WorldWideScience

Sample records for diborane

  1. Photochemistry and infrared spectrum of single-bridged diborane(5) anion isolated in solid argon

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Meng-Chen; Chin, Chih-Hao; Chen, Sian-Cong; Huang, Tzu-Ping [National Synchrotron Radiation Research Center (NSRRC), 101 Hsin-Ann Road, Hsinchu Science Park, Hsinchu 30076, Taiwan (China); Chen, Hui-Fen; Huang, Wei-Jie [Department of Medicinal and Applied Chemistry, Kaohsiung Medical University, 100, Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China); Wu, Yu-Jong, E-mail: yjw@nsrrc.org.tw [National Synchrotron Radiation Research Center (NSRRC), 101 Hsin-Ann Road, Hsinchu Science Park, Hsinchu 30076, Taiwan (China); Department of Applied Chemistry, National Chiao Tung University, 1001, Ta-Hsueh Road, Hsinchu 30010, Taiwan (China)

    2016-08-21

    Three-center two-electron bonds are important for understanding electron-deficient molecules. To examine such a molecule, we produced a diborane(5) anion with a single-bridged structure upon electron bombardment during matrix deposition of Ar containing a small proportion of diborane(6). The diborane(5) anion was destroyed upon photolysis at 180, 220, 385, and 450 nm, but not at 532 nm. Moreover, the possible formation of neutral diborane(5) was observed upon photolysis at 385 and 450 nm, whereas neutral diborane(3) was observed upon photolysis at 180 and 220 nm. The observed line wavenumbers, relative intensities, and isotopic ratios of the diborane(5) anion agreed satisfactorily with those predicted by density functional theory calculations at the B3LYP/aug-cc-pVTZ level of theory. Thus, this method produced the boron hydride anion of interest with few other fragments, which enabled us to clearly identify the IR spectrum of the diborane(5) anion.

  2. Easy access to nucleophilic boron through diborane to magnesium boryl metathesis

    Science.gov (United States)

    Pécharman, Anne-Frédérique; Colebatch, Annie L.; Hill, Michael S.; McMullin, Claire L.; Mahon, Mary F.; Weetman, Catherine

    2017-04-01

    Organoboranes are some of the most synthetically valuable and widely used intermediates in organic and pharmaceutical chemistry. Their synthesis, however, is limited by the behaviour of common boron starting materials as archetypal Lewis acids such that common routes to organoboranes rely on the reactivity of boron as an electrophile. While the realization of convenient sources of nucleophilic boryl anions would open up a wealth of opportunity for the development of new routes to organoboranes, the synthesis of current candidates is generally limited by a need for highly reducing reaction conditions. Here, we report a simple synthesis of a magnesium boryl through the heterolytic activation of the B-B bond of bis(pinacolato)diboron, which is achieved by treatment of an easily generated magnesium diboranate complex with 4-dimethylaminopyridine. The magnesium boryl is shown to act as an unambiguous nucleophile through its reactions with iodomethane, benzophenone and N,N'-di-isopropyl carbodiimide and by density functional theory.

  3. Characterization of electron-deficient chemical bonding of diborane with attosecond electron wavepacket dynamics and laser response

    International Nuclear Information System (INIS)

    Yonehara, Takehiro; Takatsuka, Kazuo

    2009-01-01

    We report a theoretical study of non-adiabatic electrons-nuclei coupled dynamics of diborane H 2 BH 2 BH 2 under several types of short pulse lasers. This molecule is known to have particularly interesting geometrical and electronic structures, which originate from the electron-deficient chemical bondings. We revisit the chemical bonding of diborane from the view point of electron wavepacket dynamics coupled with nuclear motions, and attempt to probe the characteristics of it by examining its response to intense laser fields. We study in the following three aspects, (i) bond formation of diborane by collision between two monoboranes, (ii) attosecond electron wavepacket dynamics in the ground state and first excited state by circularly polarized laser pulse, and (iii) induced fragmentation back to monoborane molecules by linearly polarized laser. The wave lengths of two types of laser field employed are 200 nm (in UV range) and 800 nm (in IR range), and we track the dynamics from hundreds of attoseconds up to few tens of femtoseconds. To this end, we apply the ab initio semiclassical Ehrenfest theory, into which the classical vector potential of a laser field is introduced. Basic features of the non-adiabatic response of electrons to the laser fields is elucidated in this scheme. To analyze the electronic wavepackets thus obtained, we figure out bond order density that is a spatial distribution of the bond order and bond order flux density arising only from the bonding regions, and so on. Main findings in this work are: (i) dimerization of monoboranes to diborane is so efficient that even intense laser is hard to prevent it; (ii) collective motions of electron flux emerge in the central BHHB bonding area in response to the circularly polarized laser fields; (iii) laser polarization with the direction of central two BH bonding vector is efficient for the cleavage of BH 3 -BH 3 ; and (iv) nuclear derivative coupling plays a critical role in the field induced

  4. Preparation of Zn(BH4)2 and diborane and hydrogen release properties of Zn(BH4)2+xMgH2 (x=1, 5, 10, and 15)

    Science.gov (United States)

    Kwak, Young Jun; Kwon, Sung Nam; Song, Myoung Youp

    2015-09-01

    Zn(BH4)2 was prepared by milling ZnCl2 and NaBH4 in a planetary ball mill under Ar atmosphere, and Zn(BH4)2+xMgH2 (x=1, 5, 10, and 15) samples were prepared. Diborane (B2H6) and hydrogen release characteristics of the Zn(BH4)2 and Zn(BH4)2+xMgH2 samples were studied. The samples synthesized by milling ZnCl2 and NaBH4 contained Zn(BH4)2 and NaCl, together with small amounts of ZnCl2 and NaBH4. We designated these samples as Zn(BH4)2(+NaCl). The weight loss up to 400 °C of the Zn(BH4)2(+NaCl) sample synthesized by milling 4 h was 11.2 wt%. FT-IR analysis showed that Zn(BH4)2 was formed in the Zn(BH4)2(+NaCl) samples. MgH2 was also milled in a planetary ball mill, and mixed with the Zn(BH4)2(+NaCl) synthesized by milling for 4 h in a mortar and pestle. The weight loss up to 400 °C of Zn(BH4)2(+NaCl)+MgH2 was 8.2 wt%, corresponding to the weight % of diborane and hydrogen released from the Zn(BH4)2(+NaCl)+MgH2 sample, with respect to the sample weight. DTA results of Zn(BH4)2(+NaCl)+xMgH2 showed that the decomposition peak of Zn(BH4)2 was at about 61 °C, and that of MgH2 was at about 370-389 °C.

  5. Synthesis, Structure, Bonding, and Reactivity of Metal Complexes Comprising Diborane(4) and Diborene(2): [{Cp*Mo(CO)2 }2 {μ-η2 :η2 -B2 H4 }] and [{Cp*M(CO)2 }2 B2 H2 M(CO)4 ], M=Mo,W.

    Science.gov (United States)

    Mondal, Bijan; Bag, Ranjit; Ghorai, Sagar; Bakthavachalam, K; Jemmis, Eluvathingal D; Ghosh, Sundargopal

    2018-04-26

    The reaction of [(Cp*Mo) 2 (μ-Cl) 2 B 2 H 6 ] (1) with CO at room temperature led to the formation of the highly fluxional species [{Cp*Mo(CO) 2 } 2 {μ-η 2 :η 2 -B 2 H 4 }] (2). Compound 2, to the best of our knowledge, is the first example of a bimetallic diborane(4) conforming to a singly bridged C s structure. Theoretical studies show that 2 mimics the Cotton dimolybdenum-alkyne complex [{CpMo(CO) 2 } 2 C 2 H 2 ]. In an attempt to replace two hydrogen atoms of diborane(4) in 2 with a 2e [W(CO) 4 ] fragment, [{Cp*Mo(CO) 2 } 2 B 2 H 2 W(CO) 4 ] (3) was isolated upon treatment with [W(CO) 5 ⋅thf]. Compound 3 shows the intriguing presence of [B 2 H 2 ] with a short B-B length of 1.624(4) Å. We isolated the tungsten analogues of 3, [{Cp*W(CO) 2 } 2 B 2 H 2 W(CO) 4 ] (4) and [{Cp*W(CO) 2 } 2 B 2 H 2 Mo(CO) 4 ] (5), which provided direct proof of the existence of the tungsten analogue of 2. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Spiro(phosphoamidite) ligand (SIPHOS)/Cu(OTf)2-catalyzed highly regio-and stereo-selective hydroborations of internal alkynes with diborane in water

    Institute of Scientific and Technical Information of China (English)

    Qing-Qing Xuan; Ya-Hui Wei; Qiu-Ling Song

    2017-01-01

    The highly regio-and stereoselective hydroborations of unactivated internal alkynes with diboron compound catalyzed by Cu(OTf)2 with spiro(phosphoamidite) as ligand in the presence of Cs2CO3 in water was developed.This protocol was applied efficiently in the aqueous synthesis of multi-substituted vinylboranes.

  7. Post-synthesis amine borane functionalization of metal-organic framework and its unusual chemical hydrogen release phenomenon

    KAUST Repository

    Berke, Heinz; Barman, Smair; Remhof, Arndt; Koitz, Ralph; Iannuzzi, Marcella; Blacque, Olivier; Yan, Yigang; Fox, Thomas; Hutter, Jü rg; Zü ttel, Andreas

    2017-01-01

    We report a novel strategy for post-synthesis amine borane functionalization of MOFs under gas-solid phase transformation utilizing gaseous diborane. The covalently confined amine borane derivative decorated on the framework backbone is stable when

  8. Hydrolysis of Mg(BH4)2 and its coordination compounds as a way to obtain hydrogen

    Science.gov (United States)

    Solovev, Mikhail V.; Chashchikhin, Oleg V.; Dorovatovskii, Pavel V.; Khrustalev, Victor N.; Zyubin, A. S.; Zyubina, T. S.; Kravchenko, O. V.; Zaytsev, Alexey A.; Dobrovolsky, Yu. A.

    2018-02-01

    Three ligand-stabilized Mg(BH4)2-based complexes have been synthesized and evaluated as potential hydrogen storage media for portable fuel cell applications. The new borohydrides: Mg(BH4)2 × 0.5Et2O and Mg(BH4)2 × diglyme (diglyme - CH3O(CH2)2O(CH2)2OCH3) have been synthesized and examined by X-ray single crystal diffraction method. Hydrolysis reactions of the compounds liberate hydrogen in quantities ranging from 46 to 96% of the theoretical yield. The hydrolysis of Mg(BH4)2 and other borohydrides is also accompanied by the diborane formation. The amount of liberated diborane depends on the Mg-coordination environment. To explain this fact quantum-chemical calculations have been performed. It is shown that formation of Mg-O-Mg-bridges enables the side process of diborane generation. It means that the size and denticity of the ligand directly affects the amount of released diborane. In general, the larger the ligand and the higher its denticity, the smaller is amount of diborane produced. The new compound Mg(BH4)2 × diglyme decomposes without diborane formation that allows one to be considered as a new promising chemical hydrogen storage compound for the practical usage.

  9. A system to deposit boron films (boronization) in the DIII-D tokamak

    International Nuclear Information System (INIS)

    Hodapp, T.R.; Jackson, G.L.; Phillips, J.; Holtrop, K.L.; Peterson, P.L.; Winters, J.

