorption-onsets films, and the obtained values were of 1.50 eV and 1.47 eV for AnPc-Tr and AnPc respectively. In solid state, a weaker π–π-interactions of conjugated systems were obtained in the case of AnPc-Tr in comparison with AnPc. This behavior was explained by steric hindrance of triazol groups, which decrease the planarity of macromolecular structure. The HOMO and LUMO levels were estimated using cyclic voltammetry analysis; two phtalocyanine derivatives show a comparable ionization potential. The phtalacyanine containing triazole groups (AnPc-Tr) reveals a higher electron affinity in comparison with AnPc. Single-layer diode devices were fabricated and showed relatively low turn-on voltages.

  12. One pot synthesis of opposing 'rose petal' and 'lotus leaf' superhydrophobic materials with zinc oxide nanorods. (United States)

    Myint, Myo Tay Zar; Hornyak, Gabor L; Dutta, Joydeep


    The synthesis in one pot(1) of opposing 'rose petal' and 'lotus leaf' superhydrophobic materials from commercially available superhydrophilic cloth substrates of varying texture is described for the first time. Surfaces of 'rough' textured cloth and 'smooth' textured cloth were simultaneously rendered superhydrophobic by growing zinc oxide (ZnO) nanorods by a hydrothermal process in the same chemical bath. Contact angle hysteresis and water pendant drop tests revealed strong water adhesion to ZnO microrod-treated rough cloth. The combination of water contact angle >150° and strong adhesion is indicative of the 'rose petal effect' with potential for water pinning. Smooth cloth with ZnO nanorods exhibited no adhesion to water droplets with facilitative roll-off. The combination of water contact angle >150° and weak to no adhesion with water is indicative of the 'lotus leaf effect' with potential for self-cleaning. Pendant water drop tests indicated cohesive failure of water on rough cloth coated with ZnO nanorods. Natural rose petals demonstrated adhesive failure between the petal surface and water droplet. A parsimonious explanation is presented. We also describe the development of superhydrophobic clothes without the need for special conditions or further chemical modification. Copyright © 2013 Elsevier Inc. All rights reserved.

  13. Epoxy resin synthesis using low molecular weight lignin separated from various lignocellulosic materials. (United States)

    Asada, Chikako; Basnet, Sunita; Otsuka, Masaya; Sasaki, Chizuru; Nakamura, Yoshitoshi


    A low molecular weight lignin from various lignocellulosic materials was used for the synthesis of bio-based epoxy resins. The lignin extracted with methanol from steam-exploded samples (steaming time of 5 min at steam pressure of 3.5 MPa) from different biomasses (i.e., cedar, eucalyptus, and bamboo) were functionalized by the reaction with epichlorohydrin, catalyzed by a water-soluble phase transfer catalyst tetramethylammonium chloride, which was further reacted with 30 wt% aqueous NaOH for ring closure using methyl ethyl ketone as a solvent. The glycidylated products of the lignin with good yields were cured to epoxy polymer networks with bio-based curing agents i.e., lignin itself and a commercial curing agent TD2131. Relatively good thermal properties of the bio-based epoxy network was obtained and thermal decomposition temperature at 5% weight loss (Td5) of cedar-derived epoxy resin was higher than that derived from eucalyptus and bamboo. The bio-based resin satisfies the stability requirement of epoxy resin applicable for electric circuit boards. The methanol-insoluble residues were enzymatically hydrolyzed to produce glucose. This study indicated that the biomass-derived methanol-soluble lignin may be a promising candidate to be used as a substitute for petroleum-based epoxy resin derived from bisphenol A, while insoluble residues may be processed to give a bioethanol precursor i.e., glucose. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Materials and vapour-phase techniques for the synthesis of ceramic coatings

    Directory of Open Access Journals (Sweden)

    Albella, J. M.


    Full Text Available A survey on recent advances in the synthesis of hard ceramic coatings is given, including materials processes and techniques. Emphasis is made on the parameters which control the coating properties (crystalline structure, morphology, etc, namely arrival energy of the atoms to the growing surface and substrate temperature. Some relevant coating materials are discussed in relation to their applications either as hard protective coatings or with decorative purposes, namely: the family of metal nitrides, carbides, and oxides, in different layer structures (monolithic, multilayers and nanocomposites and ternary compounds of the BCN system.

    Se hace un descripción de los avances recientes en la síntesis de recubrimientos duros de tipo cerámico, depositados mediante técnicas de deposición en fase vapor. Se dedica especial atención a los parámetros del proceso de deposición que controlan las propiedades finales de las capas (estructura cristalina, morfología, etc, tales como la energía de llegada de los átomos a las superficie en crecimiento, y la temperatura. Finalmente, se hace una revisión de los materiales más relevantes en lo que se refiere a sus aplicaciones como recubrimientos duros y protectores, o como recubrimientos decorativos, entre ellos, la familia de los nitruros, carburos y óxidos metálicos, depositados en diversos tipos de estructuras (monolíticas, multicapas y nanocomposites, y los compuestos ternarios del sistema BCN.

  15. Gold Nanoparticle Synthesis by 3D Integrated Micro-solution Plasma in a 3D Printed Artificial Porous Dielectric Material (United States)

    Sotoda, Naoya; Tanaka, Kenji; Shirafuji, Tatsuru


    Plasma in contact with HAuCl4 aqueous solution can promote the synthesis of gold nanoparticles. To scale up this process, we have developed 3D integrated micro-solution plasma (3D IMSP). It can generate a large number of argon microplasmas in contact with the aqueous solution flowing in a porous dielectric material. The porous dielectric material in our prototype 3D IMSP reactor, however, consists of non-regularly arranged random-sized pores. These pore parameters may be the parameters for controlling the size and dispersion of synthesized gold nanoparticles. We have hence fabricated a 3D IMSP reactor with an artificial porous dielectric material that has regularly arranged same-sized pores by using a 3D printer. We have applied the reactor to the gold- nanoparticle synthesis. We have confirmed the synthesis of gold nanoparticles through the observation of a plasmon resonance absorption peak at 550 nm in the HAuCl4 aqueous solution treated with 3D IMSP. The size and distribution of the synthesized gold nanoparticles are under investigation. We expect that these characteristics of the gold nanoparticles can be manipulated by changing pore size and their distribution in the porous dielectric material.

  16. Materials Research Society Symposium Proceedings Volume 635. Anisotropic Nanoparticles - Synthesis, Characterization and Applications

    National Research Council Canada - National Science Library

    Lyon, L


    This volume contains a series of papers originally presented at Symposium C, "Anisotropic Nanoparticles Synthesis, Characterization and Applications," at the 2000 MRS Fall Meeting in Boston, Massachusetts...

  17. Hydrothermal synthesis of new rare earth silicate fluorides: A novel class of polar materials

    Energy Technology Data Exchange (ETDEWEB)

    McMillen, Colin D., E-mail: [Department of Chemistry and Center for Optical Materials Science and Engineering Technologies (COMSET), Clemson University, 485 H.L. Hunter Laboratories, Clemson, SC 29634 (United States); Emirdag-Eanes, Mehtap, E-mail: [Department of Chemistry, Izmir Institute of Technology, Gulbahce koyu, Urla, Izmir 35430 (Turkey); Stritzinger, Jared T., E-mail: [Department of Chemistry and Center for Optical Materials Science and Engineering Technologies (COMSET), Clemson University, 485 H.L. Hunter Laboratories, Clemson, SC 29634 (United States); Kolis, Joseph W., E-mail: [Department of Chemistry and Center for Optical Materials Science and Engineering Technologies (COMSET), Clemson University, 485 H.L. Hunter Laboratories, Clemson, SC 29634 (United States)


    Polar crystals provide an interesting avenue for materials research both in the structures they form and the properties they possess. This work describes the hydrothermal synthesis and structural characterization of three novel silicate fluorides. Compound (1), LiY{sub 3}(SiO{sub 4}){sub 2}F{sub 2} crystallizes in space group C2/c, with a=17.651(4) A, b=4.8868(10) A, c=11.625(2) A and {beta}=131.13(3) Degree-Sign . BaY{sub 2}(Si{sub 2}O{sub 7})F{sub 2} (2) crystallizes in space group P-1, with a=5.1576(10) A, b=6.8389(14) A, c=11.786(2) A, {alpha}=93.02(3) Degree-Sign , {beta}=102.05(3) Degree-Sign and {gamma}=111.55(3) Degree-Sign . Finally, the structure of Ba{sub 2}Y{sub 3}(SiO{sub 4}){sub 2}F{sub 5} (3) was determined in the polar orthorhombic space group Pba2, having unit cell parameters a=8.8864(18) A, b=12.764(3) A and c=5.0843(10) A. The structures are compared based on their building blocks and long range polarities. Aligned silicate tetrahedra segregated into a single layer in (3) impart the observed polarity. - Graphical abstract: The polar structure of Ba{sub 2}Y{sub 3}(SiO{sub 4}){sub 2}F{sub 5}. Highlights: Black-Right-Pointing-Pointer Natural yttrium silicate fluoride minerals are briefly reviewed. Black-Right-Pointing-Pointer The synthesis and structures of LiY{sub 3}(SiO{sub 4}){sub 2}F{sub 2}, BaY{sub 2}(Si{sub 2}O{sub 7})F{sub 2} and Ba{sub 2}Y{sub 3}(SiO{sub 4}){sub 2}F{sub 5} are discussed. Black-Right-Pointing-Pointer Ba{sub 2}Y{sub 3}(SiO{sub 4}){sub 2}F{sub 5} crystallizes in the polar space group Pba2. Black-Right-Pointing-Pointer Polarity occurs primarily through aligned silicate tetrahedra in a segregated layer.

  18. Microwave Plasma Synthesis of Materials—From Physics and Chemistry to Nanoparticles: A Materials Scientist’s Viewpoint

    Directory of Open Access Journals (Sweden)

    Dorothée Vinga Szabó


    Full Text Available In this review, microwave plasma gas-phase synthesis of inorganic materials and material groups is discussed from the application-oriented perspective of a materials scientist: why and how microwave plasmas are applied for the synthesis of materials? First, key players in this research field will be identified, and a brief overview on publication history on this topic is given. The fundamental basics, necessary to understand the processes ongoing in particle synthesis—one of the main applications of microwave plasma processes—and the influence of the relevant experimental parameters on the resulting particles and their properties will be addressed. The benefit of using microwave plasma instead of conventional gas phase processes with respect to chemical reactivity and crystallite nucleation will be reviewed. The criteria, how to choose an appropriate precursor to synthesize a specific material with an intended application is discussed. A tabular overview on all type of materials synthesized in microwave plasmas and other plasma methods will be given, including relevant citations. Finally, property examples of three groups of nanomaterials synthesized with microwave plasma methods, bare Fe2O3 nanoparticles, different core/shell ceramic/organic shell nanoparticles, and Sn-based nanocomposites, will be described exemplarily, comprising perspectives of applications.

  19. Optimization of the freezing process for hematopoietic progenitor cells: effect of precooling, initial dimethyl sulfoxide concentration, freezing program, and storage in vapor-phase or liquid nitrogen on in vitro white blood cell quality. (United States)

    Dijkstra-Tiekstra, Margriet J; Setroikromo, Airies C; Kraan, Marcha; Gkoumassi, Effimia; de Wildt-Eggen, Janny


    Adding dimethyl sulfoxide (DMSO) to hematopoietic progenitor cells (HPCs) causes an exothermic reaction, potentially affecting their viability. The freezing method might also influence this. The aim was to investigate the effect of 1) precooling of DMSO and plasma (D/P) and white blood cell (WBC)-enriched product, 2) DMSO concentration of D/P, 3) freezing program, and 4) storage method on WBC quality. WBC-enriched product without CD34+ cells was used instead of HPCs. This was divided into six or eight portions. D/P (20 or 50%; precooled or room temperature [RT]) was added to the WBC-enriched product (precooled or RT), resulting in 10% DMSO, while monitoring temperature. The product was frozen using controlled-rate freezing ("fast-rate" or "slow-rate") and placed in vapor-phase or liquid nitrogen. After thawing, WBC recovery and viability were determined. Temperature increased most for precooled D/P to precooled WBC-enriched product, without influence of 20 or 50% D/P, but remained for all variations below 30°C. WBC recovery for both freezing programs was more than 95%. Recovery of WBC viability was higher for slow-rate freezing compared to fast-rate freezing (74% vs. 61%; p Effect of precooling D/P or WBC-enriched product and of storage in vapor-phase or liquid nitrogen was marginal. Based on these results, precooling is not necessary. Fifty percent D/P is preferred over 20% D/P. Slow-rate freezing is preferred over fast-rate freezing. For safety reasons storage in vapor-phase nitrogen is preferred over storage in liquid nitrogen. Additional testing using real HPCs might be necessary. © 2014 AABB.

  20. Precision synthesis of functional materials via RAFT polymerization and click-type chemical reactions (United States)

    Flores, Joel Diez


    The need to tailor polymeric architectures with specific physico-chemical properties via the simplest, cleanest, and most efficient synthetic route possible has become the ultimate goal in polymer synthesis. Recent progress in macromolecular science, such as the discoveries of controlled/"living" free radical polymerization (CRP) methods, has brought about synthetic capabilities to prepare (co)polymers with advanced topologies, predetermined molecular weights, narrow molecular weight distributions, and precisely located functional groups. In addition, the establishment of click chemistry has redefined the selected few highly efficient chemical reactions that become highly useful in post-polymerization modification strategies. Hence, the ability to make well-defined topologies afforded by controlled polymerization techniques and the facile incorporation of functionalities along the chain via click-type reactions have yielded complex architectures, allowing the investigation of physical phenomena which otherwise could not be studied with systems prepared via conventional methods. The overarching theme of the research work described in this dissertation is the fusion of the excellent attributes of reversible addition-fragmentation chain transfer (RAFT) polymerization method, which is one of the CRP techniques, and click-type chemical reactions in the precision of synthesis of advanced functional materials. Chapter IV is divided into three sections. In Section I, the direct RAFT homopolymerization of 2-(acryloyloxy)ethyl isocyanate (AOI) and subsequent post-polymerization modifications are described. The polymerization conditions were optimized in terms of the choice of RAFT chain transfer agent (CTA), polymerization temperature and the reaction medium. Direct RAFT polymerization of AOI requires a neutral CTA, and relatively low reaction temperature to yield AOI homopolymers with low polydispersities. Efficient side-chain functionalization of PAOI homopolymers was

  1. UV Raman spectroscopic studies on active sites and synthesis mechanisms of transition metal-containing microporous and mesoporous materials. (United States)

    Fan, Fengtao; Feng, Zhaochi; Li, Can


    Microporous and mesoporous materials are widely used as catalysts and catalyst supports. Although the incorporation of transition metal ions into the framework of these materials (by isomorphous substitution of Al and Si) is an effective means of creating novel catalytic activity, the characterization of the transition metal species within these materials is difficult. Both the low concentration of the highly dispersed transition metal and the coexistence of extraframework transition metal species present clear challenges. Moreover, the synthetic mechanisms that operate under the highly inhomogeneous conditions of hydrothermal synthesis are far from well understood. A useful technique for addressing these challenges is UV Raman spectroscopy, which is a powerful technique for catalyst characterization and particularly for transition metal-containing microporous and mesoporous materials. Conventional Raman spectroscopy, using visible and IR wavelengths, often fails to provide the information needed for proper characterization as a result of fluorescence interference. But shifting the excitation source to the UV range addresses this difficulty: interference from fluorescence (which typically occurs at 300-700 nm or greater) is greatly diminished. Moreover, signal intensity is enhanced because Raman intensity is proportional to the fourth power of the scattered light frequency. In this Account, we review recent advances in UV Raman spectroscopic characterization of (i) highly dispersed transition metal oxides on supports, (ii) transition metal ions in the framework of microporous and mesoporous materials, and (iii) the synthetic mechanisms involved in making microporous materials. By taking advantage of the strong UV resonance Raman effect, researchers have made tremendous progress in the identification of isolated transition metal ions incorporated in the framework of microporous and mesoporous materials such as TS-1, Ti-MCM-41, Fe-ZSM-5, and Fe-SBA-15. The synthetic

  2. Controlled synthesis of LiNi0.5Mn1.5O4 cathode materials with superior electrochemical performance through urea-based solution combustion synthesis


    Zhu, Chunyu; Han, Cheng-gong; Akiyama, Tomohiro


    High-voltage LiNi0.5Mn1.5O4 cathode materials were synthesized using urea-based solution combustion synthesis combined with a calcination treatment. The morphology and particle size distribution of the products were considerably dependent on the amount of urea fuel. The electrochemical characterization illustrated that the sample that was produced with a fuel ratio of phi = 0.5 had a homogenous particle size distribution of approximately 8 mu m, and showed the best cycling and rate performanc...

  3. Novel Approach toward 3,3-Difluoropiperidines from Easily Available Starting Materials and Synthesis of a New Phosphodiesterase Inhibitor

    DEFF Research Database (Denmark)

    Giacoboni, Jessica; Clausen, Rasmus P.; Marigo, Mauro


    A novel methodology for the synthesis of 3,3-difluoropiperidines has been developed. The target compounds are prepared in three steps using a robust protocol and simple starting materials. The incorporation of the fluorine is achieved by using the cheap and easily available ethyl 2-bromo-2,2-difl......,2-difluoroacetate as building block. Using this methodology, a new potent in vitro phosphodiesterase 2A (PDE2A) inhibitor containing the functionalized fluorinated piperidine scaffold has been prepared....

  4. In situ-Raman studies on thermally induced structural changes of porous MoO{sub 3} prepared in vapor phase under He and H{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Diaz-Droguett, D.E., E-mail: [Departamento de Fisica, Facultad de Fisica, Pontificia Universidad Catolica de Chile, Santiago (Chile); El Far, R. [Departamento de Fisica, Facultad de Fisica, Pontificia Universidad Catolica de Chile, Santiago (Chile); Fuenzalida, V.M. [Departamento de Fisica, Facultad de Ciencias Fisicas y Matematicas, Universidad de Chile, Santiago (Chile); Cabrera, A.L. [Departamento de Fisica, Facultad de Fisica, Pontificia Universidad Catolica de Chile, Santiago (Chile)


    The structural transformations induced by heating on MoO{sub 3} mesoporous samples grown in vapor-phase under helium and hydrogen were studied by in situ Raman spectroscopy. The samples were continuously irradiated by a He-Ne laser of 5.5 mW for 105 min and Raman spectra were dynamically acquired every 5 min, in order to evaluate the laser effects. The He-grown sample did not undergo structural transformations due to the laser irradiation while the H{sub 2}-grown sample underwent changes after just 10 min of irradiation. On the other hand, each type of sample was heated in air from room temperature up to 450 Degree-Sign C using a heating rate of 5 Degree-Sign C min{sup -1} and Raman spectra were recorded each 25 Degree-Sign C. The He-grown sample remained structural unchanged up to 250 Degree-Sign C revealing a high temperature state of its amorphous matrix whereas the H{sub 2}-grown sample exhibited changes around 70 Degree-Sign C. These changes were attributed to the crystallization onset of its amorphous matrix to {beta}-MoO{sub 3}. However, this same transition was detected between 250 Degree-Sign C and 275 Degree-Sign C for the He-grown sample. A second transformation was detected in both samples in a temperature range more similar associated to the transition of the formed {beta}-MoO{sub 3} phase to {alpha}-MoO{sub 3}. After the heat treatment, the oxide of both samples was slightly reduced, as revealed by XPS analysis. The metastability at low temperatures of the amorphous phase of the H{sub 2}-grown sample could be associated to release of hydrogen trapped inside the compound and to the break of weak bonds between Mo and OH groups. At high temperatures, above 225 Degree-Sign C, the rapid conversion to {beta}-MoO{sub 3} of the amorphous matrix of the H{sub 2}-grown sample occurred due to the dehydration of the sample. - Highlights: Black-Right-Pointing-Pointer Porous MoO{sub 3} grown in He or H{sub 2} showed structural differences by heating effects. Black

  5. Long Term Field Development of a Surfactant Modified Zeolite/Vapor Phase Bioreactor System for Treatment of Produced Waters for Power Generation

    Energy Technology Data Exchange (ETDEWEB)

    Lynn Katz; Kerry Kinney; Robert Bowman; Enid Sullivan; Soondong Kwon; Elaine Darby; Li-Jung Chen; Craig Altare


    The main goal of this research was to investigate the feasibility of using a combined physicochemical/biological treatment system to remove the organic constituents present in saline produced water. In order to meet this objective, a physical/chemical adsorption process was developed and two separate biological treatment techniques were investigated. Two previous research projects focused on the development of the surfactant modified zeolite adsorption process (DE-AC26-99BC15221) and development of a vapor phase biofilter (VPB) to treat the regeneration off-gas from the surfactant modified zeolite (SMZ) adsorption system (DE-FC26-02NT15461). In this research, the SMZ/VPB was modified to more effectively attenuate peak loads and to maintain stable biodegradation of the BTEX constituents from the produced water. Specifically, a load equalization system was incorporated into the regeneration flow stream. In addition, a membrane bioreactor (MBR) system was tested for its ability to simultaneously remove the aromatic hydrocarbon and carboxylate components from produced water. The specific objectives related to these efforts included the following: (1) Optimize the performance VPBs treating the transient loading expected during SMZ regeneration: (a) Evaluate the impact of biofilter operating parameters on process performance under stable operating conditions. (b) Investigate how transient loads affect biofilter performance, and identify an appropriate technology to improve biological treatment performance during the transient regeneration period of an SMZ adsorption system. (c) Examine the merits of a load equalization technology to attenuate peak VOC loads prior to a VPB system. (d) Evaluate the capability of an SMZ/VPB to remove BTEX from produced water in a field trial. (2) Investigate the feasibility of MBR treatment of produced water: (a) Evaluate the biodegradation of carboxylates and BTEX constituents from synthetic produced water in a laboratory-scale MBR. (b

  6. Fabrication and characterization of freestanding GaAs/AlGaAs core-shell nanowires and AlGaAs nanotubes by using selective-area metalorganic vapor phase epitaxy


    Noborisaka, J.; Motohisa, J.; S. Hara; Fukui, T.


    We fabricated GaAs/AlGaAs core-shell nanowires by using selective-area metalorganic vapor phase epitaxy. First, GaAs nanowires were selectively grown on partially masked GaAs (111)B substrates; then AlGaAs was grown to form freestanding heterostructured nanowires. Investigation of nanowire diameter as a function of AlGaAs growth time suggested that the AlGaAs was grown on the sidewalls of the GaAs nanowires, forming GaAs/AlGaAs core-shell structures. Microphotoluminescence measurements of GaA...

  7. Synthesis and characterization of bismuth telluride based nanostructured thermoelectric composite materials (United States)

    Keshavarz Khorasgani, Mohsen

    Thermoelectric (TE) materials and devices are attractive in solid-state energy conversion applications such as waste heat recovery, air-conditioning, and refrigeration. Since the 1950's lots of unremitting efforts have been made to enhance the efficiency of energy conversion in TE materials (i. e. improving the figure of merit (ZT)), however, most of commercial bulk TE materials still suffer from low efficiency with ZTs around unity. To enhance the performance of bismuth telluride based TE alloys, we have developed composite TE materials, based on the idea that introducing more engineered interfaces in the bulk TE materials may lead to thermal conductivity reduction due to increased phonon scattering by these interfaces. In this approach it is expected that the electronic transport properties of the material are not effectively affected. Consequently, ZT enhancement can be achieved. In this dissertation we will discuss synthesis and characterization of two types of bismuth telluride based bulk composite TE materials. The first type is engineered to contain the presence of coherent interfaces between phases in the material resulting from different mixtures of totally miscible compounds with similar composition. The second type includes the nanocomposites with embedded foreign nano-particles in which the matrix and the particles are delimited by incoherent interfaces. The synthesis procedure, micro- and nano-structures as well as thermoelectric properties of these composites will be presented. In our study on the composites with coherent interfaces, we produced a series of different composites of p-type bismuth antimony telluride alloys and studied their microstructure and thermoelectric properties. Each composite consists of two phases that were obtained in powder form by mechanical alloying. Mixed powders in various proportions of the two different phases were consolidated by hot extrusion to obtain each bulk composite. The minimum grain size of bulk composites as

  8. Molten salt-directed synthesis method for LiMn2O4 nanorods as a cathode material for a lithium-ion battery with superior cyclability

    CSIR Research Space (South Africa)

    Kebede, Mesfin A


    Full Text Available A molten salt synthesis technique has been used to prepare nanorods of Mn2O3 and single-crystal LiMn2O4 nanorods cathode material with superior capacity retention. The molten salt-directed synthesis involved the use of NaCl as the eutectic melt...

  9. Low-temperature plasma synthesis of carbon nanotubes and graphene based materials and their fuel cell applications. (United States)

    Wang, Qi; Wang, Xiangke; Chai, Zhifang; Hu, Wenping


    Carbon nanotubes (CNTs) and graphene, and materials based on these, are largely used in multidisciplinary fields. Many techniques have been put forward to synthesize them. Among all kinds of approaches, the low-temperature plasma approach is widely used due to its numerous advantages, such as highly distributed active species, reduced energy requirements, enhanced catalyst activation, shortened operation time and decreased environmental pollution. This tutorial review focuses on the recent development of plasma synthesis of CNTs and graphene based materials and their electrochemical application in fuel cells.

  10. Modelling materials for solar fuel synthesis by artificial photosynthesis; predicting the optical, electronic and redox properties of photocatalysts. (United States)

    Guiglion, Pierre; Berardo, Enrico; Butchosa, Cristina; Wobbe, Milena C C; Zwijnenburg, Martijn A


    In this mini-review, we discuss what insight computational modelling can provide into the working of photocatalysts for solar fuel synthesis and how calculations can be used to screen for new promising materials for photocatalytic water splitting and carbon dioxide reduction. We will extensively discuss the different relevant (material) properties and the computational approaches (DFT, TD-DFT, GW/BSE) available to model them. We illustrate this with examples from the literature, focussing on polymeric and nanoparticle photocatalysts. We finish with a perspective on the outstanding conceptual and computational challenges.

  11. Synthesis of AgGaGeS4 polycrystalline materials by vapor transporting and mechanical oscillation method (United States)

    Huang, Wei; Zhao, Beijun; Zhu, Shifu; He, Zhiyu; Chen, Baojun; Pu, Yunxiao; Lin, Li; Zhao, Zhangrui; Zhong, Yikai


    Single-phase AgGaGeS4 polycrystalline materials were synthesized directly from the constituent elements by vapor transporting and mechanical oscillation method. The problem of explosions was solved by careful control of the heating and cooling cycle and adopting the two-zone rocking furnace with specially designed temperature profile. The mechanical and temperature oscillations, as well as gradient cooling, were introduced in the synthesis process. The X-ray diffraction (XRD) analysis and Energy Dispersive Spectrometer (EDS) micro analysis indicated that the synthesized compound is a single-phase AgGaGeS4 polycrystalline material.

  12. Modelling materials for solar fuel synthesis by artificial photosynthesis; predicting the optical, electronic and redox properties of photocatalysts (United States)

    Guiglion, Pierre; Berardo, Enrico; Butchosa, Cristina; Wobbe, Milena C. C.; Zwijnenburg, Martijn A.


    In this mini-review, we discuss what insight computational modelling can provide into the working of photocatalysts for solar fuel synthesis and how calculations can be used to screen for new promising materials for photocatalytic water splitting and carbon dioxide reduction. We will extensively discuss the different relevant (material) properties and the computational approaches (DFT, TD-DFT, GW/BSE) available to model them. We illustrate this with examples from the literature, focussing on polymeric and nanoparticle photocatalysts. We finish with a perspective on the outstanding conceptual and computational challenges.

  13. Synthesis of nanostructured materials by using metal-cyanide coordination polymers and their lithium storage properties. (United States)

    Nie, Ping; Shen, Laifa; Luo, Haifeng; Li, Hongsen; Xu, Guiyin; Zhang, Xiaogang


    Herein, we demonstrate a novel and simple two-step process for preparing LiCoO2 nanocrystals by using a Prussian blue analogue Co3[Co(CN)6]2 as a precursor. The resultant LiCoO2 nanoparticles possess single crystalline nature and good uniformity with an average size of ca. 360 nm. The unique nanostructure of LiCoO2 provides relatively shorter Li(+) diffusion pathways, thus facilitating the fast kinetics of electrochemical reactions. As a consequence, high reversible capacity, excellent cycling stability and rate capability are achieved with these nanocrystals as cathodes for lithium storage. The LiCoO2 nanocrystals deliver specific capacities of 154.5, 135.8, 119, and 100.3 mA h g(-1) at 0.2, 0.4, 1, and 2 C rates, respectively. Even at a high current density of 4 C, a reversible capacity of 87 mA h g(-1) could be maintained. Importantly, a capacity retention of 83.4% after 100 cycles is achieved at a constant discharge rate of 1 C. Furthermore, owing to facile control of the morphology and size of Prussian blue analogues by varying process parameters, as well as the tailored design of multi-component metal-cyanide hybrid coordination polymers, with which we have successfully prepared porous Fe2O3@NixCo3-xO4 nanocubes, one of the potential anode materials for lithium-ion batteries, such a simple and scalable approach could also be applied to the synthesis of other nanomaterials for energy storage devices.


    Directory of Open Access Journals (Sweden)

    Drábik M.


    Full Text Available A challenge in the field of MDF materials, which has not been followed or indicated by now, are the options of improvement of cross-linking through intensified mixing of dry MDF raw mixes of cement and polymer. The potential of mechanochemical treatment to intensify the atomic level of cross-linking already in the raw mixes and, thus, the activation of raw mixes has been critically verified earlier. Processes of the mutual MDF syntheses of both standard and activated raw mixes are presented and discussed in this paper. The scope of cross-linking as a key item of the successful MDF synthesis has been studied by two independent experimental methods – thermal analysis and IR spectroscopy. The knowledge has been achieved about (i phenomenon of internal pressure during MDF synthesis from mechanochemically activated raw mixtures and (ii increase of the content of cross-links by one third in MDF materials synthesized from mechanochemically activated raw mixtures in comparison with these synthesized from standard raw mixtures. Mechanochemical activation of raw mixtures undoubtedly leads to the intensification of cross-linking in MDF materials; if applied (prior to water addition and pressure application it increases the rate of cross-links formation in the system through the effect of internal pressure. The reported approach and results represent besides the contribution to the knowledge about MDF materials themselves also the challenge for the development of a variety of new and innovative materials strategies.