    1992-01-01

    A system has been added to the DIII-D tokamak to coat its plasma facing surfaces with a film of boron using diborane gas. The system includes special health and safety equipment for handling the diborane gas which is toxic and inflammable. The purpose f the boron film is to reduce the levels of impurity atoms in the DIII-D plasmas. Experiments following the application of the boron film in DIII-D have led to significant reductions in plasma impurity levels and the observation of a new, very high confinement regime

  10. A system to deposit boron films (boronization) in the DIII-D tokamak

    International Nuclear Information System (INIS)

    Hodapp, T.R.; Jackson, G.L.; Phillips, J.; Holtrop, K.L.; Petersen, P.I.; Winter, J.

    1991-09-01

    A system has been added to the D3-D tokamak to coat its plasma facing surfaces with a film of boron using diborane gas. The system includes special health and safety equipment for handling the diborane gas which is toxic and inflammable. The purpose of the boron film is to reduce the levels of impurity atoms in the D3-D plasmas. Experiments following the application of the boron film in D3-D have led to significant reductions in plasma impurity levels and the observation of a new, very high confinement regime. 9 refs., 1 fig

  11. A Military Guide to Terrorism in the Twenty-First Century. U.S. Army DCSINT Handbook No. 1 (Version 3.0)

    Science.gov (United States)

    2005-08-15

    or varnished brown Length: 102mm Width: 61mm Weight: 773g Filler: Amatol Characteristics Color: Black and unmarked Length: 131mm Width: 55mm...isocyanate Diborane Boron tribromide Nitrogen dioxide Ethylene oxide Carbon monoxide Phosphine Fluorine Carbonyl sulfide Phosphorus oxychloride

  12. Electrically active, doped monocrystalline silicon nanoparticles produced by hot wire thermal catalytic pyrolysis

    CSIR Research Space (South Africa)

    Scriba, MR

    2011-05-01

    Full Text Available Doped silicon nanoparticles have successfully been produced by hot wire thermal catalytic pyrolysis at 40 mbar and a filament temperature of 1800 °C, using a mixture of silane and diborane or phosphine. All particles are monocrystalline with shapes...

  13. Substrate temperature dependence of microcrystallinity in plasma-deposited, boron-doped hydrogenated silicon alloys

    International Nuclear Information System (INIS)

    Rajeswaran, G.; Kampas, F.J.; Vanier, P.E.; Sabatini, R.L.; Tafto, J.

    1983-01-01

    The glow-discharge decomposition of silane diluted in hydrogen using diborane as a dopant results in the deposition of p-type microcrystalline silicon films at relatively low temperatures. The conductivity of these films is critically dependent on the substrate temperature when the ratio of silane flow rate to total gas flow rate is 1%. Electron micrographs show that highly conducting films contain numerous clusters of 2.5-nm crystallites that are embedded in an amorphous medium

  14. Formation of amorphous metal alloys by chemical vapor deposition

    Science.gov (United States)

    Mullendore, A.W.

    1988-03-18

    Amorphous alloys are deposited by a process of thermal dissociation of mixtures of organometallic compounds and metalloid hydrides,e.g., transition metal carbonyl, such as nickel carbonyl and diborane. Various sizes and shapes of deposits can be achieved, including near-net-shape free standing articles, multilayer deposits, and the like. Manipulation or absence of a magnetic field affects the nature and the structure of the deposit. 1 fig.

  15. Low-temperature synthesis of superconducting nanocrystalline MgB2

    International Nuclear Information System (INIS)

    Lu, J.; Xiao, Z.; Lin, Q.; Claus, H.; Fang, Z.Z.

    2010-01-01

    Magnesium diboride (MgB 2 ) is considered a promising material for practical application in superconducting devices, with a transition temperature near 40 K. In the present paper, nanocrystalline MgB 2 with an average particle size of approximately 70 nm is synthesized by reacting LiBH 4 with MgH 2 at temperatures as low as 450 C. This synthesis approach successfully bypasses the usage of either elemental boron or toxic diborane gas. The superconductivity of the nanostructures is confirmed by magnetization measurements, showing a superconducting critical temperature of 38.7 K.

  16. Optical Second Harmonic Spectroscopy of Boron-Reconstructed Si(001)

    International Nuclear Information System (INIS)

    Lim, D.; Downer, M. C.; Ekerdt, J. G.; Arzate, N.; Mendoza, Bernardo S.; Gavrilenko, V. I.; Wu, R. Q.

    2000-01-01

    Optical second harmonic generation (SHG) spectroscopy is used to probe Si(001) following thermal decomposition of diborane at the surface. Incorporation of boron (B) at second layer substitutional sites at H-free Si(001) intensifies and redshifts the E 1 SHG spectral peak, while subsequent H termination further intensifies and blueshifts E 1 , in sharp contrast to the effect of bulk B doping or nonsubstitutional B. Ab initio pseudopotential and semiempirical tight binding calculations independently reproduce these unique trends, and attribute them to the surface electric field associated with charge transfer to electrically active B acceptors, and rehybridization of atomic bonds. (c) 2000 The American Physical Society

  17. Boron profiles in doped amorphous-silicon solar cells formed by plasma ion deposition

    International Nuclear Information System (INIS)

    Stoddart, C.T.H.; Hunt, C.P.; Coleman, J.H.

    1979-01-01

    Amorphous silicon p-n junction solar cells of large area (100 cm 2 ) and having a quantum efficiency approaching 100% in the blue region have been prepared by plasma ion-plating, the p layer being formed from diborane and silane gases in a cathode glow-discharge. Surface secondary ion mass spectrometry combined with ion beam etching was found to be a very sensitive method with high in-depth resolution for obtaining the initial boron-silicon profile of the solar cell p-n junction. (author)

  18. Gas solubilities widespread applications

    CERN Document Server

    Gerrard, William

    1980-01-01

    Gas Solubilities: Widespread Applications discusses several topics concerning the various applications of gas solubilities. The first chapter of the book reviews Henr's law, while the second chapter covers the effect of temperature on gas solubility. The third chapter discusses the various gases used by Horiuti, and the following chapters evaluate the data on sulfur dioxide, chlorine data, and solubility data for hydrogen sulfide. Chapter 7 concerns itself with solubility of radon, thoron, and actinon. Chapter 8 tackles the solubilities of diborane and the gaseous hydrides of groups IV, V, and

  19. Preparation methods and properties of allylboranes

    International Nuclear Information System (INIS)

    Mikhajlov, B.M.

    1976-01-01

    The methods of synthesis and chemical properties of allylboron compounds of different types are considered as well as the application in organic chemistry, for example, for synthesis of 1-boroadamantane and adamantane compounds. PMR study of triallylborane reveals permanent allyl rearrangement. The paper describes the ability to complex formation, reactions with organometal compounds and some other agents, reactions with diborane and tetraalkyldiboranes, reactions with carbonyl compounds and nitriles, reactions with compounds containing activated double carbon-carbon bond, reactions with acetylene compounds, and reaction with allene compounds

  20. Reduced-pressure chemical vapor deposition of boron-doped Si and Ge layers

    International Nuclear Information System (INIS)

    Bogumilowicz, Y.; Hartmann, J.M.

    2014-01-01

    We have studied the in-situ boron (B) doping of germanium (Ge) and silicon (Si) in Reduced Pressure-Chemical Vapor Deposition. Three growth temperatures have been investigated for the B-doping of Ge: 400, 600 and 750 °C at a constant growth pressure of 13300 Pa (i.e. 100 Torr). The B concentration in the Ge:B epilayer increases linearly with the diborane concentration in the gaseous phase. Single-crystalline Ge:B layers with B concentrations in-between 9 ∙ 10 17 and 1 ∙ 10 20 cm −3 were achieved. For the in-situ B doping of Si at 850 °C, two dichlorosilane mass flow ratios (MFR) have been assessed: F[SiH 2 Cl 2 ]/F[H 2 ] = 0.0025 and F[SiH 2 Cl 2 ]/F[H 2 ] = 0.0113 at a growth pressure of 2660 Pa (i.e. 20 Torr). Linear boron incorporation with the diborane concentration in the gas phase has been observed and doping levels in-between 3.5 ∙ 10 17 and 1 ∙ 10 20 cm −3 were achieved. We almost kept the same ratio of B versus Si atoms in the gas phase and in the Si epilayer. By contrast, roughly half of the B atoms present in the gas phase were incorporated in the Ge:B layers irrespective of the growth temperature. X-Ray Diffraction (XRD) allowed us to extract from the angular position of the Ge:B layer diffraction peak the substitutional B concentration. Values close to the B concentrations obtained by 4-probe resistivity measurements were obtained. Ge:B layers were smooth (< 1 m root mean square roughness associated with 20 × 20 μm 2 Atomic Force Microscopy images). Only for high F[B 2 H 6 ]/F[GeH 4 ] MFR (3.2 10 −3 ) did the Ge:B layers became rough; they were however still mono-crystalline (XRD). Above this MFR value, Ge:B layers became polycrystalline. - Highlights: • Boron doping of germanium and silicon in Reduced Pressure-Chemical Vapor Deposition • Linear boron incorporation in Ge:B and Si:B with the diborane flow • Single-crystal Ge:B layers with B concentrations in-between 9 ∙ 10 17 and 1 ∙ 10 20 cm −3 • Single-crystal Si

  1. Superconducting phases of phosphorus hydride under pressure. Stabilization by mobile molecular hydrogen

    Energy Technology Data Exchange (ETDEWEB)

    Bi, Tiange; Miller, Daniel P.; Shamp, Andrew; Zurek, Eva [Department of Chemistry, State University of New York, Buffalo, NY (United States)

    2017-08-14

    At 80 GPa, phases with the PH{sub 2} stoichiometry, which are composed of simple cubic like phosphorus layers capped with hydrogen atoms and layers of H{sub 2} molecules, are predicted to be important species contributing to the recently observed superconductivity in compressed phosphine. The electron-phonon coupling in these phases results from the motions of the phosphorus atoms and the hydrogen atoms bound to them. The role of the mobile H{sub 2} layers is to decrease the Coulomb repulsion between the negatively charged hydrogen atoms capping the phosphorus layers. An insulating PH{sub 5} phase, the structure and bonding of which is reminiscent of diborane, is also predicted to be metastable at this pressure. (copyright 2017 Wiley-VCH Verlag GmbH and Co. KGaA, Weinheim)

  2. FTIR and electrical characterization of a-Si:H layers deposited by PECVD at different boron ratios

    Energy Technology Data Exchange (ETDEWEB)

    Orduna-Diaz, A., E-mail: abdu@susu.inaoep.mx [Instituto Nacional de Astrofisica, Optica y Electronica, Luis Enrique Erro No. 1, Tonantzintla, Puebla 72840 (Mexico); Trevino-Palacios, C.G. [Instituto Nacional de Astrofisica, Optica y Electronica, Luis Enrique Erro No. 1, Tonantzintla, Puebla 72840 (Mexico); Rojas-Lopez, M.; Delgado-Macuil, R.; Gayou, V.L. [Centro de Investigacion en Biotecnologia Aplicada (CIBA), IPN, Tlaxcala, Tlax. 72197 (Mexico); Torres-Jacome, A. [Instituto Nacional de Astrofisica, Optica y Electronica, Luis Enrique Erro No. 1, Tonantzintla, Puebla 72840 (Mexico)

    2010-10-25

    Hydrogenated amorphous silicon (a-Si:H) has found applications in flat panel displays, photovoltaic solar cell and recently has been employed in boron doped microbolometer array. We have performed electrical and structural characterizations of a-Si:H layers prepared by plasma enhanced chemical vapor deposition (PECVD) method at 540 K on glass substrates at different diborane (B{sub 2}H{sub 6}) flow ratios (500, 250, 150 and 50 sccm). Fourier transform infrared spectroscopy (FTIR) measurements obtained by specular reflectance sampling mode, show Si-Si, B-O, Si-H, and Si-O vibrational modes (611, 1300, 2100 and 1100 cm{sup -1} respectively) with different strengths which are associated to hydrogen and boron content. The current-voltage curves show that at 250 sccm flow of boron the material shows the lowest resistivity, but for the 150 sccm boron flow it is obtained the highest temperature coefficient of resistance (TCR).