  15. Design, Synthesis, and Characterization of Nanostructured Materials for Energy Storage Devices and Flexible Chemical Sensors (United States)

    Kang, Ning

    Nanomaterials have shown increasing applications in the design and fabrication of functional devices such as energy storage devices and sensor devices. A key challenge is the ability to harness the nanostructures in terms of size, shape, composition and structure so that the unique nanoscale functional properties can be exploited. This dissertation describes our findings in design, synthesis, and characterization of nanoparticles towards applications in two important fronts. The first involves the investigation of nanoalloy catalysts and functional nanoparticles for energy storage devices, including Li-air and Li-ion batteries, aiming at increasing the capacity and cycle performance. Part of this effort focuses on design of bifunctional nanocatalysts through alloying noble metal with non-noble transition metal to improve the ORR and OER activity of Li-air batteries. By manipulating the composition and alloying structure of the catalysts, synergetic effect has been demonstrated, which is substantiated by both experimental results and theoretical calculation for the charge/discharge process. The other part of the effort focuses on modification of Si nanoparticles towards high-capacity anode materials. The modification involved dopant elements, carbon coating, and graphene composite formation to manipulate the ability of the nanoparticles in accommodating the volume expansion. The second part focuses on the design, preparation and characterization of metal nanoparticles and nanocomposite materials for the application in flexible sensing devices. The investigation focuses on fabrication of a novel class of nanoparticle-nanofibrous membranes consisting of gold nanoparticles embedded in a multi-layered fibrous membrane as a tunable interfacial scaffold for flexible sweat sensors. Sensing responses to different ionic species in aqueous solutions and relative humidity changes in the environment were demonstrated, showing promising potential as flexible sensing devices for

  16. Policaprolactone/polyvinylpyrrolidone/siloxane hybrid materials: Synthesis and in vitro delivery of diclofenac and biocompatibility with periodontal ligament fibroblasts. (United States)

    Peña, José A; Gutiérrez, Sandra J; Villamil, Jean C; Agudelo, Natalia A; Pérez, León D


    In this paper, we report the synthesis of polycaprolactone (PCL) based hybrid materials containing hydrophilic domains composed of N-vinylpyrrolidone (VP), and γ-methacryloxypropyltrimethoxysilane (MPS). The hybrid materials were obtained by RAFT copolymerization of N-vinylpyrrolidone and MPS using a pre-formed dixanthate-end-functionalized PCL as macro-chain transfer agent, followed by a post-reaction crosslinking step. The composition of the samples was determined by elemental and thermogravimetric analyses. Differential scanning calorimetry and X-ray diffraction indicated that the crystallinity of PCL decreases in the presence of the hydrophilic domains. Scanning electron microscopy images revealed that the samples present an interconnected porous structure on the swelling. Compared to PCL, the hybrid materials presented low water contact angle values and higher elastic modulus. These materials showed controlled release of diclofenac, and biocompatibility with human periodontal ligament fibroblasts. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. Quick high-temperature hydrothermal synthesis of mesoporous materials with 3D cubic structure for the adsorption of lysozyme. (United States)

    Lawrence, Geoffrey; Baskar, Arun V; El-Newehy, Mohammed H; Cha, Wang Soo; Al-Deyab, Salem S; Vinu, Ajayan


    Three-dimensional cage-like mesoporous FDU-12 materials with large tuneable pore sizes ranging from 9.9 to 15.6 nm were prepared by varying the synthesis temperature from 100 to 200 °C for the aging time of just 2 h using a tri-block copolymer F-127(EO106PO70EO106) as the surfactant and 1,3,5-trimethyl benzene as the swelling agent in an acidic condition. The mesoporous structure and textural features of FDU-12-HX (where H denotes the hydrothermal method and X denotes the synthesis temperature) samples were elucidated and probed using x-ray diffraction, N2 adsorption, (29)Si magic angle spinning nuclear magnetic resonance, scanning electron microscopy and transmission electron microscopy. It has been demonstrated that the aging time can be significantly reduced from 72 to 2 h without affecting the structural order of the FDU-12 materials with a simple adjustment of the synthesis temperature from 100 to 200 °C. Among the materials prepared, the samples prepared at 200 °C had the highest pore volume and the largest pore diameter. Lysozyme adsorption experiments were conducted over FDU-12 samples prepared at different temperatures in order to understand their biomolecule adsorption capacity, where the FDU-12-HX samples displayed high adsorption performance of 29 μmol g(-1) in spite of shortening the actual synthesis time from 72 to 2 h. Further, the influence of surface area, pore volume and pore diameter on the adsorption capacity of FDU-12-HX samples has been investigated and results are discussed in correlation with the textural parameters of the FDU-12-HX and other mesoporous adsorbents including SBA-15, MCM-41, KIT-5, KIT-6 and CMK-3.

  18. Nanocomposite Materials alfa-Fe2O3 / gamma-Fe2O3:Synthesis, Crystal and Magnetic Microstructure, Morphology


    V.О. Kotsyubynsky; V.V. Mokliak; A.B.Grubiak; P.I. Kolkovsky; Al-Saedi Abdul Halek Zamil


    The paper studies the relationship between the synthesis conditions of nanocomposites α-Fe2O3 /  γ-Fe2O3 and the phase composition, morphology, crystal and magnetic microstructures of these materials.

  19. Synthesis and characterization of rare earth doped novel optical materials and their potential applications (United States)

    Pokhrel, Madhab

    There are many application of photonic materials but selection of photonic materials are always constrained by number of factors such as cost, availability of materials, thermal and chemical stability, toxicity, size and more importantly ease of synthesis and processing along with the efficient emission. For example, quantum dots are efficient emitter but they are significantly toxic, whereas dyes are also efficient emitters but they are chemically unstable. On the other hand, display and LED requires the micron size particles but bio application requires the nano-sized particles. On the other hand, laser gain media requires the ceramics glass or single crystal not the nanoparticles. So, realization of practical optical systems critically depends on suitable materials that offer specific combinations of properties. Solid-state powders such as rare-earth ions doped nano and micron size phosphors are one of the most promising candidates for several photonic applications discussed above. In this dissertation, we investigate the upconversion (UC) fluorescence characteristics of rare earth (RE) doped M2O2S (M = Y, Gd, La) oxysulphide phosphors, for near-infrared to visible UC. Both nano and micron size phosphors were investigated depending on their applications of interest. This oxysulphide phosphor possesses several excellent properties such as chemical stability, low toxicity and can be easily mass produced at low cost. Mainly, Yb3+, Er3+, and Ho3+ were doped in the host lattice, resulting in bright red, green, blue and NIR emissions under 980 nm and 1550 nm excitation at various excitation power densities. Maximum UC quantum yields (QY) up to 6.2 %, 5.8%, and 4.6% were respectively achieved in Yb3+/Er3+ :La2O2S, Y2O2S, and Gd2O 2S. Comparisons have been made with respect to reported most efficient upconverting phosphors beta-NaYF4:20 % Yb/ 2% Er. We believe that present phosphors are the most efficient and lower excitation threshold upconverting phosphors at 980 and

  20. Synthesis of microporous material faujasite-type from kaolin waste; Sintese de material microporoso do tipo faujasita a partir de rejeito de caulim

    Energy Technology Data Exchange (ETDEWEB)

    Hildebrando, E.A.; Valenzuela-Diaz, F.R., E-mail: edemarino@usp.b [Universidade de Sao Paulo (USP), SP (Brazil). Dept. de Engenharia Metalurgica e de Materiais. Lab. de Materias-Primas Particuladas e Solidos nao Metalicos; Angelica, R.S. [Universidade Federal do Para (UFPA), Belem, PA (Brazil). Inst. de Geociencias. Fac. de Geologia; Neves, R.F. [Universidade Federal do Para (UFPA), Belem, PA (Brazil). Inst. de Tecnologia. Fac. de Engenharia Quimica


    Zeolite with structure faujasite was synthesized using kaolin waste from kaolin processing industries for paper coating as predominant source of silicon and aluminum; the starting material was characterized by XRF, XRD, DTA/TG, SEM, and products obtained by XRD and SEM. Synthesis in hydrothermal conditions occurred on autoclave and time-temperature effects, as well as the relationship Si/Al were considered. The results show that the methodology developed with the waste of calcined kaolin reacting at 90 deg C for 20 hours in an alkaline medium, in the presence of an additional source of silica was obtained zeolite Y as single phase present in the product. (author)

  1. Synthesis and characterization of cycloaliphatic hydrophilic polyurethanes, modified with l-ascorbic acid, as materials for soft tissue regeneration. (United States)

    Kucinska-Lipka, J; Gubanska, I; Strankowski, M; Cieśliński, H; Filipowicz, N; Janik, H


    In this paper we described synthesis and characteristic of obtained hydrophilic polyurethanes (PURs) modified with ascorbic acid (commonly known as vitamin C). Such materials may find an application in the biomedical field, for example in the regenerative medicine of soft tissues, according to ascorbic acid wide influence on tissue regeneration Flora (2009), Szymańska-Pasternak et al. (2011), Taikarimi and Ibrahim (2011), Myrvik and Volk (1954), Li et al. (2001), Cursino et al. (2005) . Hydrophilic PURs were obtained with the use of amorphous α,ω-dihydroxy(ethylene-butylene adipate) (dHEBA) polyol, 1,4-butanediol (BDO) chain extender and aliphatic 4,4'-methylenebis(cyclohexyl isocyanate) (HMDI). HMDI was chosen as a nontoxic diisocyanate, suitable for biomedical PUR synthesis. Modification with l-ascorbic acid (AA) was performed to improve obtained PUR materials biocompatibility. Chemical structure of obtained PURs was provided and confirmed by Fourier transform infrared spectroscopy (FTIR) and Proton nuclear magnetic resonance spectroscopy ( 1 HNMR). Differential scanning calorimetry (DSC) was used to indicate the influence of ascorbic acid modification on such parameters as glass transition temperature, melting temperature and melting enthalpies of obtained materials. To determine how these materials may potentially behave, after implementation in tissue, degradation behavior of obtained PURs in various chemical environments, which were represented by canola oil, saline solution, distilled water and phosphate buffered saline (PBS) was estimated. The influence of AA on hydrophilic-hydrophobic character of obtained PURs was established by contact angle study. This experiment revealed that ascorbic acid significantly improves hydrophilicity of obtained PUR materials and the same cause that they are more suitable candidates for biomedical applications. Good hemocompatibility characteristic of studied PUR materials was confirmed by the hemocompatibility test with

  2. Plasma-chemical synthesis of carbon nanotubes and fullerenes to create frost-resistant composite building materials (United States)

    Semenov, A. P.; Smirnyagina, N. N.; Tsyrenov, B. O.; Dasheev, D. E.; Khaltarov, Z. M.


    This paper considers a method of synthesis fullerenes and carbon nanotubes at atmospheric pressure. Carbon evaporates into the plasma arc. The paper discusses the method of synthesis of helium at a pressure of 105 Pa. We show the dependence yield of fullerenes and carbon nanotubes from the buffer gas pressure. It has been found that the fullerene yield increased with increasing pressure. The obtained fullerenes and nanotubes find their application in the modification of construction materials. The use of carbon nanomodifiers in the modification of the construction is promising since their introduction significantly improves the physico-mechanical properties using a small quantity of additives. With the introduction of the carbon nanomodifier decrease the porosity of cement stone, which leads to high strength and frost-resistant indicators of the modified cement.

  3. Highly doped InP as a low loss plasmonic material for mid-IR region

    DEFF Research Database (Denmark)

    Panah, Mohammad Esmail Aryaee; Takayama, Osamu; Morozov, S. V.


    We study plasmonic properties of highly doped InP in the mid-infrared (IR) range. InP was grown by metal-organic vapor phase epitaxy (MOVPE) with the growth conditions optimized to achieve high free electron concentrations by doping with silicon. The permittivity of the grown material was found b...

  4. Ultrasonic assisted synthesis of Bikitaite zeolite: A potential material for hydrogen storage application. (United States)

    Roy, Priyanka; Das, Nandini


    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 N2 adsorption-desorption measurements was found to be 209m2/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

  5. Synthesis and characterization of zeolite material from coal ashes modified by surfactant; Sintese e caracterizacao de material zeolitico de cinzas de carvao modificado por surfactante

    Energy Technology Data Exchange (ETDEWEB)

    Fungaro, D.A., E-mail: dfungaro@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (CQMA/IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Quimica e Meio Ambiente; Borrely, S.I. [Instituto de Pesquisas Energeticas e Nucleares (CTR/IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Tecnologia das Radiacoes


    Coal ash was used as starting material for zeolite synthesis by means of hydrothermal treatment. The surfactant-modified zeolite (SMZ) was prepared by adsorbing the cationic surfactant hexadecyltrimethylammonium bromide (HDTMA-Br) on the external surface of the zeolite from coal ash. The zeolite structure stability was monitored during the characterization of the materials by FTIR, XDR and SEM. The structural parameters of surfactant-modified zeolite are very close to that of corresponding non-modified zeolite which indicates that the crystalline nature of the zeolite remained intact after required chemical treatment with HDTMA-Br molecules and heating treatment for drying. The most intense peaks in the FTIR spectrum of HDTMA-Br were observed in SMZ spectrum confirming adsorption of surfactant on zeolites. (author)

  6. Research Progress on 3D Printed Graphene Materials Synthesis Technology and Its Application in Energy Storage Field

    Directory of Open Access Journals (Sweden)

    WANG Nan


    Full Text Available Graphene is an ideal material for energy storage application as its excellent mechanical and physical properties. 3D printed graphene materials will be widely applied in energy storage field for its precisely controllable structure and it is easy to realize large-scale preparation. In this paper, the progress of 3D printed graphene materials synthesis technology and its application in energy storage field were reviewed. The viscosity and printability of graphene ink are key factors for realizing graphene 3D printing. Scalable preparation of graphene ink with facile process, controllable concentration and additive free will be the research focus of graphene 3D printing technologies in the future. The integrated printing of graphene energy storage devices such as graphene supercapacitor, lithium-sulfur battery and lithium ion battery is the development direction in this area.

  7. Synthesis of a new fluorescent materials: partially modified PVAC containing a derivative of 2-(hydroxyphenyl)benzoxazole

    Energy Technology Data Exchange (ETDEWEB)

    Maraboli, Beltran; Soto, Juan Pablo; Aristizabal, Juliet Andrea; Escalona, Cindy Luisa; Gallardo, Felipe Luis; Ahumada, Juan Carlos, E-mail: [Pontificia Universidad Catolica de Valparaiso, Campus Curauma, Valparaiso (Chile)


    A new fluorescent material is obtained from partially hydrolized polyvinyl acetate and 2- hydroxyfenilbenzoxazol derivate. The synthetic route starts by obtaining 2- (5-bromo-2-hydroxifenilbenzoxazol) -6- carboxylic acid, then the partial hydrolysis was carried out in alkaline medium using 3:1 acetone/water as solvent medium. Finally, coupling was obtained by the attachment through Steglich esterification at room temperature in dry dioxane medium. The optical properties of the combined material were examined by UV-Vis and molecular fluorescence. Benzoxazoles synthesis of derivatives used is characterized by FT-IR, {sup 1}H-NMR and {sup 13}C-NMR, for the modified PVAc polymer matrix was characterized using FT-IR, DSC and TGA, applying the same analysis for the material. (author)

  8. FY 1990 Report on the results of the research and development project for the industrial base technologies of the next generation. Research and development of nonlinear optoelectronic materials; 1990 nendo hisenkei hikari denshi zairyo no kenkyu kaihatsu seika hokokusho

    Energy Technology Data Exchange (ETDEWEB)



    Described herein are the FY 1990 results of the research and development project for the optoelectronic materials, implemented to cope with the highly information-oriented societies. The FY 1990 is the second year for the phase-I project of the basic plan, and the R and D efforts are directed to elucidation of the mechanisms involved in the nonlinear phenomena, exploration and designs of various materials, and investigations of the technologies for, e.g., the material synthesis and evaluation. The themes to be investigated by the long-term project include exploration and preparation of the superfine particles and base materials for the organic materials; and crystal growth, dispersion of the fine particles and development of the superlattices for development of the materials. The comprehensive investigation and research program investigates the trends of the related technologies, both domestic and foreign. A total of 9 research themes are recommissioned to 9 enterprises. They include organic, low-molecular-weight materials, growth of orientation-controlled crystals, films of high-molecular-weight organic conjugated compounds, glass-dispersed materials (prepared by the vapor-phase, impregnation of porous glass, sol-gel, superlow-melting glass and super-cooling methods), organic dispersed materials, development of the organic superlattices, and development of the three-dimensional superstructures. (NEDO)

  9. Microwave-assisted Synthesis and Biomedical Applications of Inorganic Nanostructured Materials (United States)

    Jia, Juncai

    Inorganic nanostrucured materials have attracted much attention owing to their unique features and important applications in biomedicine. This thesis describes the development of rapid and efficient approaches to synthesize inorganic nanostructures, and introduces some potential applications. Magnetic nanostructures, such as necklace-like FeNi3 magnetic nanochains and magnetite nanoclusters, were synthesized by an efficient microwave-hydrothermal process. They were used as magnetic resonance imaging (MRI) contrast agents. Magnetic FeNi3 nanochains were synthesized by reducing iron(III) acetylacetonate and nickel(II) acetylacetonate with hydrazine in ethylene glycol solution without any template under microwave irradiation. This was a rapid and economical route based on an efficient microwave-hydrothermal process which significantly shortened the synthesis time to mins. The morphologies and size of the materials could be effectively controlled by adjusting the reaction conditions, such as, the reaction time, temperature and concentrations of reactants. The morphology and composition of the as-prepared products were characterized by field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The size of the aligned nanospheres in the magnetic FeNi 3 chains could be adjusted from 150nm to 550nm by increasing the amounts of the precursors. Magnetic measurements revealed that the FeNi3 nanochains showed enhanced coercivity and saturation magnetization. Toxicity tests by exposure of FeNi3 nanochains to the zebrafish larvae showed that the as-prepared nanochains were biocompatible. In vitro magnetic resonance imaging (MRI) confirms the effectiveness of the FeNi 3 nanochains as sensitive MRI probes. Magnetite nanoclusters were synthesized by reducing iron(III) acetylacetonate with hydrazine in ethylene glycol under microwave irradiation. The nanoclusters showed enhanced T2

  10. Mechanistic Studies Of Combustion And Structure Formation During Combustion Synthesis Of Advanced Materials: Phase Separation Mechanism For Bio-Alloys (United States)

    Varma, A.; Lau, C.; Mukasyan, A.


    Among all implant materials, Co-Cr-Mo alloys demonstrate perhaps the most useful balance of resistance to corrosion, fatigue and wear, along with strength and biocompatibility [1]. Currently, these widely used alloys are produced by conventional furnace technology. Owing to high melting points of the main alloy elements (e.g. Tm.p.(Co) 1768 K), high-temperature furnaces and long process times (several hours) are required. Therefore, attempts to develop more efficient and flexible methods for production of such alloys with superior properties are of great interest. The synthesis of materials using combustion phenomena is an advanced approach in powder metallurgy [2]. The process is characterized by unique conditions involving extremely fast heating rates (up to 10(exp 6 K/s), high temperatures (up to 3500 K), and short reaction times (on the order of seconds). As a result, combustion synthesis (CS) offers several attractive advantages over conventional metallurgical processing and alloy development technologies. The foremost is that solely the heat of chemical reaction (instead of an external source) supplies the energy for the synthesis. Also, simple equipment, rather than energy-intensive high-temperature furnaces, is sufficient. This work was devoted to experiments on CS of Co-based alloys by utilizing thermite (metal oxide-reducing metal) reactions, where phase separation subsequently produces materials with tailored compositions and properties. Owing to high reaction exothermicity, the CS process results in a significant increase of temperature (up to 3000 C), which is higher than melting points of all products. Since the products differ in density, phase separation may be a gravitydriven process: the heavy (metallic phase) settles while the light (slag) phase floats. The goal was to determine if buoyancy is indeed the major mechanism that controls phase segregation.

  11. Compact Layers of Hybrid Halide Perovskites Fabricated via the Aerosol Deposition Process—Uncoupling Material Synthesis and Layer Formation

    Directory of Open Access Journals (Sweden)

    Fabian Panzer


    Full Text Available We present the successful fabrication of CH3NH3PbI3 perovskite layers by the aerosol deposition method (ADM. The layers show high structural purity and compactness, thus making them suitable for application in perovskite-based optoelectronic devices. By using the aerosol deposition method we are able to decouple material synthesis from layer processing. Our results therefore allow for enhanced and easy control over the fabrication of perovskite-based devices, further paving the way for their commercialization.

  12. Early-Transition-Metal Silicon Compounds and Their Roles in the Synthesis of New Polymeric and Ceramic Materials (United States)


    trimethylsilyl)silyl Derivatives of Tri (tert- b Utoxy) zircon ium and - Hafnium . X-ray Crystal Structure Of (Me 3 CO)3ZrSi(SiMe 3 )3 ." R. 1-1. H-eyn and T. D...Rules in the Synthesis of New Polymeric and Ceramic Materials 12. PERSONAL AUTHOR(S) T. Don Tilley 13a. TYPE OF REPORT 13b. TIME COVERED 14. DATE OF...California, San Diego, 9500 Gilman Drive, La Jolla, CA 92093-0506 ____ Acc’-ion For - INCLUSIVE DATES : 01 June1 1988 -31 May 1991NTSC& GRANT NUMBER: Al-OSIR-88

  13. Facile synthesis of benzoindoles and naphthofurans through carbonaceous material-catalyzed cyclization of naphthylamines/naphthols with nitroolefins in water. (United States)

    Zhang, Furen; Li, Chunmei; Wang, Chen; Qi, Chenze


    A facile and efficient approach has been established for the synthesis of benzoindole and naphthofuran derivatives via the metal-free cyclization reaction of nitroolefins with naphthylamines/naphthols. Various substituted benzoindoles and naphthofurans are obtained in good to excellent yields. Moreover, the ability to recycle the carbonaceous material makes this method quite cost-effective and environmentally benign compared to traditional acid-catalyzed methods. Theoretical studies indicated that the reaction between naphthylamine and nitroolefin catalyzed by this solid acid was thermodynamically controlled at 60 °C, resulting in the formation of the benzoindoles.

  14. Synthesis of Large-Area 2D Layered Materials and Their Heterostacking Structures (United States)


    by the location and shape of the seeds and the 2nd 2DL materials follows the morphology of the 1st 2DL materials. (2) Study the epitaxial...processes and explore methods to implant seeds at selected areas for subsequent 2DL material growth. Ideally, the growth of 1st 2DL materials can be guided...edge depending on the lattice, edge morphology of the 2DL materials and the growth regime (thermodynamically or kinetically controlled). Efforts

  15. Synthesis, toxicity, biocompatibility, and biomedical applications of graphene and graphene-related materials. (United States)

    Gurunathan, Sangiliyandi; Kim, Jin-Hoi


    Graphene is a two-dimensional atomic crystal, and since its development it has been applied in many novel ways in both research and industry. Graphene possesses unique properties, and it has been used in many applications including sensors, batteries, fuel cells, supercapacitors, transistors, components of high-strength machinery, and display screens in mobile devices. In the past decade, the biomedical applications of graphene have attracted much interest. Graphene has been reported to have antibacterial, antiplatelet, and anticancer activities. Several salient features of graphene make it a potential candidate for biological and biomedical applications. The synthesis, toxicity, biocompatibility, and biomedical applications of graphene are fundamental issues that require thorough investigation in any kind of applications related to human welfare. Therefore, this review addresses the various methods available for the synthesis of graphene, with special reference to biological synthesis, and highlights the biological applications of graphene with a focus on cancer therapy, drug delivery, bio-imaging, and tissue engineering, together with a brief discussion of the challenges and future perspectives of graphene. We hope to provide a comprehensive review of the latest progress in research on graphene, from synthesis to applications.

  16. The vapor-phase multi-stage CMD test for characterizing contaminant mass discharge associated with VOC sources in the vadose zone: Application to three sites in different lifecycle stages of SVE operations. (United States)

    Brusseau, M L; Mainhagu, J; Morrison, C; Carroll, K C


    Vapor-phase multi-stage contaminant mass discharge (CMD) tests were conducted at three field sites to measure mass discharge associated with contaminant sources located in the vadose zone. The three sites represent the three primary stages of the soil vapor extraction (SVE) operations lifecycle-pre/initial-SVE, mid-lifecycle, and near-closure. A CMD of 32g/d was obtained for a site at which soil vapor SVE has been in operation for approximately 6years, and for which mass removal is currently in the asymptotic stage. The contaminant removal behavior exhibited for the vapor extractions conducted at this site suggests that there is unlikely to be a significant mass of non-vapor-phase contaminant (e.g., DNAPL, sorbed phase) remaining in the advective domains, and that most remaining mass is likely located in poorly accessible domains. Given the conditions for this site, this remaining mass is hypothesized to be associated with the low-permeability (and higher water saturation) region in the vicinity of the saturated zone and capillary fringe. A CMD of 25g/d was obtained for a site wherein SVE has been in operation for several years but concentrations and mass-removal rates are still relatively high. A CMD of 270g/d was obtained for a site for which there were no prior SVE operations. The behavior exhibited for the vapor extractions conducted at this site suggest that non-vapor-phase contaminant mass (e.g., DNAPL) may be present in the advective domains. Hence, the asymptotic conditions observed for this site most likely derive from a combination of rate-limited mass transfer from DNAPL (and sorbed) phases present in the advective domain as well as mass residing in lower-permeability ("non-advective") regions. The CMD values obtained from the tests were used in conjunction with a recently developed vapor-discharge tool to evaluate the impact of the measured CMDs on groundwater quality. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. Evaluation of Co-precipitation Processes for the Synthesis of Mixed-Oxide Fuel Feedstock Materials

    Energy Technology Data Exchange (ETDEWEB)

    Collins, Emory D [ORNL; Voit, Stewart L [ORNL; Vedder, Raymond James [ORNL


    The focus of this report is the evaluation of various co-precipitation processes for use in the synthesis of mixed oxide feedstock powders for the Ceramic Fuels Technology Area within the Fuels Cycle R&D (FCR&D) Program's Advanced Fuels Campaign. The evaluation will include a comparison with standard mechanical mixing of dry powders and as well as other co-conversion methods. The end result will be the down selection of a preferred sequence of co-precipitation process for the preparation of nuclear fuel feedstock materials to be used for comparison with other feedstock preparation methods. A review of the literature was done to identify potential nitrate-to-oxide co-conversion processes which have been applied to mixtures of uranium and plutonium to achieve recycle fuel homogeneity. Recent studies have begun to study the options for co-converting all of the plutonium and neptunium recovered from used nuclear fuels, together with appropriate portions of recovered uranium to produce the desired mixed oxide recycle fuel. The addition of recycled uranium will help reduce the safeguard attractiveness level and improve proliferation resistance of the recycled fuel. The inclusion of neptunium is primarily driven by its chemical similarity to plutonium, thus enabling a simple quick path to recycle. For recycle fuel to thermal-spectrum light water reactors (LWRs), the uranium concentration can be {approx}90% (wt.), and for fast spectrum reactors, the uranium concentration can typically exceed 70% (wt.). However, some of the co-conversion/recycle fuel fabrication processes being developed utilize a two-step process to reach the desired uranium concentration. In these processes, a 50-50 'master-mix' MOX powder is produced by the co-conversion process, and the uranium concentration is adjusted to the desired level for MOX fuel recycle by powder blending (milling) the 'master-mix' with depleted uranium oxide. In general, parameters that must be

  18. Metal organic vapor phase epitaxy growth of (Al)GaN heterostructures on SiC/Si(111) templates synthesized by topochemical method of atoms substitution

    DEFF Research Database (Denmark)

    Rozhavskaya, Mariia M.; Kukushkin, Sergey A.; Osipov, Andrey V.


    crystalline interfaces with epitaxial relationship between SiC/Si and AlN/SiC layers. Optimization of SiC morphology and AlN seed layer thickness facilitates the growth of GaN layers free of pits (v-defects). It is also found that Si doping eliminates these defects in the case of growth on SiC templates...... with non-optimized surface morphology. Thus, synthesis of thin SiC buffer layer is suggested as a solution for the interface problems at the initial stage of III-N on Si epitaxy....

  19. The synthesis of Fe-Cu-Si oxide as a potential catalyst material for Fischer Tropsch reaction (United States)

    Tjahjanto, Rachmat Triandi; Mustaqimah, Aili Millatul; Ayun, Qurratu


    Variations of iron(III) concentration were made during the synthesis of iron-copper-silicon oxide with sol-gel technique. The material was synthesized as a potential catalyst material for Fischer Tropsch reaction. A solution of sodium metasilicate was added dropwise onto solutions of iron(III) and copper(II) nitrate in diluted nitric acid. At pH 5 gels were obtained, followed with drying, calcination, and grinding to obtain fine powders. At concentration of iron(III) nitrate of 22.99% and 23.81% the process provided pale yellow colored powders, while those with 24.20%, 26.93%, and 27.58% of iron(III) nitrates gave brown powders. One of the brown powders showed crystalline phase in its diffractograms, while the yellow one was completely amorphous.

  20. Graphene-Oxide-Assisted Synthesis of GaN Nanosheets as a New Anode Material for Lithium-Ion Battery. (United States)

    Sun, Changlong; Yang, Mingzhi; Wang, Tailin; Shao, Yongliang; Wu, Yongzhong; Hao, Xiaopeng


    As the most-studied III-nitride, theoretical researches have predicted the presence of gallium nitride (GaN) nanosheets (NSs). Herein, a facile synthesis approach is reported to prepare GaN NSs using graphene oxide (GO) as sacrificial template. As a new anode material of Li-ion battery (LIBs), GaN NSs anodes deliver the reversible discharge capacity above 600 mA h g-1 at 1.0 A g-1 after 1000 cycles, and excellent rate performance at current rates from 0.1 to 10 A g-1. These results not only extend the family of 2D materials but also facilitate their use in energy storage and other applications.

  1. Low-resistivity m-plane freestanding GaN substrate with very low point-defect concentrations grown by hydride vapor phase epitaxy on a GaN seed crystal synthesized by the ammonothermal method (United States)

    Kojima, Kazunobu; Tsukada, Yusuke; Furukawa, Erika; Saito, Makoto; Mikawa, Yutaka; Kubo, Shuichi; Ikeda, Hirotaka; Fujito, Kenji; Uedono, Akira; Chichibu, Shigefusa F.


    An m-plane freestanding GaN substrate satisfying both low resistivity (ρ = 8.5 × 10-3 Ω·cm) and a low point-defect concentration, being applicable to vertically conducting power-switching devices, was grown by hydride vapor phase epitaxy on a nearly bowing-free bulk GaN seed wafer synthesized by the ammonothermal method in supercritical ammonia using an acidic mineralizer. Its threading dislocation and basal-plane staking-fault densities were approximately 104 cm-2 and lower than 100 cm-1, respectively. A record-long fast-component photoluminescence lifetime of 2.07 ns at room temperature was obtained for the near-band-edge emission, reflecting a significantly low concentration of nonradiative recombination centers composed of Ga vacancies.