  3. Post-synthesis amine borane functionalization of metal-organic framework and its unusual chemical hydrogen release phenomenon

    KAUST Repository

    Berke, Heinz

    2017-05-11

    We report a novel strategy for post-synthesis amine borane functionalization of MOFs under gas-solid phase transformation utilizing gaseous diborane. The covalently confined amine borane derivative decorated on the framework backbone is stable when preserved at low temperature, but spontaneously liberates soft chemical hydrogen at room temperature leading to the development of an unusual borenium type species (-NH=BH2+) ion-paired with hydroborate anion. Furthermore, the unsaturated amino borane (-NH=BH2) and the -iminodiborane ((--NHB2H5) were detected as final products. A combination of DFT based molecular dynamics simulations and solid state NMR spectroscopy, utilizing isotopically enriched materials, were undertaken to unequivocally elucidate the mechanistic pathways for H2 liberation.

  4. Magnesium silicide production and silane synthesis on its basis

    International Nuclear Information System (INIS)

    Taurbaev, T.I.; Mukashev, F.A.; Manakov, S.M.; Francev, U.V.; Kalblanbekov, B.M.; Akhter, P.; Abbas, M.; Hussain, A.

    2003-01-01

    We had developed an alternative method of production of magnesium silicide with use of ferroalloys of silicon. Magnesium silicide is raw material for silane synthesis. The essence of the method consist of sintering FS -75 (ferrosilicium with 75 % of silicon and 25 % of iron, made by ferroalloy factories) with metal magnesium at temperature of 650 deg. C. The X-ray analysis has shown formation of magnesium silicide. That is further used for synthesis of silane. The output of silane is 60 % in respect of the contents of silicon. After removing the water vapors the mass-spectrometer analysis has estimated the purity of silane as 99.95 % with no detection of phosphine and diborane. (author)

  5. Plasma-wall interactions in RFX

    International Nuclear Information System (INIS)

    Valisa, M.; Bartiromo, R.; Carraro, L.

    1999-01-01

    Plasma wall interactions become a crucial issue in the Reversed Field Pinch RFX at high current (>0.7 MA). Wall-Mode Locking (WML) leads to carbon bloom, enhanced recycling and makes the density control very difficult to achieve. Several wall conditioning techniques have improved the capability of controlling recycling, especially boronization with diborane, but at 1 MA of plasma current removal of the WML becomes mandatory. Encouraging results have been achieved by rotating an externally induced perturbation that can unlock the WML. The strong impurity screening mechanism found at intermediate current does not degrade significantly at 1 MA. Modification of the tiles geometry could further reduce the power density dissipation and mitigate the PWI. (author)

  6. Plasma-wall interactions in RFX

    International Nuclear Information System (INIS)

    Valisa, M.; Bartiromo, R.; Carraro, L.

    2001-01-01

    Plasma wall interactions become a crucial issue in the Reversed Field Pinch RFX at high current (>0.7 MA). Wall-Mode Locking (WML) leads to carbon bloom, enhanced recycling and makes the density control very difficult to achieve. Several wall conditioning techniques have improved the capability of controlling recycling, especially boronisation with diborane, but at 1 MA of plasma current removal of the WML becomes mandatory. Encouraging results have been achieved by rotating an externally induced perturbation that can unlock the WML. The strong impurity screening mechanism found at intermediate current does not degrade significantly at 1 MA. Modification of the tiles geometry could further reduce the power density dissipation and mitigate the PWI. (author)

  7. Control of discharge conditions to reduce hydrogen content in low Z films produced with DC glow

    International Nuclear Information System (INIS)

    Natsir, M.; Sagara, A.; Tsuzuki, K.; Tsuchiya, B.; Hasegawa, Y.; Motojima, O.

    1995-09-01

    Boronization at near room temperature has been performed in plasma processing teststand (PPT) by using a 5 % diborane gases B 2 H 6 in He on electrically floating or unfloating Al samples under various conditions on DC glow discharge power or total gas pressure. The hydrogen concentration was analyzed by using elastic recoil detection method (ERD) and a new modified normalizing technique with Rutherford back scattering (RBS). Results showed that a high growth rate of film formation and floating surface were effective in reducing hydrogen concentration in B films. This result was in good agreement with earlier measurements of H with flash filament (FF) desorption method. In particular the H/B ratio was reduced by decreasing ions but increasing radicals for B film formation. (author)

  8. Optimization of transparent and reflecting electrodes for amorphous silicon solar cells. Annual subcontract report, 1 May 1991--30 April 1992

    Energy Technology Data Exchange (ETDEWEB)

    Gordon, R.G. [Harvard Univ., Cambridge, MA (United States). Dept. of Chemistry

    1993-04-01

    This report describes work to improve the performance of solar cells by improving the electrical and optical properties of their transparent conducting oxides (TCO) layers. Boron-doped zinc-oxide films were deposited by atmospheric pressure chemical vapor deposition in a laminar-flow reactor from diethyl zinc, tert-butanol, and diborane in the temperature range between 300{degrees}C and 420{degrees}C. When the deposition temperature was above 320{degrees}C, both doped and undoped films have highly oriented crystallites with their c-axes perpendicular to the substrate plane. Films deposited from 0.07% diethyl zinc and 2.4% tert-butanol have electron densities between 3.5 {times} 10{sup 20} cm{sup {minus}3} and 5.5 {times} 10{sup 20} cm{sup {minus}3}, conductivities between 250 {Omega}{sup {minus}1} and 2500 {Omega}{sup {minus}1} and mobilities between 2.5 cm{sup 2}/V-s and 35.0 cm{sup 2}/V-s, depending on dopant concentration, film thickness, and deposition temperature. Optical measurements show that the maximum infrared reflectance of the doped films is close to 90%, compared to about 20% for undoped films. Film visible absorption and film conductivity were found to increase with film thickness. The ratio of conductivity to visible absorption coefficient for doped films was between 0.1 {Omega} and 1.1 {Omega}{sup {minus}1}. The band gap of the film changes from 3.3 eV to 3.7 eV when the film is doped with 0.012% diborane.

  9. Mg{sub x}Mn{sub (1-x)}(BH{sub 4}){sub 2} (x = 0-0.8), a cation solid solution in a bimetallic borohydride

    Energy Technology Data Exchange (ETDEWEB)

    Cerny, Radovan, E-mail: radovan.cerny@unige.ch [Laboratory of Crystallography, University of Geneva, 1211 Geneva (Switzerland); Penin, Nicolas [Laboratory of Crystallography, University of Geneva, 1211 Geneva (Switzerland); CNRS, Universite de Bordeaux 1, ICMCB, 87 Avenue du Docteur Albert Schweitzer, F-33608 Pessac Cedex (France); D' Anna, Vincenza; Hagemann, Hans [Department of Physical Chemistry, University of Geneva, 1211 Geneva (Switzerland); Durand, Etienne [CNRS, Universite de Bordeaux 1, ICMCB, 87 Avenue du Docteur Albert Schweitzer, F-33608 Pessac Cedex (France); Ruzicka, Jakub [Charles University, Faculty of Science, Department of Inorganic Chemistry, Hlavova 2030, 128 40, Prague 2 (Czech Republic)

    2011-08-15

    Highlights: {yields} The magnesium and manganese borohydrides form a solid solution Mg{sub x}Mn{sub (1-x)}(BH{sub 4}){sub 2} (x = 0-0.8) which conserves the trigonal structure of Mn{sub (}(BH{sub 4}){sub 2}. {yields} Coexistence of both trigonal and hexagonal borohydrides occurs within nominal composition ranging from x{sub Mg} = 0.8-0.9. {yields} The decomposition temperature of trigonal Mg{sub x}Mn{sub (1-x)}(BH{sub 4}){sub 2} (x = 0-0.8) does not vary significantly with magnesium content (433-453 K). {yields} The desorbed gas contains mostly hydrogen and 3-7.5 mol.% of diborane B{sub 2}H{sub 6}. - Abstract: A solid solution of magnesium and manganese borohydrides was studied by in situ synchrotron radiation X-ray powder diffraction and infrared spectroscopy. A combination of thermogravimetry, mass and infrared spectroscopy, and atomic emission spectroscopy were applied to clarify the thermal gas desorption of pure Mn(BH{sub 4}){sub 2} and a solid solution of composition Mg{sub 0.5}Mn{sub 0.5}(BH{sub 4}){sub 2}. Mg{sub x}Mn{sub (1-x)}(BH{sub 4}){sub 2} (x = 0-0.8) conserves the trigonal structure of Mn(BH{sub 4}){sub 2} at room temperature. Manganese is dissolved in the hexagonal structure of {alpha}-Mg(BH{sub 4}){sub 2}, with the upper solubility limit not exceeding 10 mol.% at room temperature. There exists a two-phase region of trigonal and hexagonal borohydrides within the compositional range x = 0.8-0.9 at room temperature. Infrared spectra show splitting of various vibrational modes, indicating the presence of two cations in the trigonal Mg{sub x}Mn{sub (1-x)}(BH{sub 4}){sub 2} solid solutions, as well as the appearance of a second phase, hexagonal {alpha}-Mg(BH{sub 4}){sub 2}, at higher magnesium contents. All vibrational frequencies are shifted to higher values with increasing magnesium content. The decomposition temperature of the trigonal Mg{sub x}Mn{sub (1-x)}(BH{sub 4}){sub 2} (x = 0-0.8) does not vary significantly as a function of the magnesium

  10. Study on the bound water of several high specific surface-area oxides (beryllia, alumina, silica-alumina); Etude de l'eau de constitution de plusieurs oxydes a grande surface specifique (glucine, alumine, silice-alumine)

    Energy Technology Data Exchange (ETDEWEB)

    Rouquerol, J. [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1964-11-01

    This study is concerned with the bound water of several oxides (beryllia, alumina, silica-alumina) at different steps of their dehydration (heating temperatures between 150 and 1100 deg. C). The following techniques have been used simultaneously: Thermal analysis (a new method has been developed), nitrogen adsorption (study of the texture), Diborane hydrolysis (qualitative and quantitative analysis of surface water), Infra-red spectrography (in the absorption range of water), Nuclear magnetic resonance (in the resonance range of protons). Thanks to these different techniques, five kinds of bound water have been observed. Attention is called on the great influence of the thermal treatment conditions on the evolution of the products resulting from the decomposition of alumina {alpha}-trihydrate Al(OH){sub 3} and beryllium {alpha}-hydroxide, in the course of the dehydration. Moreover, the author emphasizes the peculiar properties of the two kinds of oxides (alumina and beryllia) prepared through a new method of treatment under low pressure and constant speed of decomposition. Such particular features concern mainly texture, bound water, and consequently, also catalytic activity. (author) [French] Ce travail porte sur l'eau de constitution de plusieurs oxydes (glucine, alumine, silice-alumine) aux differents degres de leur deshydratation (temperatures de traitement comprises entre 150 et 1100 deg. C). Cette etude met simultanement en oeuvre: l'analyse thermique (proposition d'une nouvelle methode), l'adsorption d'azote (etude de texture), l'hydrolyse du diborane (analyse qualitative et quantitative de l'eau de surface), la spectrographie infra-rouge (dans le domaine d'absorption de l'eau), la resonance magnetique nucleaire (dans le domaine de resonance des protons). A l'aide de ces differentes techniques, cinq formes d'eau de constitution ont ete observees. L'attention est attiree sur la tres grande influence

  11. Study on the bound water of several high specific surface-area oxides (beryllia, alumina, silica-alumina); Etude de l'eau de constitution de plusieurs oxydes a grande surface specifique (glucine, alumine, silice-alumine)

    Energy Technology Data Exchange (ETDEWEB)

    Rouquerol, J [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1964-11-01

    This study is concerned with the bound water of several oxides (beryllia, alumina, silica-alumina) at different steps of their dehydration (heating temperatures between 150 and 1100 deg. C). The following techniques have been used simultaneously: Thermal analysis (a new method has been developed), nitrogen adsorption (study of the texture), Diborane hydrolysis (qualitative and quantitative analysis of surface water), Infra-red spectrography (in the absorption range of water), Nuclear magnetic resonance (in the resonance range of protons). Thanks to these different techniques, five kinds of bound water have been observed. Attention is called on the great influence of the thermal treatment conditions on the evolution of the products resulting from the decomposition of alumina {alpha}-trihydrate Al(OH){sub 3} and beryllium {alpha}-hydroxide, in the course of the dehydration. Moreover, the author emphasizes the peculiar properties of the two kinds of oxides (alumina and beryllia) prepared through a new method of treatment under low pressure and constant speed of decomposition. Such particular features concern mainly texture, bound water, and consequently, also catalytic activity. (author) [French] Ce travail porte sur l'eau de constitution de plusieurs oxydes (glucine, alumine, silice-alumine) aux differents degres de leur deshydratation (temperatures de traitement comprises entre 150 et 1100 deg. C). Cette etude met simultanement en oeuvre: l'analyse thermique (proposition d'une nouvelle methode), l'adsorption d'azote (etude de texture), l'hydrolyse du diborane (analyse qualitative et quantitative de l'eau de surface), la spectrographie infra-rouge (dans le domaine d'absorption de l'eau), la resonance magnetique nucleaire (dans le domaine de resonance des protons). A l'aide de ces differentes techniques, cinq formes d'eau de constitution ont ete observees. L'attention est attiree sur la tres grande influence des conditions de traitement thermique sur l'evolution des

  12. Contribution to the study of the structure and properties of silica gel (1962); Contribution a l'etude de la structure et des proprietes des gels de silice (1962)

    Energy Technology Data Exchange (ETDEWEB)

    Fraissard, J [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1961-04-15

    The study of the texture of two types of silica gels, xerogels and aerogels, shows that the latter evolve differently on heating. By I.R. spectrography it has been possible to establish that this is due to the existence, in these solids, of a microstructure undetectable by X-rays and which depends on the preparation conditions initially. By using both chemical (thermogravimetry, hydrolysis of diborane) and physical (I.R. spectrography and wide-band N.M.R.) methods we have been able to determine the state of the water of constitution of these gels (water molecules and hydroxyls) and to show that the density, the distribution and the mobility of the protons of this water are very different. For example, the relaxation time T{sub 1} of the protons of a xerogel is about 1 second whilst that of the protons in an aerogel is of the order of a microsecond. Finally, it has been possible by using high resolution N.M.R. to propose a mechanism for the adsorption of formic acid on two types of gel thereby explaining, with the help of previous results, the differences in specificity of these two solids in the decomposition reaction of this acid. (author) [French] L'etude de la texture de deux types de gels de silice, les xerogels et les aerogels, montre que ceux-ci evoluent differemment en fonction de la temperature. La spectrographie I.R a permis de preciser que ceci est du a l'existence, dans ces solides, d'une microstructure indecelable aux rayons X, et fonction des conditions initiales de preparation. Par des methodes chimiques (thermogravimetrie, hydrolyse du diborane) et physiques (spectrographie I.R et R.M.N. large bande), nous avons pu determiner l'etat de l'eau de constitution de ces gels (molecules d'eau et hydroxyles) et montrer que la densite, la repartition et la mobilite des protons de cette eau sont tres differentes. Ainsi le temps de relaxation T{sub 1} des protons d'un xerogel est de l'ordre de la seconde, celui des protons d'un aerogel de l'ordre de la

  13. Discharge cleaning on TFTR after boronization

    International Nuclear Information System (INIS)

    Mueller, D.; Dylla, H.F.; LaMarche, P.H.; Bell, M.G.; Blanchard, W.; Bush, C.E.; Gentile, C.; Hawryluk, R.J.; HIll, K.W.; Janos, A.C.; Jobes, F.C; Owens, D.K.; Pearson, G.; Schivell, J.; Ulrickson, M.A.; Vannoy, C.; Wong, K.L.

    1991-05-01

    At the beginning of the 1990 TFTR experimental run, after replacement of POCO-AXF-5Q graphite tiles on the midplane of the bumper limiter by carbon fiber composite (CFC) tiles and prior to any Pulse Discharge Cleaning (PDC), boronization was performed. Boronization is the deposition of a layer of boron and carbon on the vacuum vessel inner surface by a glow discharge in a diborane, methane and helium mixture. The amount of discharge cleaning required after boronization was substantially reduced compared to that which was needed after previous openings when boronization was not done. Previously, after a major shutdown, about 10 5 low current (∼20 kA) Taylor Discharge Cleaning (TDC) pulses were required before high current (∼400 kA) aggressive Pulse Discharge Cleaning (PDC) pulses could be performed successfully. Aggressive PDC is used to heat the limiters from the vessel bakeout temperature of 150 degrees C to 250 degrees C for a period of several hours. Heating the limiters is important to increase the rate at which water is removed from the carbon limiter tiles. After boronization, the number of required TDC pulses was reduced to <5000. The number of aggressive PDC pulses required was approximately unchanged. 14 refs., 1 tab

  14. Achievement report for fiscal 1981 on Sunshine Program research and development of photovoltaic power systems. Research and development of amorphous solar cells (Research on amorphous silicon defect density); 1981 nendo taiyoko hatsuden system no kenkyu kaihatsu seika hokokusho. Amorphous taiyo denchi no kenkyu kaihatsu (Amorphous silicon no kekkan mitsudo no kenkyu)

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1982-03-01

    So as to determine the energy distribution of defect level density in a-Si, which is indispensable for an optimum solar cell design, the hitherto unclear theoretical relationship between the field effect method and MOS (metal oxide semiconductor) capacity method is made clear, and a unified theory is newly established. A high-speed totally automatic evaluation system is developed, capable of high-accuracy determination of defect levels. For the realization of an a-Si MOS structure required for fulfilling the above purpose, a-Si is grown and then diborane and ammonia are subjected to a glow discharge decomposition process for the formation of a new insulation film. It is found that the material may be utilized for MOS structure construction for defect density evaluation. Studies are conducted on plasma emission spectroscopy and infrared absorption analysis for the elucidation of growth mechanism for the growth of high-quality a-Si. Key radicals in plasma that govern film growth are investigated. It is disclosed that excited hydrogen in plasma plays an important part in microcrystalline phase deposition. It is also disclosed that hydrogenation greatly improves on CVD (chemical vapor deposition) a-Si doping efficiency. (NEDO)

  15. Boronic, diboronic, and α-amino-boronic acids derived from 1-ethynyl-3, 4-dimethoxybenzene

    International Nuclear Information System (INIS)

    Nakagawa, Toshio; Mishima, Yutaka

    1985-01-01

    This work was undertaken with the intention of synthesizing (α-amino-β-(3, 4-dihydroxyphenyl) ethylboronic acid. Unfortunately, the goal could not be attained since the isolation of the target compound could not be achieved though some information suggested its existence in the final product. The methods of synthesis used in the second half of the attempted preparation are described here (compounds in the first half have been published elsewhere). In this procedure, (β-(3, 4-dimethoxyphenyl)) ethenylboronic acid is esterified and azeotropic distillation is conducted to provide diethyl (β-(3, 4-dimethoxyphenyl)) ethenylboronate. This compound is dissolved in diglyme and diborane gas is introduced. The hydroboration product is then subjected to amination with hydroxylamine-0-sulfonic acid. (β-(3, 4-dimethoxyphenyl)) ethyl-α, α-diboronic acid is obtained from the residue of acetone extraction. The acetone extract is concentrated to a solid caramel, from which (α-borono-β-(3, 4-dimethoxyphenyl)) ethylammonium tetraphenylborate is formed. Conversion from the tetraphenylborate salt to (α-amino-β-(3, 4-dimethoxyphenyl)) ethylboronic acid hydrochloride is attempted by the double decomposition RH BPh 4 + CsCl -- RH Cl + CsBPh 4 . The product is subjected to demethylation and treated with sodium tetraphenylborate to precipitate (α-borono-β-(3, 4-dihydroxyphenyl)) ethylammonium tetraphenylborate. Conversion of this to the target compound is tried by double decomposition. (Nogami, K.)

  16. Fluorine and boron co-doped diamond-like carbon films deposited by pulsed glow discharge plasma immersion ion processing

    CERN Document Server

    He, X M; Peters, A M; Taylor, B; Nastasi, M

    2002-01-01

    Fluorine (F) and boron (B) co-doped diamond-like carbon (FB-DLC) films were prepared on different substrates by the plasma immersion ion processing (PIIP) technique. A pulse glow discharge plasma was used for the PIIP deposition and was produced at a pressure of 1.33 Pa from acetylene (C sub 2 H sub 2), diborane (B sub 2 H sub 6), and hexafluoroethane (C sub 2 F sub 6) gas. Films of FB-DLC were deposited with different chemical compositions by varying the flow ratios of the C sub 2 H sub 2 , B sub 2 H sub 6 , and C sub 2 F sub 6 source gases. The incorporation of B sub 2 H sub 6 and C sub 2 F sub 6 into PIIP deposited DLC resulted in the formation of F-C and B-C hybridized bonding structures. The levels of the F and B concentrations effected the chemical bonding and the physical properties as was evident from the changes observed in density, hardness, stress, friction coefficient, and contact angle of water on films. Compared to B-doped or F-doped DLC films, the F and B co-doping of DLC during PIIP deposition...

  17. Boron-doped zinc oxide thin films for large-area solar cells grown by metal organic chemical vapor deposition

    International Nuclear Information System (INIS)

    Chen, X.L.; Xu, B.H.; Xue, J.M.; Zhao, Y.; Wei, C.C.; Sun, J.; Wang, Y.; Zhang, X.D.; Geng, X.H.