  2. Synthesis of Foam-Shaped Nanoporous Zeolite Material: A Simple Template-Based Method (United States)

    Saini, Vipin K.; Pires, Joao


    Nanoporous zeolite foam is an interesting crystalline material with an open-cell microcellular structure, similar to polyurethane foam (PUF). The aluminosilicate structure of this material has a large surface area, extended porosity, and mechanical strength. Owing to these properties, this material is suitable for industrial applications such as…

  3. Plasma techniques for nanostructured carbon materials synthesis. A case study: carbon nanowall growth by low pressure expanding RF plasma (United States)

    Vizireanu, S.; Stoica, S. D.; Luculescu, C.; Nistor, L. C.; Mitu, B.; Dinescu, G.


    A short description of approaches for carbon nanostructures synthesis is made and the advantages of using plasma during the growth are presented. As a particular example of a plasma based technique we detail the process of downstream carbon nanowall (CNW) synthesis by a radiofrequency expanding plasma beam. The technique combines magnetron sputtering for catalyst deposition and plasma enhanced chemical vapor deposition (main gas: argon, active gas: hydrogen, precursor gas: acetylene) for carbon growth in a single reactor. The analysis focuses on the correlation between the material properties and the plasma characteristics measured at different points along the flow axis, aiming to reveal the importance of plasma species in the growth process. The material properties were investigated by scanning and transmission electron microscopy, whereas the plasma data were obtained by optical emission spectroscopy, Langmuir probes and mass spectrometry. CNWs with a large area and well isolated from each other are obtained at an optimum distance from the precursor injection point where the plasma presents an enhanced content of carbon nanoclusters. The possible processes responsible for the growth are discussed.

  4. Plasma techniques for nanostructured carbon materials synthesis. A case study: carbon nanowall growth by low pressure expanding RF plasma

    Energy Technology Data Exchange (ETDEWEB)

    Vizireanu, S; Stoica, S D; Luculescu, C; Mitu, B; Dinescu, G [National Institute for Laser, Plasma and Radiation Physics Magurele-Bucharest, PO Box MG-16, 077125 (Romania); Nistor, L C, E-mail: dinescug@infim.r [National Institute for Materials Physics Magurele-Bucharest, 077125 (Romania)


    A short description of approaches for carbon nanostructures synthesis is made and the advantages of using plasma during the growth are presented. As a particular example of a plasma based technique we detail the process of downstream carbon nanowall (CNW) synthesis by a radiofrequency expanding plasma beam. The technique combines magnetron sputtering for catalyst deposition and plasma enhanced chemical vapor deposition (main gas: argon, active gas: hydrogen, precursor gas: acetylene) for carbon growth in a single reactor. The analysis focuses on the correlation between the material properties and the plasma characteristics measured at different points along the flow axis, aiming to reveal the importance of plasma species in the growth process. The material properties were investigated by scanning and transmission electron microscopy, whereas the plasma data were obtained by optical emission spectroscopy, Langmuir probes and mass spectrometry. CNWs with a large area and well isolated from each other are obtained at an optimum distance from the precursor injection point where the plasma presents an enhanced content of carbon nanoclusters. The possible processes responsible for the growth are discussed.

  5. Facile Synthesis and High performance of a New Carbazole-Based Hole Transporting Material for Hybrid Perovskite Solar Cells

    KAUST Repository

    Wang, Hong


    Perovskite solar cells are very promising for practical applications owing to their rapidly rising power conversion efficiency and low cost of solution-based processing. 2,2’,7,7’-tetrakis-(N,N-di-p-methoxyphenylamine) 9,9’-spirobifluorene (Spiro-OMeTAD) is most widely used as hole transporting material (HTM) in perovskite solar cells. However, the tedious synthesis and high cost of Spiro-OMeTAD inhibit its commercial-scale application in the photovoltaic industry. In this article, we report a carbazole-based compound (R01) as a new HTM in efficient perovskite solar cells. R01 is synthesized via a facile route consisting of only two steps from inexpensive commercially available materials. Furthermore, R01 exhibits higher hole mobility and conductivity than the state-of-the-art Spiro-OMeTAD. Perovskite solar cells fabricated with R01 produce a power conversion efficiency of 12.03%, comparable to that obtained in devices using Spiro-OMeTAD in this study. Our findings underscore R01 as a highly promising HTM with high performance, and its facile synthesis and low cost may facilitate the large-scale applications of perovskite solar cells.

  6. Sol-gel synthesis of carbon based materials reinforced ultra high temperature ceramic composites


    Wang, Xiaojing


    This Ph.D. research is based on the development of novel sol-gel techniques for synthesis of nanostructured ultra high temperature ceramics (UHTCs) and subsequent spark plasma sintering (SPS) for densifying the UHTC composites. The liquid nature of the sol-gel process offers advantages such as high purity and ability for mixing and infiltration, and thus it can overcome some shortcomings of the conventional power processing of ceramics. SPS delivers microstructures with good density and fine ...

  7. Influence of the V/III ratio in the gas phase on thin epitaxial AlN layers grown on (0001) sapphire by high temperature hydride vapor phase epitaxy

    Energy Technology Data Exchange (ETDEWEB)

    Claudel, A., E-mail: [ACERDE, 354 Voie Magellan — Alpespace, 73800 Ste Hélène du Lac (France); Fellmann, V. [ACERDE, 354 Voie Magellan — Alpespace, 73800 Ste Hélène du Lac (France); Science et Ingénierie des Matériaux et des Procédés, Grenoble INP-CNRS-UJF, BP 75, 38402 Saint Martin d' Hères (France); Gélard, I. [ACERDE, 354 Voie Magellan — Alpespace, 73800 Ste Hélène du Lac (France); Coudurier, N. [ACERDE, 354 Voie Magellan — Alpespace, 73800 Ste Hélène du Lac (France); Science et Ingénierie des Matériaux et des Procédés, Grenoble INP-CNRS-UJF, BP 75, 38402 Saint Martin d' Hères (France); Sauvage, D. [ACERDE, 354 Voie Magellan — Alpespace, 73800 Ste Hélène du Lac (France); Balaji, M. [ACERDE, 354 Voie Magellan — Alpespace, 73800 Ste Hélène du Lac (France); Science et Ingénierie des Matériaux et des Procédés, Grenoble INP-CNRS-UJF, BP 75, 38402 Saint Martin d' Hères (France); Crystal Growth Center, Anna University, Chennai 600025 (India); and others


    Thin (0001) epitaxial aluminum nitride (AlN) layers were grown on c-plane sapphire using high temperature hydride vapor phase epitaxy. The experimental set-up consists of a vertical cold-wall quartz reactor working at low pressure in which the reactions take place on a susceptor heated by induction. The reactants used are ammonia and aluminum chlorides in situ formed via hydrogen chloride reaction with high purity aluminum pellets. As-grown AlN layers have been characterized by scanning electron microscopy, atomic force microscopy, X-ray diffraction, transmission electron microscopy, photoluminescence and Raman spectroscopies. The influence of the V/III ratio in the gas phase, from 1.5 to 15, on growth rate, surface morphology, roughness and crystalline quality is investigated in order to increase the quality of thin epitaxial AlN layers grown at high temperature. Typical growth rates of around 0.45 μm/h were obtained for such thin epitaxial AlN layers. The growth rate was unaffected by the V/III ratio. An optimum for roughness, crystalline quality and optical properties seems to exist at V/III = 7.5. As a matter of fact, for a V/III ratio of 7.5, best root mean square roughness and crystalline quality — measured on 0002 symmetric reflection — as low as 6.9 nm and 898 arcsec were obtained, respectively. - Highlights: • Growth of thin epitaxial AlN layers by high temperature hydride vapor phase epitaxy • Influence of V/III ratio on growth rate, morphology and crystalline quality • The effect of surface morphology on strain state and crystal quality is established.

  8. A Survey on Synthesis Processes of Structured Materials for Biomedical Applications: Iron-based Magnetic Nanoparticles, Polymeric Materials and Polymerization Processes. (United States)

    Neto, Weslany Silvério; Jensen, Alan Thyago; Ferreira, Gabriella Ribeiro; Valadares, Leonardo Fonseca; Gambetta, Rossano; Gonçalves, Sílvia Belém; Machado, Fabricio


    Magnetic materials based on iron oxides are extensively designed for several biomedical applications. Heterogeneous polymerization processes are powerful tools for the production of tailored micro-sized and nanosized magneto-polymeric particles. Although several polymerization processes have been adopted along the years, suspension, emulsion and miniemulsion systems deserve special attention due to its ability to produce spherical polymer particles containing magnetic nanoparticles homogeneously dispersed into the polymer thermoplastic matrices. The main objective of this paper is to review the main methods of synthesis of iron-based magnetic nanoparticles and to illustrate how typical polymerization processes in different dispersion medium can be successfully used to produce engineered magnetic core-shell structures. It is exemplified the use of suspension, emulsion and miniemulsion polymerization processes in order to support experimental methodologies required for the production of magnetic polymer particles intended for biomedical applications such as intravascular embolization treatments, drug delivery systems and hyperthermia treatment.

  9. Synthesis and characterization of inorganic materials precipitated into polymeric and novel liquid crystalline systems (United States)

    Lubeck, Christopher Ryan

    The use of nanostructured, hybrid materials possesses great future potential. Many examples of nanostructured materials exist within nature, such as animal bone, animal teeth, and seashells. This research, inspired by nature, strove to mimic salient properties of natural materials, utilizing methods observed within nature to produce materials. Further, this research increased the functionality of the templates from "mere" template to functional participant. Different chemical methods to produce hybrid materials were employed within this research to achieve these goals. First, electro-osmosis was utilized to drive ions into a polymeric matrix to form hybrid inorganic polymer material, creating a material inspired by naturally occurring bone or seashell in which the inorganic component provides strength and the polymeric material decreases the brittleness of the combined hybrid material. Second, self-assembled amphiphiles, forming higher ordered structures, acted as a template for inorganic cadmium sulfide. Electronically active molecules based on ethylene oxide and aniline segments were synthesized to create interaction between the templating material and the resulting inorganic cadmium sulfide. The templating process utilized self-assembly to create the inorganic structure through the interaction of the amphiphiles with water. The use of self-assembly is itself inspired by nature. Self-assembled structures are observed within living cells as cell walls and cell membranes are created through hydrophilic and hydrophobic interactions. Finally, the mesostructured inorganic cadmium sulfide was itself utilized as a template to form mesostructured copper sulfide.

  10. Synthesis of novel inorganic-organic hybrid materials for simultaneous adsorption of metal ions and organic molecules in aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Jin, Xinliang [State Key Laboratory of Applied Organic Chemistry, College of Chemistry and Chemical Engineering, Institute of Biochemical Engineering and Environmental Technology, Lanzhou University, Lanzhou 730000 (China); Li, Yanfeng, E-mail: [State Key Laboratory of Applied Organic Chemistry, College of Chemistry and Chemical Engineering, Institute of Biochemical Engineering and Environmental Technology, Lanzhou University, Lanzhou 730000 (China); Yu, Cui; Ma, Yingxia; Yang, Liuqing; Hu, Huaiyuan [State Key Laboratory of Applied Organic Chemistry, College of Chemistry and Chemical Engineering, Institute of Biochemical Engineering and Environmental Technology, Lanzhou University, Lanzhou 730000 (China)


    Highlights: Black-Right-Pointing-Pointer Novel hybrid materials were synthesized and employed in the absorption of heavy metal and organic pollutants. Black-Right-Pointing-Pointer A novel method for amphiphilic adsorbent material synthesis was first reported in this paper. Black-Right-Pointing-Pointer The adsorbent material showed excellent adsorption capacity to Pb(II) and phenol. - Abstract: In this paper, atom transfer radical polymerization (ATRP) and radical grafting polymerization were combined to synthesize a novel amphiphilic hybrid material, meanwhile, the amphiphilic hybrid material was employed in the absorption of heavy metal and organic pollutants. After the formation of attapulgite (ATP) ATRP initiator, ATRP block copolymers of styrene (St) and divinylbenzene (DVB) were grafted from it as ATP-P(S-b-DVB). Then radical polymerization of acrylonitrile (AN) was carried out with pendent double bonds in the DVD units successfully, finally we got the inorganic-organic hybrid materials ATP-P(S-b-DVB-g-AN). A novel amphiphilic hybrid material ATP-P(S-b-DVB-g-AO) (ASDO) was obtained after transforming acrylonitrile (AN) units into acrylamide oxime (AO) as hydrophilic segment. The adsorption capacity of ASDO for Pb(II) could achieve 131.6 mg/g, and the maximum removal capacity of ASDO towards phenol was found to be 18.18 mg/g in the case of monolayer adsorption at 30 Degree-Sign C. The optimum pH was 5 for both lead and phenol adsorption. The adsorption kinetic suited pseudo-second-order equation and the equilibrium fitted the Freundlich model very well under optimal conditions. At the same time FT-IR, TEM and TGA were also used to study its structure and property.

  11. Synthesis, Fabrication, and Characterization of Multidimensional Nanoparticle Based Thermoelectric Materials Composed of Bismuth, Antimony, and Tellurium


    Mott, Derrick; Mai, Nguyen T.; Thuy, Nguyen T. B.; Sakata, Teruyoshi; Koyano, Mikio; Maenosono, Shinya


    With the event of nanotechnology, the field of thermoelectric (TE) materials has been re-invigorated with many recent advances towards materials with high thermoelectric efficiency (dimensionless figure of merit, ZT). The realization of such materials opens up new avenues to the creation of devices that can be used in freon-less refrigeration, micro-electronic cooling, or for harnessing lost heat energy from sources such as car engines. In our own research work, we have successfully devised a...

  12. Synthesis of TiO2 Materials Using Ionic Liquids and Its Applications for Sustainable Energy and Environment. (United States)

    Yoo, Kye Sang


    Titanium dioxide (TiO2) has received significant attention because of the global climate change and the consumption of fossil fuel resources. Specifically, using TiO2 in photocatalytic applications, such as the removal of organic pollutants and a hydrogen production has become an important issue. Thus, many researchers have attempted to prepare highly active TiO2 materials using various synthetic approaches. Modifications of the conventional sol-gel method, such as the addition of surfactants, have been employed in synthetic procedures. Moreover, hydrothermal, solvothermal, sonochemical and microwave methods have also been used as alternative approaches. Recently, the use of ionic liquids represents a burgeoning direction in inorganic material synthesis. Ionic liquids are exceptional solvents consisting of ions possessing low vapor pressure and tunable solvent properties. This article reviews the preparation of TiO2 materials using ionic liquids with various synthetic approaches. Also, sustainable energy and environmental cleanup applications of TiO2 materials, including the treatment of hazardous organic substances and hydrogen energy derived from electrochemical methods, are discussed.