    2007-01-01

    Boron-doped zinc oxide (ZnO:B) films were grown by metal organic chemical vapor deposition using diethylzinc (DEZn), and H 2 O as reactant gases and diborane (B 2 H 6 ) as an n-type dopant gas. The structural, electrical and optical properties of ZnO films doped at different B 2 H 6 flow rates were investigated. X-ray diffraction spectra and scanning electron microscopy images indicate that boron-doping plays an important role on the microstructure of ZnO films, which induced textured morphology. With optimized conditions, low sheet resistance (∼ 30 Ω/□), high transparency (> 85% in the visible light and infrared range) and high mobility (17.8 cm 2 V -1 s -1 ) were obtained for 700-nm ZnO:B films deposited on 20 cm x 20 cm glass substrates at the temperature of 443 K. After long-term exposure in air, the ZnO:B films also showed a better electrical stability than the un-doped samples. With the application of ZnO:B/Al back contacts, the short circuit current density was effectively enhanced by about 3 mA/cm 2 for a small area a-Si:H cell and a high efficiency of 9.1% was obtained for a large-area (20 cm x 20 cm) a-Si solar module

  18. Design and fabrication of a bidimentional microbolometer array for Terahertz detection characterized at different temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Orduna-Diaz, A [CIBA-Tlaxcala, IPN, Tlaxcala, Tlax.(Mexico); Castillo-DomInguez, E; Torres-Jacome, A; De la Hidalga-Wade, F J; Trevino-Palacios, C G, E-mail: abdu@inaoep.mx [Instituto Nacional de Astrofisica, Optica y Electronica, Apdo. Postal 51 y 216, Puebla, Pue. 72000 (Mexico)

    2011-01-01

    We present the design, micromachining and characterization of a bidimentional bolometer array for radiation detection in the 0.7-1.5 THz frequency range. The detector is based on a boron doped amorphous silicon film (a-Si-B:H). The film optimized for sensitivity enhancement was obtained using 500 sccm diborane flow with 95 nm thickness. The sensing layer was deposited using plasma enhanced chemical vapor deposition (PECVD) technique at low frequency on a 0.45 {mu}m thick silicon nitride membrane sustained by a micromachined frame in crystalline silicon. The design consists of four 5x5 bolometer arrays made by conventional lithography. The bolometer active area is 660 {mu}m x 420 {mu}m and the detector will operate as a focal plane array. The current-voltage characteristics present an ohmic behaviour; the temperature coefficient of resistance (TCR) was obtained by measuring the bolometer performance from room temperature down to liquid nitrogen temperature. The responsivity was measured under illumination from a black body radiating at 300, 500, 700, 900 and 1100 deg. C, obtaining a value of R =1.17 x 10{sup -2} A/W with a dark current of 4.43 x 10{sup -9} A

  19. Boron mediation on the growth of Ge quantum dots on Si (1 0 0) by ultra high vacuum chemical vapor deposition system

    International Nuclear Information System (INIS)

    Chen, P.S.; Pei, Z.; Peng, Y.H.; Lee, S.W.; Tsai, M.-J.

    2004-01-01

    Self-assembled Ge quantum dots (QDs) with boron mediation are grown on Si (1 0 0) by an industrial hot wall ultra-high-vacuum chemical vapor deposition (UHV/CVD) system with different growth temperatures and dopant gas flow rates. Diborane (B 2 H 6 ) gas is applied as a surfactant on the Si (1 0 0) prior to the growth of Ge QDs. Small dome and pyramid shaped Ge QDs are observed after boron treatment as compared to the hut shaped Ge cluster without boron pre-treatment at 525 and 550 deg. C. The Ge QDs have a typical base width and height of about 30 and 6 nm, respectively, and the density is about 2.5x10 10 cm -2 for the growth temperature of 525 deg. C. Through weakening the Si-H bond during the epitaxy growth and changing the stress field on the surface of the Si (1 0 0) buffer, boron mediation can modify the growth mode of Ge QDs. When the growth temperature is low (525-550 deg. C), the former factor is dominate, as the growth temperature is raised (600 deg. C), the latter parameter may play an important role on the formation of Ge QDs. Optical transition from Ge QDs is demonstrated from photoluminescence (PL) spectra. Furthermore, multifold Ge/Si layers are also carried out to enhance the PL intensity with first Ge layer treated by B 2 H 6 and avoid the generation of threading dislocations

  20. Study on the bound water of several high specific surface-area oxides (beryllia, alumina, silica-alumina)

    International Nuclear Information System (INIS)

    Rouquerol, J.

    1964-11-01

    This study is concerned with the bound water of several oxides (beryllia, alumina, silica-alumina) at different steps of their dehydration (heating temperatures between 150 and 1100 deg. C). The following techniques have been used simultaneously: Thermal analysis (a new method has been developed), nitrogen adsorption (study of the texture), Diborane hydrolysis (qualitative and quantitative analysis of surface water), Infra-red spectrography (in the absorption range of water), Nuclear magnetic resonance (in the resonance range of protons). Thanks to these different techniques, five kinds of bound water have been observed. Attention is called on the great influence of the thermal treatment conditions on the evolution of the products resulting from the decomposition of alumina α-trihydrate Al(OH) 3 and beryllium α-hydroxide, in the course of the dehydration. Moreover, the author emphasizes the peculiar properties of the two kinds of oxides (alumina and beryllia) prepared through a new method of treatment under low pressure and constant speed of decomposition. Such particular features concern mainly texture, bound water, and consequently, also catalytic activity. (author) [fr

  1. Solid Aluminum Borohydrides for Prospective Hydrogen Storage.

    Science.gov (United States)

    Dovgaliuk, Iurii; Safin, Damir A; Tumanov, Nikolay A; Morelle, Fabrice; Moulai, Adel; Černý, Radovan; Łodziana, Zbigniew; Devillers, Michel; Filinchuk, Yaroslav

    2017-12-08

    Metal borohydrides are intensively researched as high-capacity hydrogen storage materials. Aluminum is a cheap, light, and abundant element and Al 3+ can serve as a template for reversible dehydrogenation. However, Al(BH 4 ) 3 , containing 16.9 wt % of hydrogen, has a low boiling point, is explosive on air and has poor storage stability. A new family of mixed-cation borohydrides M[Al(BH 4 ) 4 ], which are all solid under ambient conditions, show diverse thermal decomposition behaviors: Al(BH 4 ) 3 is released for M=Li + or Na + , whereas heavier derivatives evolve hydrogen and diborane. NH 4 [Al(BH 4 ) 4 ], containing both protic and hydridic hydrogen, has the lowest decomposition temperature of 35 °C and yields Al(BH 4 ) 3 ⋅NHBH and hydrogen. The decomposition temperatures, correlated with the cations' ionic potential, show that M[Al(BH 4 ) 4 ] species are in the most practical stability window. This family of solids, with convenient and versatile properties, puts aluminum borohydride chemistry in the mainstream of hydrogen storage research, for example, for the development of reactive hydride composites with increased hydrogen content. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Textured surface boron-doped ZnO transparent conductive oxides on polyethylene terephthalate substrates for Si-based thin film solar cells

    International Nuclear Information System (INIS)

    Chen Xinliang; Lin Quan; Ni Jian; Zhang Dekun; Sun Jian; Zhao Ying; Geng Xinhua

    2011-01-01

    Textured surface boron-doped zinc oxide (ZnO:B) thin films were directly grown via low pressure metal organic chemical vapor deposition (LP-MOCVD) on polyethylene terephthalate (PET) flexible substrates at low temperatures and high-efficiency flexible polymer silicon (Si) based thin film solar cells were obtained. High purity diethylzinc and water vapors were used as source materials, and diborane was used as an n-type dopant gas. P-i-n silicon layers were fabricated at ∼ 398 K by plasma enhanced chemical vapor deposition. These textured surface ZnO:B thin films on PET substrates (PET/ZnO:B) exhibit rough pyramid-like morphology with high transparencies (T ∼ 80%) and excellent electrical properties (Rs ∼ 10 Ω at d ∼ 1500 nm). Finally, the PET/ZnO:B thin films were applied in flexible p-i-n type silicon thin film solar cells (device structure: PET/ZnO:B/p-i-n a-Si:H/Al) with a high conversion efficiency of 6.32% (short-circuit current density J SC = 10.62 mA/cm 2 , open-circuit voltage V OC = 0.93 V and fill factor = 64%).

  3. Plasma deposition of cubic boron nitride films from non-toxic material at low temperatures

    International Nuclear Information System (INIS)

    Karim, M.Z.; Cameron, D.C.; Murphy, M.J.; Hashmi, M.S.J.

    1991-01-01

    Boron nitride has become the focus of a considerable amount of interest because of its properties which relate closely to those of carbon. In particular, the cubic nitride phase has extreme hardness and very high thermal conductivity similar to the properties of diamond. The conventional methods of synthesis use the highly toxic and inflammable gas diborane (B 2 H 6 ) as the reactant material. A study has been made of the deposition of thin films of boron nitride (BN) using non-toxic material by the plasma-assisted chemical vapour deposition technique. The source material was borane-ammonia (BH 3 -NH 3 ) which is a crystalline solid at room temperature with a high vapour pressure. The BH 3 -NH 3 vapour was decomposed in a 13.56 MHz nitrogen plasma coupled either inductively or capacitively with the system. The composition of the films was assessed by measuring their IR absorption when deposited on silicon and KBr substrates. The hexagonal (graphitic) and cubic (diamond-like) allotropes can be distinguished by their characteristic absorption bands which occur at 1365 and 780 cm -1 (hexagonal) and 1070 cm -1 (cubic). We have deposited BN films consisting of a mixture of hexagonal and cubic phases; the relative content of the cubic phase was found to be directly dependent on r.f. power and substrate bias. (orig.)

  4. Scratch-resistant transparent boron nitride films

    Energy Technology Data Exchange (ETDEWEB)

    Dekempeneer, E.H.A.; Kuypers, S.; Vercammen, K.; Meneve, J.; Smeets, J. [Vlaamse Instelling voor Technologisch Onderzoek (VITO), Mol (Belgium); Gibson, P.N.; Gissler, W. [Joint Research Centre of the Commission of the European Communities, Institute for Advanced Materials, Ispra (Vatican City State, Holy See) (Italy)

    1998-03-01

    Transparent boron nitride (BN) coatings were deposited on glass and Si substrates in a conventional capacitively coupled RF PACVD system starting from diborane (diluted in helium) and nitrogen. By varying the plasma conditions (bias voltage, ion current density), coatings were prepared with hardness values ranging from 2 to 12 GPa (measured with a nano-indenter). Infrared absorption measurements indicated that the BN was of the hexagonal type. A combination of glancing-angle X-ray diffraction measurements and simulations shows that the coatings consist of hexagonal-type BN crystallites with different degrees of disorder (nanocrystalline or turbostratic material). High-resolution transmission electron microscopy analysis revealed the presence of an amorphous interface layer and on top of this interface layer a well-developed fringe pattern characteristic for the basal planes in h-BN. Depending on the plasma process conditions, these fringe patterns showed different degrees of disorder as well as different orientational relationships with respect to the substrate surface. These observations were correlated with the mechanical properties of the films. (orig.) 14 refs.

  5. FY 2000 report on the results of the R and D of 'frontier carbon technology.' R and D of a system to support production of undersea oil; 2000 nendo 'tansokei kokino zairyo gijutsu' no kenkyu kaihatsu seika hokokusho. Kaitei sekiyu seisan shien system kenkyu kaihatsu

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2001-05-01

    This report summarized the results of the FY 2000 R and D of frontier carbon technology (FCT). In Chapter 1, technology of original production of substances, new carbon-base substances such as hetero-diamond and carbon nitride with high-grade and various characteristics are synthesized. And, the following are also established: method to synthesize nanotubes, etc. in quantity, technology to control interatomic bonding, technology to control hetero-element replacement, etc. BCN films were obtained by film formation by changing the gas component ratio of diborane, methane and nitrogen by the electron beam excitation CVD method. The sp{sup 3} bonding control in carbon film was advanced. By reacting benzene with raw materials using nickel phthalocyanine as catalyst, carbon nanotube with a 60nm diameter was obtained. Using ECRCVD device, carbon fiber was synthesized on Si substrate. In Chapter 2, original production process technology of mechanical high function materials, subjects are as follows: composition gradient film forming technology, complicated morphology film formation/micro processing technology, technology to apply carbon-base materials to tribology. The application of the materials to the movable part of various industrial machines is considered by making use of characteristics such as low friction and low abrasion which are expected of amorphous carbon, diamond, carbon nitride, etc. (NEDO)

  6. Diverse roles of hydrogen in rhenium carbonyl chemistry: hydrides, dihydrogen complexes, and a formyl derivative.

    Science.gov (United States)

    Li, Nan; Xie, Yaoming; King, R Bruce; Schaefer, Henry F

    2010-11-04

    Rhenium carbonyl hydride chemistry dates back to the 1959 synthesis of HRe(CO)₅ by Hieber and Braun. The binuclear H₂Re₂(CO)₈ was subsequently synthesized as a stable compound with a central Re₂(μ-H)₂ unit analogous to the B₂(μ-H)₂ unit in diborane. The complete series of HRe(CO)(n) (n = 5, 4, 3) and H₂Re₂(CO)(n) (n = 9, 8, 7, 6) derivatives have now been investigated by density functional theory. In contrast to the corresponding manganese derivatives, all of the triplet rhenium structures are found to lie at relatively high energies compared with the corresponding singlet structures consistent with the higher ligand field splitting of rhenium relative to manganese. The lowest energy HRe(CO)₅ structure is the expected octahedral structure. Low-energy structures for HRe(CO)(n) (n = 4, 3) are singlet structures derived from the octahedral HRe(CO)₅ structure by removal of one or two carbonyl groups. For H₂Re₂(CO)₉ a structure HRe₂(CO)₉(μ-H), with one terminal and one bridging hydrogen atom, lies within 3 kcal/mol of the structure Re₂(CO)₉(η²-H₂), similar to that of Re₂(CO)₁₀. For H₂Re₂(CO)(n) (n = 8, 7, 6) the only low-energy structures are doubly bridged singlet Re₂(μ-H)₂(CO)(n) structures. Higher energy dihydrogen complex structures are also found.

  7. Li-Al-borohydride as a potential candidate for on-board hydrogen storage

    Energy Technology Data Exchange (ETDEWEB)

    Lindemann, Inge; Domenech Ferrer, Roger; Dunsch, Lothar; Schultz, Ludwig; Gutfleisch, Oliver [IFW Dresden, PO Box 270016, D-01171 Dresden (Germany); Filinchuk, Yaroslav [Swiss-Norwegian Beam Lines at ESRF, BP-220, 38043 Grenoble (France); Hagemann, Hans; Cerny, Radovan [University of Geneva, Crystallography and Physical Chemistry Department, 1211 Geneva (Switzerland)

    2010-07-01

    Recently, double-cation borohydride systems have attracted great interest. It was found that the desorption temperature of the borohydrides decreases with increasing electronegativity of the cation. Consequently, it is possible to tailor a feasible on-board hydrogen storage material by combination of appropriate cations. Li-Al-borohydride shows a desorption temperature suitable for applications ({approx} 70 C) combined with an high hydrogen density (17.2 wt.%). It was synthesised via high energy ball milling of AlCl{sub 3} and LiBH{sub 4}. The structure of the compound was obtained from high-resolution synchrotron powder diffraction and shows a unique complex structure within the borohydrides. The material was characterized by means of in-situ-Raman, DSC, TG and thermal desorption measurements to study its decomposition pathway. The desorption at {approx} 70 C results in the formation of LiBH{sub 4} while the high mass loss of about 20% points to the release of not only hydrogen but also diborane. This is right now the main drawback for applications because it hinders reversibility.

  8. FY 2000 report on the results of the R and D of 'frontier carbon technology.' R and D of a system to support production of undersea oil; 2000 nendo 'tansokei kokino zairyo gijutsu' no kenkyu kaihatsu seika hokokusho. Kaitei sekiyu seisan shien system kenkyu kaihatsu

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2001-05-01

    This report summarized the results of the FY 2000 R and D of frontier carbon technology (FCT). In Chapter 1, technology of original production of substances, new carbon-base substances such as hetero-diamond and carbon nitride with high-grade and various characteristics are synthesized. And, the following are also established: method to synthesize nanotubes, etc. in quantity, technology to control interatomic bonding, technology to control hetero-element replacement, etc. BCN films were obtained by film formation by changing the gas component ratio of diborane, methane and nitrogen by the electron beam excitation CVD method. The sp{sup 3} bonding control in carbon film was advanced. By reacting benzene with raw materials using nickel phthalocyanine as catalyst, carbon nanotube with a 60nm diameter was obtained. Using ECRCVD device, carbon fiber was synthesized on Si substrate. In Chapter 2, original production process technology of mechanical high function materials, subjects are as follows: composition gradient film forming technology, complicated morphology film formation/micro processing technology, technology to apply carbon-base materials to tribology. The application of the materials to the movable part of various industrial machines is considered by making use of characteristics such as low friction and low abrasion which are expected of amorphous carbon, diamond, carbon nitride, etc. (NEDO)

  9. Atomic-level spatial distributions of dopants on silicon surfaces: toward a microscopic understanding of surface chemical reactivity

    Science.gov (United States)

    Hamers, Robert J.; Wang, Yajun; Shan, Jun

    1996-11-01

    We have investigated the interaction of phosphine (PH 3) and diborane (B 2H 6) with the Si(001) surface using scanning tunneling microscopy, infrared spectroscopy, and ab initio molecular orbital calculations. Experiment and theory show that the formation of PSi heterodimers is energetically favorable compared with formation of PP dimers. The stability of the heterodimers arises from a large strain energy associated with formation of PP dimers. At moderate P coverages, the formation of PSi heterodimers leaves the surface with few locations where there are two adjacent reactive sites. This in turn modifies the chemical reactivity toward species such as PH 3, which require only one site to adsorb but require two adjacent sites to dissociate. Boron on Si(001) strongly segregates into localized regions of high boron concentration, separated by large regions of clean Si. This leads to a spatially-modulated chemical reactivity which during subsequent growth by chemical vapor deposition (CVD) leads to formation of a rough surface. The implications of the atomic-level spatial distribution of dopants on the rates and mechanisms of CVD growth processes are discussed.

  10. Chemical and Electronic Structure Studies of Refractory and Dielectric Thin Films.

    Science.gov (United States)

    Corneille, Jason Stephen

    1300 K yielded a stoichiometric film of rm SiO_2. The suboxides are believed to further react with oxygen forming rm SiO_2 at an elevated temperature. The growth of thin metallic iron films on Mo(100) was characterized as a preliminary study to the synthesis of iron oxides. By varying the substrate temperature during either the post or in-situ oxidation process, oxide films consisting of virtually pure phases of rm Fe_2O_3 and FeO can be successfully obtained as well as intermediate phases including rm Fe_3O_4. In addition, fairly discrete phase changes were found corresponding to the thermally induced reduction of the higher oxides. The adsorption of diborane on clean Ru(0001) and on surfaces precovered by ammonia was studied to lay the groundwork for the synthesis of boron nitride thin films. Boron -nitrogen adlayers were formed by exposing B/Ru(0001) surfaces to 5-10 Torr of ammonia or by coadsorbing ammonia and diborane at 90K with subsequent annealing to 600K. The adlayers formed were rich in boron and decomposed at temperatures well above 1100K. Finally, the adsorption and pyrolysis of tetrakis -(dimethylamido)-titanium (TDMAT) on several metal surfaces was studied as a precursor to the synthesis of titanium nitride thin films. TDMAT was found to decompose readily above {~}{480K} on metallic substrates, producing films with high carbon content. However, in the presence of ammonia, well below the threshold of gas-phase reaction ({< }{10^{-4}} Torr), the growth of low carbon-content titanium nitride films proceeds readily, via surface mediated reaction(s) of TDMAT and ammonia between 550-750K. The effects of surface temperature and reagent pressures are reported and discussed.

  11. Research on ZnO/Si heterojunction solar cells

    Science.gov (United States)

    Chen, Li; Chen, Xinliang; Liu, Yiming; Zhao, Ying; Zhang, Xiaodan

    2017-06-01

    We put forward an n-ZnO/p-Si heterojunction solar cell model based on AFORS-HET simulations and provide experimental support in this article. ZnO:B (B-doped ZnO) thin films deposited by metal-organic chemical vapor deposition (MOCVD) are planned to act as electrical emitter layer on p-type c-Si substrate for photovoltaic applications. We investigate the effects of thickness, buffer layer, ZnO:B affinity and work function of electrodes on performances of solar cells through computer simulations using AFORS-HET software package. The energy conversion efficiency of the ZnO:B(n)/ZnO/c-Si(p) solar cell can achieve 17.16% ({V}{oc}: 675.8 mV, {J}{sc}: 30.24 mA/cm2, FF: 83.96%) via simulation. On a basis of optimized conditions in simulation, we carry out some experiments, which testify that the ZnO buffer layer of 20 nm contributes to improving performances of solar cells. The influences of growth temperature, thickness and diborane (B2H6) flow rates are also discussed. We achieve an appropriate condition for the fabrication of the solar cells using the MOCVD technique. The obtained conversion efficiency reaches 2.82% ({V}{oc}: 294.4 mV, {J}{sc}: 26.108 mA/cm2, FF: 36.66%). Project supported by the State Key Development Program for Basic Research of China (Nos. 2011CBA00706, 2011CBA00707), the Tianjin Applied Basic Research Project and Cutting-Edge Technology Research Plan (No. 13JCZDJC26900), the Tianjin Major Science and Technology Support Project (No. 11TXSYGX22100), the National High Technology Research and Development Program of China (No. 2013AA050302), and the Fundamental Research Funds for the Central Universities (No. 65010341).

  12. Investigation of the toroidal dependence of first wall conditions in the Large Helical Device

    International Nuclear Information System (INIS)

    Hino, T.; Ashikawa, N.; Masuzaki, S.; Sagara, A.; Komori, A.; Yamauchi, Y.; Nobuta, Y.; Matsunaga, Y.