  13. Green synthesis of boron doped graphene and its application as high performance anode material in Li ion battery

    Energy Technology Data Exchange (ETDEWEB)

    Sahoo, Madhumita; Sreena, K.P.; Vinayan, B.P.; Ramaprabhu, S., E-mail:


    Graphical abstract: Boron doped graphene (B-G), synthesized by simple hydrogen induced reduction technique using boric acid as boron precursor, have more uneven surface as a result of smaller bonding distance of boron compared to carbon, showed high capacity and high rate capability compared to pristine graphene as an anode material for Li ion battery application. - Abstract: The present work demonstrates a facile route for the large-scale, catalyst free, and green synthesis approach of boron doped graphene (B-G) and its use as high performance anode material for Li ion battery (LIB) application. Boron atoms were doped into graphene framework with an atomic percentage of 5.93% via hydrogen induced thermal reduction technique using graphite oxide and boric acid as precursors. Various characterization techniques were used to confirm the boron doping in graphene sheets. B-G as anode material shows a discharge capacity of 548 mAh g{sup −1} at 100 mA g{sup −1} after 30th cycles. At high current density value of 1 A g{sup −1}, B-G as anode material enhances the specific capacity by about 1.7 times compared to pristine graphene. The present study shows a simplistic way of boron doping in graphene leading to an enhanced Li ion adsorption due to the change in electronic states.

  14. One-pot synthesis of magnetic hybrid materials based on ovoid-like carboxymethyl-cellulose/cetyltrimethylammonium-bromide templates

    Energy Technology Data Exchange (ETDEWEB)

    Torres-Martínez, Nubia E. [Universidad Autónoma de Nuevo León, Facultad de Ingeniería Mecánica y Eléctrica, San Nicolás de los Garza, 66450 Nuevo León (Mexico); Garza-Navarro, M.A., E-mail: [Universidad Autónoma de Nuevo León, Facultad de Ingeniería Mecánica y Eléctrica, San Nicolás de los Garza, 66450 Nuevo León (Mexico); Universidad Autónoma de Nuevo León, Centro de Innovación, Investigación y Desarrollo en Ingeniería y Tecnología, Apodaca, 66600 Nuevo León (Mexico); Lucio-Porto, Raúl [Université de Nantes, CNRS, Institut des Matériaux Jean Rouxel (IMN), 2 rue de la Houssinière, BP32229, 44322 Nantes Cedex 3 (France); and others


    A novel one-pot synthetic procedure to obtain magnetic hybrid nanostructured materials (HNM), based on magnetic spinel-metal-oxide (SMO) nanoparticles stabilized in ovoid-like carboxymethyl-cellulose (CMC)/cetyltrimethylammonium-bromide (CTAB) templates, is reported. The HNM were synthesized from the controlled hydrolysis of inorganic salts of Fe (II) and Fe (III) into aqueous dissolutions of CMC and CTAB. The synthesized HNM were characterized by transmission electron microscopy, Fourier transform infrared spectroscopy and static magnetic measurements. The experimental evidence suggests that, due to the competition between CTAB molecules and SMO nanoparticles to occupy CMC intermolecular sites nearby to its carboxylate functional groups, the size of both, SMO nanoparticles and ovoid-like CMC/CTAB templates can be tuned, varying the CTAB:SMO weight ratio. Moreover, it was found that the magnetic response of the HNM depends on the confinement degree of the SMO nanoparticles into the CMC/CTAB template. Hence, their magnetic characteristics can be adjusted controlling the size of the template, the quantity and distribution of the SMO nanoparticles within the template and their size. - Graphical abstract: Display Omitted - Highlights: • The synthesis of magnetic hybrid materials is reported. • The hybrid materials were synthesized following a novel one-pot procedure. • The magnetic nanoparticles were stabilized in ovoid-like templates. • The size of the templates was tuned adjusting nanoparticles weight content. • The magnetic properties of hybrid materials depend on the size of the template.

  15. Graphene and Carbon Quantum Dot-Based Materials in Photovoltaic Devices: From Synthesis to Applications

    Directory of Open Access Journals (Sweden)

    Sofia Paulo


    Full Text Available Graphene and carbon quantum dots have extraordinary optical and electrical features because of their quantum confinement properties. This makes them attractive materials for applications in photovoltaic devices (PV. Their versatility has led to their being used as light harvesting materials or selective contacts, either for holes or electrons, in silicon quantum dot, polymer or dye-sensitized solar cells. In this review, we summarize the most common uses of both types of semiconducting materials and highlight the significant advances made in recent years due to the influence that synthetic materials have on final performance.

  16. Graphene and Carbon Quantum Dot-Based Materials in Photovoltaic Devices: From Synthesis to Applications. (United States)

    Paulo, Sofia; Palomares, Emilio; Martinez-Ferrero, Eugenia


    Graphene and carbon quantum dots have extraordinary optical and electrical features because of their quantum confinement properties. This makes them attractive materials for applications in photovoltaic devices (PV). Their versatility has led to their being used as light harvesting materials or selective contacts, either for holes or electrons, in silicon quantum dot, polymer or dye-sensitized solar cells. In this review, we summarize the most common uses of both types of semiconducting materials and highlight the significant advances made in recent years due to the influence that synthetic materials have on final performance.

  17. Graphene and Carbon Quantum Dot-Based Materials in Photovoltaic Devices: From Synthesis to Applications (United States)

    Paulo, Sofia; Palomares, Emilio; Martinez-Ferrero, Eugenia


    Graphene and carbon quantum dots have extraordinary optical and electrical features because of their quantum confinement properties. This makes them attractive materials for applications in photovoltaic devices (PV). Their versatility has led to their being used as light harvesting materials or selective contacts, either for holes or electrons, in silicon quantum dot, polymer or dye-sensitized solar cells. In this review, we summarize the most common uses of both types of semiconducting materials and highlight the significant advances made in recent years due to the influence that synthetic materials have on final performance. PMID:28335285

  18. Metal-organic framework templated synthesis of porous inorganic materials as novel sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Taylor-Pashow, Kathryn M. L.; Lin, Wenbin; Abney, Carter W.


    A novel metal-organic framework (MOF) templated process for the synthesis of highly porous inorganic sorbents for removing radionuclides, actinides, and heavy metals is disclosed. The highly porous nature of the MOFs leads to highly porous inorganic sorbents (such as oxides, phosphates, sulfides, etc) with accessible surface binding sites that are suitable for removing radionuclides from high level nuclear wastes, extracting uranium from acid mine drainage and seawater, and sequestering heavy metals from waste streams. In some cases, MOFs can be directly used for removing these metal ions as MOFs are converted to highly porous inorganic sorbents in situ.


    Directory of Open Access Journals (Sweden)

    S. Kasmi-Mir


    Full Text Available We describe the synthesis of new organic Schiff bases  chromophores 5 containing a  rhodanine-3- acetic as electron accepteur moiety. Imines 3 were obtained by a condensation reaction from a lead molecule, the aminothiazolinethione 1 with versatile commercial aldehydes. The structure of all the compounds obtained was determined by the spectroscopic methods (IR, 1H NMR and 13C NMR. The study of UV-Vis imines 3 and 5 in methanol exhibit the phenomenon of π delocalized electrons responsible for the bathochromic effect

  20. High-throughput development of amphiphile self-assembly materials: fast-tracking synthesis, characterization, formulation, application, and understanding. (United States)

    Mulet, Xavier; Conn, Charlotte E; Fong, Celesta; Kennedy, Danielle F; Moghaddam, Minoo J; Drummond, Calum J


    Amphiphile self-assembly materials, which contain both a hydrophilic and a hydrophobic domain, have great potential in high-throughput and combinatorial approaches to discovery and development. However, the materials chemistry community has not embraced these ideas to anywhere near the extent that the medicinal chemistry community has. While this situation is beginning to change, extracting the full potential of high-throughput approaches in the development of self-assembling materials will require further development in the synthesis, characterization, formulation, and application domains. One of the key factors that make small molecule amphiphiles prospective building blocks for next generation multifunctional materials is their ability to self-assemble into complex nanostructures through low-energy transformations. Scientists can potentially tune, control, and functionalize these structures, but only after establishing their inherent properties. Because both robotic materials handling and customized rapid characterization equipment are increasingly available, high-throughput solutions are now attainable. These address traditional development bottlenecks associated with self-assembling amphiphile materials, such as their structural characterization and the assessment of end-use functional performance. A high-throughput methodology can help streamline materials development workflows, in accord with existing high-throughput discovery pipelines such as those used by the pharmaceutical industry in drug discovery. Chemists have identified several areas that are amenable to a high-throughput approach for amphiphile self-assembly materials development. These allow an exploration of not only a large potential chemical, compositional, and structural space, but also material properties, formulation, and application variables. These areas of development include materials synthesis and preparation, formulation, characterization, and screening performance for the desired end

  1. Synthesis and characterization of a new photoluminescent material, tris-[1-10 phenanthroline] aluminium (United States)

    Kumar, Rahul; Dvivedi, Avanish; Bhargava, Parag


    A new photoluminescent material namely tris-[1-10 Phenanthroline] Aluminium Al(Phen)3 has been synthesized and characterized. This material was characterized by fourier transform infrared spectroscopy (FTIR),nuclear magnetic resonance (NMR),mass spectroscopy, thermal gravimetric analysis (TGA),ultraviolet-visible spectroscopy(UV) and photoluminescence (PL). This material shows thermal stability up to 300°C. This material showed absorption maxima at 352nm which may be attributed to the moderate energy (π-π*) transition. Photoluminescence spectra for this material showed the most intense peak at 423 nm and the time resolved photoluminescence spectra showed two life time components. The decay times of the first and second component were 1.4ns and 4.8 ns respectively.

  2. Synthesis and characterization of a new photoluminescent material, tris-[1-10 phenanthroline] aluminium

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Rahul, E-mail:; Bhargava, Parag [Department of Metallurgical Engineering and Materials Science Indian Institute of Technology-Bombay, Mumbai-400076 (India); Dvivedi, Avanish [Department of Chemistry Indian Institute of Technology-Bombay, Mumbai-400076 (India)


    A new photoluminescent material namely tris-[1-10 Phenanthroline] Aluminium Al(Phen){sub 3} has been synthesized and characterized. This material was characterized by fourier transform infrared spectroscopy (FTIR),nuclear magnetic resonance (NMR),mass spectroscopy, thermal gravimetric analysis (TGA),ultraviolet-visible spectroscopy(UV) and photoluminescence (PL). This material shows thermal stability up to 300°C. This material showed absorption maxima at 352nm which may be attributed to the moderate energy (π–π{sup *}) transition. Photoluminescence spectra for this material showed the most intense peak at 423 nm and the time resolved photoluminescence spectra showed two life time components. The decay times of the first and second component were 1.4ns and 4.8 ns respectively.

  3. Facile synthesis of novel soluble cellulose-grafted hyperbranched polymers as potential natural antimicrobial materials. (United States)

    Demircan, Deniz; Zhang, Baozhong


    A new class of soluble cellulose-grafted hyperbranched polymers has been synthesized by a facile "hypergrafting" reaction using bis(2-chloroethyl)amine and soluble cellulose tosylates. The molecular structures of the obtained new materials were characterized by (13)C NMR, FTIR spectroscopy, and elemental analysis. The degree of substitution of the hyperbranched cellulose derivatives ranges between 0.13-0.53. The new cellulose-based materials were soluble in various polar aprotic organic solvents. The thermal properties of the new cellulose materials were investigated by thermal gravimetric analysis. Antibacterial activity of the new cellulose derivatives was evaluated by diffusion disk tests against various gram negative and positive bacteria. Our results suggested that the obtained natural cellulosic materials can act as effective polymeric biocides, and may have great potential in various antimicrobial materials applications. Copyright © 2016. Published by Elsevier Ltd.

  4. Living Polycondensation: Synthesis of Well-Defined Aromatic Polyamide-Based Polymeric Materials

    KAUST Repository

    Alyami, Mram Z.


    Chain growth condensation polymerization is a powerful tool towards the synthesis of well-defined polyamides. This thesis focuses on one hand, on the synthesis of well-defined aromatic polyamides with different aminoalkyl pendant groups with low polydispersity and controlled molecular weights, and on the other hand, on studying their thermal properties. In the first project, well-defined poly (N-octyl-p-aminobenzoate) and poly (N-butyl-p-aminobenzoate) were synthesized, and for the first time, their thermal properties were studied. In the second project, ethyl4-aminobenzoate, ethyl 4-octyl aminobenzoate and 4-(hydroxymethyl) benzoic acid were used as novel efficient initiators of ε-caprolactone with t-BuP2 as a catalyst. Macroinitiator and Macromonomer of poly (ε-caprolactone) were synthesized with ethyl 4-octyl aminobenzoate and ethyl 4-aminobenzoate as initiators to afford polyamide-block-poly (ε-caprolactone) and polyamide-graft-poly (ε-caprolactone) by chain growth condensation polymerization (CGCP). In the third project, a new study has been done on chain growth condensation polymerization to discover the probability to synthesize new polymers and studied their thermal properties. For this purpose, poly (N-cyclohexyl-p-aminobenzoate) and poly (N-hexyl-p-aminobenzoate) were synthesized with low polydispersity and controlled molecular weights.

  5. Synthesis and studies of polypeptide materials: Enantioselective polymerization of gamma-benzyl glutamate-N-carboxyanhydride and synthesis of optically active poly(beta-peptides) (United States)

    Cheng, Jianjun

    (beta-aspartates) bearing short ethylene glycol side chains were obtained with controlled molecular weights and narrow molecular weight distributions when Sc(N(TMS)2)3 was used as initiator for the beta-lactam polymerizations. Polymer chain lengths could be controlled by both stoichiometry and monomer conversion, characteristic of a living polymerization system. Di- and tri-block copoly(beta-peptides) with desired chain lengths were also synthesized using this method. It was found that these techniques were generally applicable for the synthesis of poly(beta-peptides), bearing other proteinogetic side chains. Synthesis and studies of polypeptide materials were extended to unexplored areas by incorporation of both alpha- and beta-amino acid residues into single polymer chains. Two sequence specific polypeptides bearing alternating beta-alpha, or beta-alpha-alpha amino acid residues were synthesized. Both polymers were found to adopt unprecedented stable conformations in solution.

  6. Chitosan Film Containing an Iron Complex: Synthesis and Prospects for Heterocyclic Aromatic Amines (HAAs) Recognition. (United States)

    da Silva, Maria Aparecida S; Abreu, Dieric S; Costa, Leandro A; Aguiar, Natanna de A; Paulo, Tércio F; Longhinotti, Elisane; Diógenes, Izaura C N


    Hybrid organic-inorganic materials have been seen as a promising approach to produce sensors for the detection and/or recognition of heterocyclic aromatic amines (HAAs). This work shows the synthesis of a hybrid film as a result of the incorporation of [Fe(CN)5(NH3)]3- into chitosan (CS); CS-[(CN)5Fe(NH3)]3-. The sensitivity of CS-[(CN)5Fe(NH3)]3- toward HAA-like species was evaluated by using pyrazine (pz) as probe molecule in vapor phase by means of electrochemistry and spectroscopic techniques. The crystallinity (SEM-EDS and XRD) decrease of CS-[(CN)5Fe(NH3)]3- in comparison to CS was assigned to the disturbance of the hydrogen bond network within the polymer. Such conclusion was reinforced by the water contact angle measurements. The results presented in this work indicate physical and intermolecular interactions, mostly hydrogen bond, between [Fe(CN)5(NH3)]3- and CS, where the complex is likely trapped in the polymer with its sixth coordination site available for substitution reactions.

  7. Synthesis, growth and characterization of organic nonlinear optical material: N-benzyl-2-methyl-4-nitroaniline (BNA) (United States)

    Kalaivanan, R.; Srinivasan, K.


    Synthesis of the organic nonlinear optical compound N-benzyl-2-methyl-4-nitroaniline (BNA) was carried out in a newer chemical environment using the mixture of benzyl chloride and 2-methl-4-nitroaniline by a preferred laboratory synthesis process. The synthesized BNA compound was separated by column chromatography (CC) with low pressure silica gell using petrollium benzine and purity of the separated resultant product was confirmed by thin layer chromatography (TLC). Further, the material was recrystallized atleast four times in methanol and the highly purified BNA was used for the growth of single crystals from solutions with selected solvents by slow evaporation method at room temperature. Single crystals having natural growth morphology were harvested and their different growth faces were identified by optical goniometry. The grown crystals were subjected to different characterization techniques such as powder x-ray diffraction (PXRD), fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC) and UV-vis-Near IR spectroscopy. Further, the second harmonic generation (SHG) efficiency of the grown BNA crystal was studied by Kurtz and Perry powder technique using Nd:YAG laser as fundamental source and found to be twice that of inorganic standard KDP.

  8. Development of Novel Polymeric Materials for Gene Therapy and pH-Sensitive Drug Delivery: Modeling, Synthesis, Characterization, and Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Anderson, Brian Curtis [Iowa State Univ., Ames, IA (United States)


    The underlying theme of this thesis is the use of polymeric materials in bioapplications. Chapters 2-5 either develop a fundamental understanding of current materials used for bioapplications or establish protocols and procedures used in characterizing and synthesizing novel materials. In chapters 6 and 7 these principles and procedures are applied to the development of materials to be used for gene therapy and drug delivery. Chapter one is an introduction to the ideas that will be necessary to understand the subsequent chapters, as well as a literature review of these topics. Chapter two is a paper that has been published in the ''Journal of Controlled Release'' that examines the mechanism of drug release from a polymer gel, as well as experimental design suggestions for the evaluation of water soluble drug delivery systems. Chapter three is a paper that has been published in the ''Journal of Pharmaceutical Sciences'' that discusses the effect ionic salts have on properties of the polymer systems examined in chapter two. Chapter four is a paper published in the Materials Research Society Fall 2000 Symposium Series dealing with the design and synthesis of a pH-sensitive polymeric drug delivery device. Chapter five is a paper that has been published in the journal ''Biomaterials'' proposing a novel polymer/metal composite for use as a biomaterial in hip arthroplasty surgery. Chapter six is a paper that will appear in an upcoming volume of the Journal ''Biomaterials'' dealing with the synthesis of a novel water soluble cationic polymer with possible applications in non-viral gene therapy. Chapter seven is a paper that has been submitted to ''Macromolecules'' discussing several novel block copolymers based on poly(ethylene glycol) and poly(diethylamino ethyl methacrylate) that possess both pH-sensitive and temperature sensitive properties. Chapter eight contains a

  9. The New Graphene Family Materials: Synthesis and Applications in Oxygen Reduction Reaction

    Directory of Open Access Journals (Sweden)

    Xin Tong


    Full Text Available Graphene family materials, including graphene quantum dots (GQDs, graphene nanoribbons (GNRs and 3D graphene (3D-G, have attracted much research interest for the oxygen reduction reaction (ORR in fuel cells and metal-air batteries, due to their unique structural characteristics, such as abundant activate sites, edge effects and the interconnected network. In this review, we summarize recent developments in fabricating various new graphene family materials and their applications for use as ORR electrocatalysts. These new graphene family materials play an important role in improving the ORR performance, thus promoting the practical use in metal-air batteries and fuel cells.

  10. Synthesis of Hollow Sphere and 1D Structural Materials by Sol-Gel Process. (United States)

    Li, Fa-Liang; Zhang, Hai-Jun


    The sol-gel method is a simple and facile wet chemical process for fabricating advanced materials with high homogeneity, high purity, and excellent chemical reactivity at a relatively low temperature. By adjusting the processing parameters, the sol-gel technique can be used to prepare hollow sphere and 1D structural materials that exhibit a wide application in the fields of catalyst, drug or gene carriers, photoactive, sensors and Li-ion batteries. This feature article reviewed the development of the preparation of hollow sphere and 1D structural materials using the sol-gel method. The effects of calcination temperature, soaking time, pH value, surfactant, etc., on the preparation of hollow sphere and 1D structural materials were summarized, and their formation mechanisms were generalized. Finally, possible future research directions of the sol-gel technique were outlined.

  11. Synthesis of Hollow Sphere and 1D Structural Materials by Sol-Gel Process (United States)

    Li, Fa-Liang; Zhang, Hai-Jun


    The sol-gel method is a simple and facile wet chemical process for fabricating advanced materials with high homogeneity, high purity, and excellent chemical reactivity at a relatively low temperature. By adjusting the processing parameters, the sol-gel technique can be used to prepare hollow sphere and 1D structural materials that exhibit a wide application in the fields of catalyst, drug or gene carriers, photoactive, sensors and Li-ion batteries. This feature article reviewed the development of the preparation of hollow sphere and 1D structural materials using the sol-gel method. The effects of calcination temperature, soaking time, pH value, surfactant, etc., on the preparation of hollow sphere and 1D structural materials were summarized, and their formation mechanisms were generalized. Finally, possible future research directions of the sol-gel technique were outlined. PMID:28841188

  12. Synthesis of hydrogen-carbon clathrate material and hydrogen evolution therefrom at moderate temperatures and pressures (United States)

    Lueking, Angela [State College, PA; Narayanan, Deepa [Redmond, WA


    A process for making a hydrogenated carbon material is provided which includes forming a mixture of a carbon source, particularly a carbonaceous material, and a hydrogen source. The mixture is reacted under reaction conditions such that hydrogen is generated and/or released from the hydrogen source, an amorphous diamond-like carbon is formed, and at least a portion of the generated and/or released hydrogen associates with the amorphous diamond-like carbon, thereby forming a hydrogenated carbon material. A hydrogenated carbon material including a hydrogen carbon clathrate is characterized by evolution of molecular hydrogen at room temperature at atmospheric pressure in particular embodiments of methods and compositions according to the present invention.

  13. Investigating the Heavy Metal Adsorption of Mesoporous Silica Materials Prepared by Microwave Synthesis

    National Research Council Canada - National Science Library

    Wenjie Zhu; Jingxuan Wang; Di Wu; Xitong Li; Yongming Luo; Caiyun Han; Wenhui Ma; Sufang He


    Mesoporous silica materials (MSMs) of the MCM-41 type were rapidly synthesized by microwave heating using silica fume as silica source and evaluated as adsorbents for the removal of Cu2+, Pb2+, and Cd2...

  14. Additive Manufacturing Synthesis of Novel Materials for 3000?C Applications Project (United States)

    National Aeronautics and Space Administration — Environmentally durable material systems capable of operating at temperatures from 1500 to 3000?C while maintaining structural integrity are enabling for future hot...

  15. Synthesis of suitable SiO2 nano particles as the core in core-shell nanostructured materials. (United States)

    Ghahari, Mehdi; Aghababazadeh, Roya; Ebadzadeh, Touradj; Mirhabibi, Alireza; Brydson, Rik; Fabbri, Paola; Najafi, Farhod


    The effect of surfactant on the luminescent intensity of SiO2 @Y2O3:Eu3+ particles with a core shell structure is described. Core-shell particles are used in phosphor materials and employing spherical particles with a narrow size distribution is vital for the enhancement of luminescent properties. Three kinds of different surfactants were used to synthesis SiO2 nano particles via a sol gel process. The results demonstrated that comb polycarboxylic acid surfactant had a significant influence on the morphology and particle size distribution. Somehow, particles with 100 nm size and narrow size distribution were produced. These particles had relatively uniform packing, unlike particles produced with other surfactants or without surfactant which had irregular assembly. The photoluminescence intensity of SiO2 @Y2O3:Eu3+ particles that was synthesized by comb polycarboxylic acid surfactant was higher than those which were produced without surfactant.

  16. Luminescence properties of ZnMoO4:Eu3+:Y3+ materials synthesized by solution combustion synthesis method (United States)

    Verma, Naveen; Mari, Bernabe; Singh, Krishan Chander; Jindal, Jitender; Mollar, Miguel; Yadav, Suprabha


    The Zn(1-x-y)MoO4:Eu3+(x): Y3+(y) (x = 1 mol% and y = 1 or 2 mol%) compounds were prepared by combustion synthesis method. The crystal structure of the samples was identified by X-ray diffraction (XRD). The photoluminescence properties were investigated and it is observed that the co-doping of Y3+ enhances the luminescence emission intensity of ZnMoO4:Eu3+ material. The Y3+ acts as a sensitizer in the ZnMoO4:Eu3+ lattice. The particle size is calculated from XRD data by using Scherer Equation. The particles has been found in the range of 30-40 nm.

  17. New Unsymmetrically Benzene-Fused Bis (Tetrathiafulvalene: Synthesis, Characterization, Electrochemical Properties and Electrical Conductivity of Their Materials

    Directory of Open Access Journals (Sweden)

    Tahar Abbaz


    Full Text Available The synthesis of new unsymmetrically benzene-fused bis (tetrathiafulvalene has been carried out by a cross-coupling reaction of the respective 4,5-dialkyl-1,3-dithiole-2-selenone 6–9 with 2-(4-(p-nitrophenyl-1,3-dithiole-2-ylidene-1,3,5,7-tetrathia-s-indacene-6-one 5 prepared by olefination of 4-(p-nitrophenyl-1,3-dithiole-2-selenone 3 and 1,3,5,7-tetrathia-s-indacene-2,6-dione 4. The conversion of the nitro moiety 10a–d to amino 11a–d then dibenzylamine 12a–d groups respectively used reduction and alkylation methods. The electron donor ability of these new compounds has been measured by cyclic voltammetry (CV technique. Charge transfer complexes with tetracyanoquino-dimethane (TCNQ were prepared by chemical redox reactions. The complexes have been proven to give conducting materials.

  18. Synthesis and Properties of Waterborne Polyurethane (WBPU/Modified Lignin Amine (MLA Adhesive: A Promising Adhesive Material

    Directory of Open Access Journals (Sweden)

    Mohammad Mizanur Rahman


    Full Text Available A series of waterborne polyurethane (WBPU/modified lignin amine (MLA adhesives was prepared using MLA as a chain extender by a prepolymer mixing process. A successful Mannich reaction was achieved during the synthesis of MLA by reacting lignin with bis(3-aminopropylamine. Higher tensile strength, Young’s modulus, and thermal stability were recorded for WBPU/MLA adhesives with higher MLA contents. The WBPU/MLA adhesive materials were used to coat polyvinyl chloride (PVC substrates. The adhesive strength increased with increasing MLA content. More importantly, the MLA also enhanced the WBPU/MLA coating in terms of adhesive strength at moderately high temperatures as well as under natural weather exposed conditions. The adhesive strength was essentially unaffected with 6.48 mol % MLA in the WBPU/MLA coating after exposure to natural weather conditions for 180 days.

  19. Solution plasma applications for the synthesis/modification of inorganic nanostructured materials and the treatment of natural polymers (United States)

    Watthanaphanit, Anyarat; Saito, Nagahiro


    Reducing the use of toxic chemicals, production steps, and time consumption are important concerns for researchers and process engineers to contribute in the quest for an efficient process in any production. If an equipment setup is simple, the process additionally becomes more profitable. Combination of the mentioned requirements has opened up various applications of the solution plasma process (SPP) — a physical means of generating plasma through an electrical discharge in a liquid medium at atmospheric pressure and room temperature. This review shows the progress of scientific research on the applications of the SPP for the synthesis/modification of inorganic nanostructured materials and the treatment of natural polymers. Development achieved in each application is demonstrated.

  20. Nickel hydroxides and related materials: a review of their structures, synthesis and properties


    Hall, David S.; Lockwood, David J.; Bock, Christina; MacDougall, Barry R.


    This review article summarizes the last few decades of research on nickel hydroxide, an important material in physics and chemistry, that has many applications in engineering including, significantly, batteries. First, the structures of the two known polymorphs, denoted as α-Ni(OH)2 and β-Ni(OH)2, are described. The various types of disorder, which are frequently present in nickel hydroxide materials, are discussed including hydration, stacking fault disorder, mechanical stresses and the inco...

  1. Synthesis-Structure-Property Relationships in Lead-Free Piezoelectric Materials


    Maurya, Deepam


    Piezoelectric materials find applications in multitude of devices such as sensors, actuators and energy harvesters. However, most of these piezoelectric materials utilize lead-based systems which are becoming serious problem owing to the restrictions imposed by regulatory agencies across the globe. In the functional ceramics community, currently there is no problem more important than to find a replacement for lead-based piezoelectrics used for actuators. The electromechanical properties requ...

  2. Recent Progress in Synthesis and Application of Low-Dimensional Silicon Based Anode Material for Lithium Ion Battery

    Directory of Open Access Journals (Sweden)

    Yuandong Sun


    Full Text Available Silicon is regarded as the next generation anode material for LIBs with its ultra-high theoretical capacity and abundance. Nevertheless, the severe capacity degradation resulting from the huge volume change and accumulative solid-electrolyte interphase (SEI formation hinders the silicon based anode material for further practical applications. Hence, a variety of methods have been applied to enhance electrochemical performances in terms of the electrochemical stability and rate performance of the silicon anodes such as designing nanostructured Si, combining with carbonaceous material, exploring multifunctional polymer binders, and developing artificial SEI layers. Silicon anodes with low-dimensional structures (0D, 1D, and 2D, compared with bulky silicon anodes, are strongly believed to have several advanced characteristics including larger surface area, fast electron transfer, and shortened lithium diffusion pathway as well as better accommodation with volume changes, which leads to improved electrochemical behaviors. In this review, recent progress of silicon anode synthesis methodologies generating low-dimensional structures for lithium ion batteries (LIBs applications is listed and discussed.

  3. De novo synthesis of a metal-organic framework material featuring ultrahigh surface area and gas storage capacities. (United States)

    Farha, Omar K; Yazaydın, A Özgür; Eryazici, Ibrahim; Malliakas, Christos D; Hauser, Brad G; Kanatzidis, Mercouri G; Nguyen, SonBinh T; Snurr, Randall Q; Hupp, Joseph T


    Metal-organic frameworks--a class of porous hybrid materials built from metal ions and organic bridges--have recently shown great promise for a wide variety of applications. The large choice of building blocks means that the structures and pore characteristics of the metal-organic frameworks can be tuned relatively easily. However, despite much research, it remains challenging to prepare frameworks specifically tailored for particular applications. Here, we have used computational modelling to design and predictively characterize a metal-organic framework (NU-100) with a particularly high surface area. Subsequent experimental synthesis yielded a material, matching the calculated structure, with a high BET surface area (6,143 m(2) g(-1)). Furthermore, sorption measurements revealed that the material had high storage capacities for hydrogen (164 mg g(-1)) and carbon dioxide (2,315 mg g(-1))--gases of high importance in the contexts of clean energy and climate alteration, respectively--in excellent agreement with predictions from modelling.