    2010-11-01

    The non-uniform wall conditions such as the fuel hydrogen retention and the erosion/deposition have been investigated in the Large Helical Device (LHD) by using toroidally and poloidally distributed material probes. They were installed in every experimental campaign from 2003 to 2010, and the evolutions of the wall conditions were clearly obtained. The wall conditions significantly depended on the operational procedures and the positions of in-vessel devices such as anodes for glow discharge and the ICRF antennas. The toroidal profiles for the amounts of retained hydrogen and helium, and the depth of wall erosion, were systematically measured. The hydrogen, helium and neon glow discharges have been conducted by using two anodes before and after the hydrogen or helium main discharges. The amount of retained hydrogen was large in the vicinity of the anodes, and drastically decreased as increase of the campaign number. This reduction well corresponds to the time period used for the hydrogen glow discharge conditioning. The erosion depth was large at the walls relatively close to the anodes, which is owing to the sputtering during the helium and neon glow discharges. The depositions of carbon and boron also depended on the positions of NBI and diborane gas inlet used for boronization, respectively. The amount of the retained helium was large at the walls close to the anodes owing to the helium glow discharge. The amount of retained helium became large at the walls close to the ICRF antennas owing to the implantation of high energy helium during the helium main discharge with the ICRF heating. In the present study, the toroidal dependences of the gas retention and the erosion/deposition in LHD were obtained, and the effects of the in-vessel devices on these plasma wall interactions were clarified. (author)

  13. Plasma boriding of a cobalt–chromium alloy as an interlayer for nanostructured diamond growth

    Energy Technology Data Exchange (ETDEWEB)

    Johnston, Jamin M.; Jubinsky, Matthew; Catledge, Shane A., E-mail: catledge@uab.edu

    2015-02-15

    Highlights: • Metal-boride layer creates a compatible surface for NSD deposition. • PECVD boriding on CoCrMo produces robust metal-boride layer. • Deposition temperature comparison shows 750 °C boriding masks surface cobalt. • EDS shows boron diffusion as well as deposition. • Nanoindentation hardness of CoCrMo substantially increases after boriding. - Abstract: Chemical vapor deposited (CVD) diamond coatings can potentially improve the wear resistance of cobalt–chromium medical implant surfaces, but the high cobalt content in these alloys acts as a catalyst to form graphitic carbon. Boriding by high temperature liquid baths and powder packing has been shown to improve CVD diamond compatibility with cobalt alloys. We use the microwave plasma-enhanced (PE) CVD process to deposit interlayers composed primarily of the borides of cobalt and chromium. The use of diborane (B{sub 2}H{sub 6}) in the plasma feedgas allows for the formation of a robust boride interlayer for suppressing graphitic carbon during subsequent CVD of nano-structured diamond (NSD). This metal–boride interlayer is shown to be an effective diffusion barrier against elemental cobalt for improving nucleation and adhesion of NSD coatings on a CoCrMo alloy. Migration of elemental cobalt to the surface of the interlayer is significantly reduced and undetectable on the surface of the subsequently-grown NSD coating. The effects of PECVD boriding are compared for a range of substrate temperatures and deposition times and are evaluated using glancing-angle X-ray diffraction (XRD), cross-sectional scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and micro-Raman spectroscopy. Boriding of CoCrMo results in adhered nanostructured diamond coatings with low surface roughness.

  14. A liquid-based eutectic system: LiBH4·NH 3-nNH3BH3 with high dehydrogenation capacity at moderate temperature

    KAUST Repository

    Tan, Yingbin

    2011-01-01

    A novel eutectic hydrogen storage system, LiBH4·NH 3-nNH3BH3, which exists in a liquid state at room temperature, was synthesized through a simple mixing of LiBH 4·NH3 and NH3BH3 (AB). In the temperature range of 90-110 °C, the eutectic system showed significantly improved dehydrogenation properties compared to the neat AB and LiBH 4·NH3 alone. For example, in the case of the LiBH4·NH3/AB with a mole ratio of 1:3, over 8 wt.% hydrogen could be released at 90 °C within 4 h, while only 5 wt.% hydrogen released from the neat AB at the same conditions. Through a series of experiments it has been demonstrated that the hydrogen release of the new system is resulted from an interaction of AB and the NH3 group in the LiBH4·NH3, in which LiBH4 works as a carrier of ammonia and plays a crucial role in promoting the interaction between the NH3 group and AB. The enhanced dehydrogenation of LiBH 4·NH3/AB may result from the polar liquid state reaction environments and the initially promoted formation of the diammoniate of diborane, which will facilitate the B-H⋯H-N interaction between LiBH4·NH3 and AB. Kinetics analysis revealed that the rate-controlling steps of the dehydrogenation process are three-dimensional diffusion of hydrogen at temperatures ranging from 90 to 110 °C. This journal is © The Royal Society of Chemistry.

  15. Analysis of Gas Membrane Ultra-High Purification of Small Quantities of Mono-Isotopic Silane

    Energy Technology Data Exchange (ETDEWEB)

    de Almeida, Valmor F [ORNL; Hart, Kevin J [ORNL

    2016-09-01

    A small quantity of high-value, crude, mono-isotopic silane is a prospective gas for a small-scale, high-recovery, ultra-high membrane purification process. This is an unusual application of gas membrane separation for which we provide a comprehensive analysis of a simple purification model. The goal is to develop direct analytic expressions for estimating the feasibility and efficiency of the method, and guide process design; this is only possible for binary mixtures of silane in the dilute limit which is a somewhat realistic case. Among the common impurities in crude silane, methane poses a special membrane separation challenge since it is chemically similar to silane. Other potential problematic surprises are: ethylene, diborane and ethane (in this order). Nevertheless, we demonstrate, theoretically, that a carefully designed membrane system may be able to purify mono-isotopic, crude silane to electronics-grade level in a reasonable amount of time and expenses. We advocate a combination of membrane materials that preferentially reject heavy impurities based on mobility selectivity, and light impurities based on solubility selectivity. We provide estimates for the purification of significant contaminants of interest. To improve the separation selectivity, it is advantageous to use a permeate chamber under vacuum, however this also requires greater control of in-leakage of impurities in the system. In this study, we suggest cellulose acetate and polydimethylsiloxane as examples of membrane materials on the basis of limited permeability data found in the open literature. We provide estimates on the membrane area needed and priming volume of the cell enclosure for fabrication purposes when using the suggested membrane materials. These estimates are largely theoretical in view of the absence of reliable experimental data for the permeability of silane. Last but not least, future extension of this work to the non-dilute limit may apply to the recovery of silane from

  16. Ultrathin, wafer-scale hexagonal boron nitride on dielectric surfaces by diffusion and segregation mechanism

    Science.gov (United States)

    Sonde, Sushant; Dolocan, Andrei; Lu, Ning; Corbet, Chris; Kim, Moon J.; Tutuc, Emanuel; Banerjee, Sanjay K.; Colombo, Luigi

    2017-06-01

    Chemical vapor deposition (CVD) of two-dimensional (2D) hexagonal boron nitride (h-BN) is at the center of numerous studies for its applications in novel electronic devices. However, a clear understanding of the growth mechanism is lacking for its wider industrial adoption on technologically relevant substrates such as SiO2. Here, we demonstrate a controllable growth method of thin, wafer scale h-BN films on arbitrary substrates. We also clarify the growth mechanism to be diffusion and surface segregation (D-SS) of boron (B) and nitrogen (N) in Ni and Co thin films on SiO2/Si substrates after exposure to diborane and ammonia precursors at high temperature. The segregation was found to be independent of the cooling rates employed in this report, and to our knowledge has not been found nor reported for 2D h-BN growth so far, and thus provides an important direction for controlled growth of h-BN. This unique segregation behavior is a result of a combined effect of high diffusivity, small film thickness and the inability to achieve extremely high cooling rates in CVD systems. The resulting D-SS h-BN films exhibit excellent electrical insulating behavior with an optical bandgap of about 5.8 eV. Moreover, graphene-on-h-BN field effect transistors using the as-grown D-SS h-BN films show a mobility of about 6000 cm2 V-1 s-1 at room temperature.

  17. Hydrogen diffusion and microstructure in undoped and boron-dope hydrogenated amorphous silicon: An IR and SIMS study

    International Nuclear Information System (INIS)

    Mitra, S.

    1991-01-01

    Hydrogenated amorphous silicon (a-Si:H) prepared by rf sputtering of a polycrystalline Si target at various rf powers 50 ≤ P ≤ 550 W (0.27--2.97 W/cm 2 ), target to substrate distance 1 ≤ d ≤ 2 double-prime, and varying hydrogen partial pressures. Doping was accomplished by introducing diborane (B 2 H 6 ) in the plasma. Hydrogen diffusion was studied from the depth profiles obtained from the SIMS on multilayered a-Si:H/a-Si:(H,D)/a-Si:H samples. The properties of the samples were characterized by IR absorption, optical gap measurements and ESR. IR yielded quantitative and qualitative information total hydrogen content and the nature of the hydrogen bonding, respectively. Hence the hydrogen microstructure of the samples could be varied in a systematic manner and monitored from the hydrogen vibrational modes. The ESR gave information on the number of paramagnetic defects per unit volume in the samples. The IR absorption of both as-deposited and annealed samples were closely monitored and the results clearly demonstrate a strong correlation between hydrogen diffusion and its microstructure. It is shown that microvoids in a-Si:H play a critical role in the process of diffusion by inducing deep hydrogen trapping sites that render them immobile. Consequently, as the microvoid density increases beyond a critical density hydrogen diffusion is totally quenched. The diffusion results are discussed both in the context of multiple trapping transport of hydrogen in an exponential distribution of trapping sites and the floating bond model

  18. Polycrystalline ZnO: B grown by LPCVD as TCO for thin film silicon solar cells

    International Nuclear Information System (INIS)

    Fay, Sylvie; Steinhauser, Jerome; Nicolay, Sylvain; Ballif, Christophe

    2010-01-01

    Conductive zinc oxide (ZnO) grown by low pressure chemical vapor deposition (LPCVD) technique possesses a rough surface that induces an efficient light scattering in thin film silicon (TF Si) solar cells, which makes this TCO an ideal candidate for contacting such devices. IMT-EPFL has developed an in-house LPCVD process for the deposition of nanotextured boron doped ZnO films used as rough TCO for TF Si solar cells. This paper is a general review and synthesis of the study of the electrical, optical and structural properties of the ZnO:B that has been performed at IMT-EPFL. The influence of the free carrier absorption and the grain size on the electrical and optical properties of LPCVD ZnO:B is discussed. Transport mechanisms at grain boundaries are studied. It is seen that high doping of the ZnO grains facilitates the tunnelling of the electrons through potential barriers that are located at the grain boundaries. Therefore, even if these potential barriers increase after an exposition of the film to a humid atmosphere, the heavily doped LPCVD ZnO:B layers show a remarkable stable conductivity. However, the introduction of diborane in the CVD reaction induces also a degradation of the intra-grain mobility and increases over-proportionally the optical absorption of the ZnO:B films. Hence, the necessity to finely tune the doping level of LPCVD ZnO:B films is highlighted. Finally, the next challenges to push further the optimization of LPCVD ZnO:B films for thin film silicon solar cells are discussed, as well as some remarkable record cell results achieved with LPCVD ZnO:B as front electrode.