  4. Synthesis and hydrophobic adsorption properties of microporous/mesoporous hybrid materials. (United States)

    Hu, Qin; Li, Jinjun; Qiao, Shizhang; Hao, Zhengping; Tian, Hua; Ma, Chunyan; He, Chi


    Hybrid materials of silicalite-1 (Sil-1)-coated SBA-15 particles (MSs) have been successfully synthesized by crystallization process under hydrothermal conditions. These MSs materials were characterized by X-ray diffraction, nitrogen adsorption/desorption and TEM techniques, which illustrated that the silicalite-1-coated SBA-15 particles were successfully prepared and had large pore volume and hierarchical pore size distribution. Further experimental studies indicated that longer crystallization time under basic condition caused the mesostructure of SBA-15 materials to collapse destructively and higher calcination temperature tended to disrupt the long-range mesoscopic order while they had little influence on the phase of microcrystalline silicalite-1 zeolite. The resultant MSs materials were investigated by estimating dynamic adsorption capacity under dry and wet conditions to evaluate their adsorptive and hydrophobic properties. The hydrophobicity index (HI) value followed the sequence of silicalite-1>MSs>SBA-15, which revealed that the SBA-15 particles coated with the silicalite-1 seeds enhanced the surface hydrophobicity, and also were consistent with FTIR results. Our studies show that MSs materials combined the advantages of the ordered mesoporous material (high adsorptive capacity, large pore volume) and silicalite-1 zeolite (super-hydrophobic property, high hydrothermal stability), and the presence of micropores directly led to an increase in the dynamic adsorption capacity of benzene under dry and wet conditions.

  5. Synthesis and characterization of zeolite P using technical-grade materials

    CERN Document Server

    Aghabozorg, H R; Aghabozorg, H R; Sharif, M


    Research attempts on zeolites show structural and industrial importance of these inorganic compounds. In this regard, the synthesis of zeolites is of great importance, because their natural occurring counterparts are often impure. Zeolite Na-P with a silicon to aluminium ratio of one has a better ion exchange capacity than Na-A and can be used as a detergent builder. In this work, zeolite Na-P of high purity was successfully synthesized using commercial silica and alumina sources. parameters such as H sub 2 O:A1 sub 2 O sub 3 and SiO sub 2 :A1 sub 2 O sub 3 molar ratios and crystallization temperature and time were investigated. So that the optimum condition was obtained. X-ray powder diffraction, infrared, scanning electron microscopy and elemental analysis were utilized for the characterization of the product.

  6. On the anomalies in gold nanoparticles prepared by micelle nanolithography and their impact on one-dimensional material synthesis. Role of substrate, size effects and impurity

    Energy Technology Data Exchange (ETDEWEB)

    Mbenkum, B.N.


    The synthesis of one-dimensional (1-D) inorganic semiconductor materials such as nanotubes and silicon (Si) nanowires is usually achieved by catalyst nanoparticlemediated synthetic routes. Despite the well-established nature of this technique, problems such as low temperature synthesis and adequate control of catalyst nanoparticle diameter in order to control 1-D material diameter still prevail. Additionally, the expansion of this technology from crystalline to cheaper substrates such as glass remains demanding. This work employs a previously established selfassembly route to produce controlled spatial distribution of substrate anchored small diameter gold nanoparticles with controlled size. This enabled successful synthesis of Si 1-D structures with controlled diameters less than 20 nm. Low temperature synthesis due to enhanced catalytic activity was achieved via introduction of impurity by treatment of gold nanoparticles in different plasma environments. This enabled Si 1-D structure growth on Si, SiO{sub x}/Si and borosilicate glass substrates at 320 C. Substrate-induced stress affected Si diffusion at the gold nanoparticle determining whether Si nanowires or nanotubes were grown. These results are of technological relevance because low temperature synthesis provides an economical approach and controlled diameter enhances material functionality. Additionally, exploiting substrate-induced stress to influence Si diffusion in nanoparticles provides an alternate route to tuning Si 1-D structure. (orig.)

  7. Design and synthesis of vanadium hydrazide gels for Kubas-type hydrogen adsorption: a new class of hydrogen storage materials. (United States)

    Hoang, Tuan K A; Webb, Michael I; Mai, Hung V; Hamaed, Ahmad; Walsby, Charles J; Trudeau, Michel; Antonelli, David M


    In this paper we demonstrate that the Kubas interaction, a nondissociative form of weak hydrogen chemisorption with binding enthalpies in the ideal 20-30 kJ/mol range for room-temperature hydrogen storage, can be exploited in the design of a new class of hydrogen storage materials which avoid the shortcomings of hydrides and physisorpion materials. This was accomplished through the synthesis of novel vanadium hydrazide gels that use low-coordinate V centers as the principal Kubas H(2) binding sites with only a negligible contribution from physisorption. Materials were synthesized at vanadium-to-hydrazine ratios of 4:3, 1:1, 1:1.5, and 1:2 and characterized by X-ray powder diffraction, X-ray photoelectron spectroscopy, nitrogen adsorption, elemental analysis, infrared spectroscopy, and electron paramagnetic resonance spectroscopy. The material with the highest capacity possesses an excess reversible storage of 4.04 wt % at 77 K and 85 bar, corresponding to a true volumetric adsorption of 80 kg H(2)/m(3) and an excess volumetric adsorption of 60.01 kg/m(3). These values are in the range of the ultimate U.S. Department of Energy goal for volumetric density (70 kg/m(3)) as well as the best physisorption material studied to date (49 kg H(2)/m(3) for MOF-177). This material also displays a surprisingly high volumetric density of 23.2 kg H(2)/m(3) at room temperature and 85 bar--roughly 3 times higher than that of compressed gas and approaching the DOE 2010 goal of 28 kg H(2)/m(3). These materials possess linear isotherms and enthalpies that rise on coverage and have little or no kinetic barrier to adsorption or desorption. In a practical system these materials would use pressure instead of temperature as a toggle and can thus be used in compressed gas tanks, currently employed in many hydrogen test vehicles, to dramatically increase the amount of hydrogen stored and therefore the range of any vehicle.

  8. Design, synthesis, and initial evaluation of D-glyceraldehyde crosslinked gelatin-hydroxyapatite as a potential bone graft substitute material (United States)

    Florschutz, Anthony Vatroslav

    Utilization of bone grafts for the treatment of skeletal pathology is a common practice in orthopaedic, craniomaxillofacial, dental, and plastic surgery. Autogenous bone graft is the established archetype but has disadvantages including donor site morbidity, limited supply, and prolonging operative time. In order to avoid these and other issues, bone graft substitute materials are becoming increasingly prevalent among surgeons for reconstructing skeletal defects and arthrodesis applications. Bone graft substitutes are biomaterials, biologics, and guided tissue/bone regenerative devices that can be used alone or in combinations as supplements or alternatives to autogenous bone graft. There is a growing interest and trend to specialize graft substitutes for specific indications and although there is good rationale for this indication-specific approach, the development and utility of a more universal bone graft substitute may provide a better answer for patients and surgeons. The aim of the present research focuses on the design, synthesis, and initial evaluation of D-glyceraldehyde crosslinked gelatin-hydroxyapatite composites for potential use as a bone graft substitutes. After initial establishment of rational material design, gelatinhydroxyapatite scaffolds were fabricated with different gelatin:hydroxyapatite ratios and crosslinking concentrations. The synthesized scaffolds were subsequently evaluated on the basis of their swelling behavior, porosity, density, percent composition, mechanical properties, and morphology and further assessed with respect to cell-biomaterial interaction and biomineralization in vitro. Although none of the materials achieved mechanical properties suitable for structural graft applications, a reproducible material design and synthesis was achieved with properties recognized to facilitate bone formation. Select scaffold formulations as well as a subset of scaffolds loaded with recombinant human bone morphogenetic protein-2 were

  9. Synthesis, characterization and bioevaluation of drug-collagen hybrid materials for biomedical applications. (United States)

    Voicu, Georgeta; Geanaliu-Nicolae, Ruxandra-Elena; Pîrvan, Adrian-Alexandru; Andronescu, Ecaterina; Iordache, Florin


    This work presents a study based on the preparation and characterization of drug-collagen hybrid materials. Materials used for obtaining drug-collagen hybrids were collagen type I (Coll) as matrix and fludarabine (F) and epirubicin (E) as hydrophilic active substances. After incorporation of drugs into Coll in different ratios, the obtained hybrid materials (Coll/F and Coll/E) could be used according to our results as potential drug delivery systems in medicine for the topical (local) treatment of cancerous tissues (e.g. the treatment of breast, stomach, lung, colorectal or advanced ovarian cancer). The materials were characterized considering their composition (by XRD, FT-IR and DTA-TG) and their morphology (by SEM). The delivery of drug was assessed by UV-vis. The in vitro citotoxicity demonstrates an antitumoral activity of the obtained hybrid materials and their potential use for biomedical applications as drug delivery systems in tumoral treatments. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Synthesis of granular zeolitic materials with high cation exchange capacity from agglomerated coal fly ash

    Energy Technology Data Exchange (ETDEWEB)

    Roberto Juan; Susana Hernandez; Jose Manuel Andres; Carmen Ruiz [Instituto de Carboquimica (CSIC), Zaragoza (Spain)


    Fly ash from coal combustion is a potential source of pollution and there is continuous interest in its recycling by converting it into products such as zeolitic materials for use in retaining pollutants. In this paper, production of granular zeolitic material from a commercially-unusable fine-fraction of a lightweight aggregate (LA) building material made from coal fly ash agglomerated with lime, by conventional alkaline activation is described. NaP1 zeolite, K-F zeolite, K-Phillipsite and K-Chabazite were synthesised. The process was optimised by combining four reaction parameters (temperature, alkali concentration, solution/fly ash ratio and reaction time). Zeolitic materials with the highest zeolite yields and cation exchange capacities were selected for future application in environmental processes. End-product zeolitic materials maintain its granular form and this could favour their use in some particular applications for environmental waste treatment (e.g. ionic exchange in column) without any further transformation stages. 21 refs., 6 figs., 6 tabs.

  11. Cost-effective synthesis of environmentally benign materials on the basis of poly-3-hydroxybutyrate

    Directory of Open Access Journals (Sweden)

    H. Häberlein


    Full Text Available As an example for an environmentally benign and low-cost material we prepared blends from 1. copolyester-urethanes (PEU and 2. cellulose acetate recycling material (CAR. The copolyester-urethanes were prepared by joining blocks of alpha, omega-(poly-(R-3-hydroxybutyrate-diol and poly-butylenglycol-adipate-diol with hexamethylene diisocyanate. Fibrous CAR was transformed into a short-fiber felt by textile technology and calendared into the PEU melt. The processing of the blends was done at 80 - 100 °C mainly by injection molding. The mechanical properties of the tough-elastic materials were studied with respect to the influence of the PEU composition and the ratio of CAR admixture. The starting materials, (R-PHB and cellulose derivatives are obtained from agrarian resources. Therefore, the resulting polymers are stable under conditions of usage, yet readily bio-degradable on soil deposition. Mixing with cellulose acetate waste material allows for cost-effective production of such blends.

  12. Poly-L-arginine based materials as instructive substrates for fibroblast synthesis of collagen. (United States)

    Bygd, Hannah C; Akilbekova, Dana; Muñoz, Adam; Forsmark, Kiva D; Bratlie, Kaitlin M


    The interactions of cells and surrounding tissues with biomaterials used in tissue engineering, wound healing, and artificial organs ultimately determine their fate in vivo. We have demonstrated the ability to tune fibroblast responses with the use of varied material chemistries. In particular, we examined cell morphology, cytokine production, and collagen fiber deposition angles in response to a library of arginine-based polymeric materials. The data presented here shows a large range of vascular endothelial growth factor (VEGF) secretion (0.637 ng/10(6) cells/day to 3.25 ng/10(6) cells/day), cell migration (∼15 min materials in wound healing and tissue engineering applications. Copyright © 2015 Elsevier Ltd. All rights reserved.

  13. Synthesis and biological evaluation of PMMA/MMT nanocomposite as denture base material. (United States)

    Zheng, Junping; Su, Qiang; Wang, Chen; Cheng, Gang; Zhu, Ran; Shi, Jin; Yao, Kangde


    Inorganic-polymer nanocomposites are of significant interest for emerging materials due to their improved properties and unique combination of properties. Poly (methylmethacrylate) (PMMA)/montmorillonite (MMT) nanocomposites were prepared by in situ suspension polymerization with dodecylamine used as MMT-modifier. X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used to characterize the structures of the nanocomposites. Cytotoxicity test, hemolysis test, acute systemic toxicity test, oral mucous membrane irritation test, guinea-pig maximization test and mouse bone-marrow micronucleus test were used to evaluate the biocompatibility of PMMA/MMT nanocomposites. The results indicated that an exfoliated nanocomposite was achieved, and the resulting nanocomposites exhibited excellent biocompatibility as denture base material and had potential application in dental materials.

  14. Nanoporous Materials as New Engineered Catalysts for the Synthesis of Green Fuels

    Directory of Open Access Journals (Sweden)

    Ioana Fechete


    Full Text Available This review summarizes the importance of nanoporous materials and their fascinating structural properties with respect to the catalytic and photocatalytic reduction of CO2 to methane, toward achieving a sustainable energy supply. The importance of catalysis as a bridge step for advanced energy systems and the associated environmental issues are stressed. A deep understanding of the fundamentals of these nanoporous solids is necessary to improve the design and efficiency of CO2 methanation. The role of the support dominates the design in terms of developing an efficient methanation catalyst, specifically with respect to ensuring enhanced metal dispersion and a long catalyst lifetime. Nanoporous materials provide the best supports for Ni, Ru, Rh, Co, Fe particles because they can prevent sintering and deactivation through coking, which otherwise blocks the metal surface as carbon accumulates. This review concludes with the major challenges facing the CO2 methanation by nanoporous materials for fuel applications.

  15. The synthesis, properties and uses of carbon materials with helical morphology

    Directory of Open Access Journals (Sweden)

    Ahmed Shaikjee


    Full Text Available Carbon nanostructures have been widely studied due to their unique properties and potential use in various applications. Of interest has been the study of carbonaceous material with helical morphologies, due to their unique chemical, mechanical, electrical and field emission properties. As such it is envisaged that these materials could be excellent candidates for incorporation in numerous nanotechnology applications. However in order to achieve these aspirations, an understanding of the growth mechanisms and synthetic strategies is necessary. Herein we consider historical and current investigations as reported in the literature, and provide a comprehensive outline of growth mechanisms, synthetic strategies and applications related to helical carbon nanomaterials.

  16. Truly Absorbed Microbial Protein Synthesis, Rumen Bypass Protein, Endogenous Protein, and Total Metabolizable Protein from Starchy and Protein-Rich Raw Materials

    NARCIS (Netherlands)

    Parand, Ehsan; Vakili, Alireza; Mesgaran, Mohsen Danesh; Duinkerken, Van Gert; Yu, Peiqiang


    This study was carried out to measure truly absorbed microbial protein synthesis, rumen bypass protein, and endogenous protein loss, as well as total metabolizable protein, from starchy and protein-rich raw feed materials with model comparisons. Predictions by the DVE2010 system as a more

  17. Effect of the raw material type and the reaction time on the synthesis of halloysite based Zeolite Na-P1 (United States)

    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.

  18. A facile approach for the synthesis of monolithic hierarchical porous carbons – high performance materials for amine based CO2 capture and supercapacitor electrode

    KAUST Repository

    Estevez, Luis


    An ice templating coupled with hard templating and physical activation approach is reported for the synthesis of hierarchically porous carbon monoliths with tunable porosities across all three length scales (macro- meso- and micro), with ultrahigh specific pore volumes [similar]11.4 cm3 g−1. The materials function well as amine impregnated supports for CO2 capture and as supercapacitor electrodes.

  19. Paper pulp waste—A new source of raw material for the synthesis of ...

    Indian Academy of Sciences (India)


    Abstract. A synthetic porous ceramic composite material consisting of the mullite, cordierite and cristobalite phases is produced from a mixture of paper pulp waste and clay by reaction sintering at 1400°C. Physico- mechanical properties such as bul