  19. METHODS FOR THE SAFE STORAGE, HANDLING, AND DISPOSAL OF PYROPHORIC LIQUIDS AND SOLIDS IN THE LABORATORY

    Energy Technology Data Exchange (ETDEWEB)

    Simmons, F.; Kuntamukkula, M.; Alnajjar, M.; Quigley, D.; Freshwater, D.; Bigger, S.

    2010-02-02

    Pyrophoric reagents represent an important class of reactants because they can participate in many different types of reactions. They are very useful in organic synthesis and in industrial applications. The Occupational Safety and Health Administration (OSHA) and the National Fire Protection Association (NFPA) define Pyrophorics as substances that will self-ignite in air at temperatures of 130 F (54.4 C) or less. However, the U.S. Department of Transportation (DOT) uses criteria different from the auto-ignition temperature criterion. The DOT defines a pyrophoric material as a liquid or solid that, even in small quantities and without an external ignition source, can ignite within five minutes after coming in contact with air when tested according to the United Nations Manual of Tests and Criteria. The Environmental Protection Agency has adopted the DOT definition. Regardless of which definition is used, oxidation of the pyrophoric reagents by oxygen or exothermic reactions with moisture in the air (resulting in the generation of a flammable gas such as hydrogen) is so rapid that ignition occurs spontaneously. Due to the inherent nature of pyrophoric substances to ignite spontaneously upon exposure to air, special precautions must be taken to ensure their safe handling and use. Pyrophoric gases (such as diborane, dichloroborane, phosphine, etc.) are typically the easiest class of pyrophoric substances to handle since the gas can be plumbed directly to the application and used remotely. Pyrophoric solids and liquids, however, require the user to physically manipulate them when transferring them from one container to another. Failure to follow proper safety precautions could result in serious injury or unintended consequences to laboratory personnel. Because of this danger, pyrophorics should be handled only by experienced personnel. Users with limited experience must be trained on how to handle pyrophoric reagents and consult with a knowledgeable staff member prior

  20. The synthesis and pharmacological evaluation of (±-2,3-seco-fentanyl analogues

    Directory of Open Access Journals (Sweden)

    LJ. DOSEN-MICOVIC

    2004-11-01

    Full Text Available An efficient, five-step synthetic approach to various acyclic 1,3-diamines has been developed and applied to the preparation of a novel class of open-chained fentanyl analogues. The acyclic derivatives 5.1–5.5 (all new compounds were synthesized with the aim of estimating the significance of the piperidine ring for the opioid analgesic activity of anilido-piperidines. The starting b-keto-amide 1.1, prepared by the aminolysis of methyl acetoacetate with methylphenethylamine, (93 % yield, was successively reacted with NaH and BuLi, to form the highly reactive a,g-dienolate anion 1.1a. Regio and chemoselective g-alkylation of the dienolate with various primary and secondary alkyl halides furnished the b-keto-amides 1.2–1.5 (76–91 %. Reductive amination of the keto-amides 1.1–1.5 with aniline and Zn powder in acetic acid, via the enamine intermediates 2.1–2.5, afforded the b-anilino amides 3.1–3.5 (74–85 %. After reductive deoxygenation of the tertiary amide group, using in situ generated diborane, the corresponding 1,3-diamines 4.1–4.5 were obtained (87–97 %. The synthesis of (±-2,3-seco-fentanyls 5.1–5.5 was completed by N-acylation of the diamines 4.1–4.5 with propionyl chloride, followed by precipitation of the monooxalate salts (86–95 %. The parent compound, 2,3-seco-fentanyl 5.1, was found to be a 40 times less potent narcotic analgesic than fentanyl but still 5–6 times more active than morphine in rats, while i-Pr derivative 5.3 was inactive. Apart from the pharmacological significance, the general procedure described herein may afford various functionalized, 1,3-diamines as potential complexing agents and building blocks for the synthesis of aza-crown ethers.

  1. trans-[Pt(BCat')Me(PCy3)2]: an experimental case study of reductive elimination processes in Pt-Boryls through associative mechanisms.

    Science.gov (United States)

    Braunschweig, Holger; Bertermann, Rüdiger; Brenner, Peter; Burzler, Michael; Dewhurst, Rian D; Radacki, Krzysztof; Seeler, Fabian

    2011-10-10

    A stable trans-(alkyl)(boryl) platinum complex trans-[Pt(BCat')Me(PCy(3))(2)] (Cat'=Cat-4-tBu; Cy=cyclohexyl=C(6)H(11)) was synthesised by salt metathesis reaction of trans-[Pt(BCat')Br(PCy(3))(2)] with LiMe and was fully characterised. Investigation of the reactivity of the title compound showed complete reductive elimination of Cat'BMe at 80 °C within four weeks. This process may be accelerated by the addition of a variety of alkynes, thereby leading to the formation of the corresponding η(2) -alkyne platinum complexes, of which [Pt(η(2)-MeCCMe)(PCy(3))(2)] was characterised by X-ray crystallography. Conversion of the trans-configured title compound to a cis derivative remained unsuccessful due to an instantaneous reductive elimination process during the reaction with chelating phosphines. Treatment of trans-[Pt(BCat')Me(PCy(3))(2)] with Cat(2)B(2) led to the formation of CatBMe and Cat'BMe. In the course of further investigations into this reaction, indications for two indistinguishable reaction mechanisms were found: 1) associative formation of a six-coordinate platinum centre prior to reductive elimination and 2) σ-bond metathesis of B-B and C-Pt bonds. Mechanism 1 provides a straightforward explanation for the formation of both methylboranes. Scrambling of diboranes(4) Cat(2)B(2) and Cat'(2)B(2) in the presence of [Pt(PCy(3))(2)], fully reductive elimination of CatBMe or Cat'BMe from trans-[Pt(BCat')Me(PCy(3))(2)] in the presence of sub-stoichiometric amounts of Cat(2)B(2), and evidence for the reversibility of the oxidative addition of Cat(2)B(2) to [Pt(PCy(3))(2)] all support mechanism 2, which consists of sequential equilibria reactions. Furthermore, the solid-state molecular structure of cis-[Pt(BCat)(2)(PCy(3))(2)] and cis-[Pt(BCat')(2)(PCy(3))(2)] were investigated. The remarkably short B-B separations in both bis(boryl) complexes suggest that the two boryl ligands in each case are more loosely bound to the Pt(II) centre than in related bis

  2. Growth of boron doped hydrogenated nanocrystalline cubic silicon carbide (3C-SiC) films by Hot Wire-CVD

    Energy Technology Data Exchange (ETDEWEB)

    Pawbake, Amit [School of Energy Studies, Savitribai Phule Pune University, Pune 411 007 (India); Tata Institute of Fundamental Research, Colaba, Mumbai 400 005 (India); Mayabadi, Azam; Waykar, Ravindra; Kulkarni, Rupali; Jadhavar, Ashok [School of Energy Studies, Savitribai Phule Pune University, Pune 411 007 (India); Waman, Vaishali [Modern College of Arts, Science and Commerce, Shivajinagar, Pune 411 005 (India); Parmar, Jayesh [Tata Institute of Fundamental Research, Colaba, Mumbai 400 005 (India); Bhattacharyya, Somnath [Department of Metallurgical and Materials Engineering, IIT Madras, Chennai 600 036 (India); Ma, Yuan‐Ron [Department of Physics, National Dong Hwa University, Hualien 97401, Taiwan (China); Devan, Rupesh; Pathan, Habib [Department of Physics, Savitribai Phule Pune University, Pune 411007 (India); Jadkar, Sandesh, E-mail: sandesh@physics.unipune.ac.in [Department of Physics, Savitribai Phule Pune University, Pune 411007 (India)

    2016-04-15

    Highlights: • Boron doped nc-3C-SiC films prepared by HW-CVD using SiH{sub 4}/CH{sub 4}/B{sub 2}H{sub 6}. • 3C-Si-C films have preferred orientation in (1 1 1) direction. • Introduction of boron into SiC matrix retard the crystallanity in the film structure. • Film large number of SiC nanocrystallites embedded in the a-Si matrix. • Band gap values, E{sub Tauc} and E{sub 04} (E{sub 04} > E{sub Tauc}) decreases with increase in B{sub 2}H{sub 6} flow rate. - Abstract: Boron doped nanocrystalline cubic silicon carbide (3C-SiC) films have been prepared by HW-CVD using silane (SiH{sub 4})/methane (CH{sub 4})/diborane (B{sub 2}H{sub 6}) gas mixture. The influence of boron doping on structural, optical, morphological and electrical properties have been investigated. The formation of 3C-SiC films have been confirmed by low angle XRD, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), Fourier transform infra-red (FTIR) spectroscopy and high resolution-transmission electron microscopy (HR-TEM) analysis whereas effective boron doping in nc-3C-SiC have been confirmed by conductivity, charge carrier activation energy, and Hall measurements. Raman spectroscopy and HR-TEM analysis revealed that introduction of boron into the SiC matrix retards the crystallanity in the film structure. The field emission scanning electron microscopy (FE-SEM) and non contact atomic force microscopy (NC-AFM) results signify that 3C-SiC film contain well resolved, large number of silicon carbide (SiC) nanocrystallites embedded in the a-Si matrix having rms surface roughness ∼1.64 nm. Hydrogen content in doped films are found smaller than that of un-doped films. Optical band gap values, E{sub Tauc} and E{sub 04} decreases with increase in B{sub 2}H{sub 6} flow rate.

  3. Efecto de la temperatura de deposición en las características estructurales y ópticas de películas delgadas de nitruro de boro obtenidas por CVD

    Directory of Open Access Journals (Sweden)

    Essafti, A.

    2007-06-01

    Full Text Available Boron nitride (BN thin films were deposited on silicon substrates by thermal CVD using mixtures of ammoniac and diborane. The effect of the deposition temperature (T on the structural and optical characteristics of the BN samples was studied in the temperature range of 500 – 1000 oC. The deposition rate reached its maximum (1600 Å/min at T = 900 oC. The activation energy (Ea of the reaction NH3 + B2H6, determined from the Arrhenius plot, is of 13.6 kcal/mol in the 500 – 900 oC range. The Infrared spectroscopy revealed the existence of different bands corresponding to B-H, N-H and B-N bonds. The concentration of B-H and N-H species is below the detection limit of IR spectroscopy in the BN films deposited at T ≥ 800 oC. The chemical analysis by XPS spectroscopy showed the presence of B-B and B-N bonds. An increase of the deposition temperature lead to a decrease of B-B bonds, which favors the formation of quasi-stoichiometric BN at T = 1000 oC. At this temperature, the resulting BN films are highly transparent with a refractive index of 1.7. The BN films deposited at T ≤ 900 oC are amorphous, nevertheless at T = 1000 oC they are partially crystallized with a turbostratic structure.

    Se depositaron películas de nitruro de boro (BN sobre sustratos de silicio mediante CVD térmico utilizando mezclas de diborano y amoníaco. Se estudió el efecto de la temperatura de deposición (T, en el rango 500 – 1000 oC, sobre las características estructurales y ópticas de las muestras de BN. La velocidad de deposición alcanza su máximo (1600 Å/min a T = 900 oC. La energía de activación (Ea de la reacción NH3 + B2H6, determinada a partir de la representación de Arrhenius, es de 13.6 kcal/mol en el rango 500 – 900 oC. La espectroscopia IR reveló la existencia de diferentes bandas correspondientes a enlaces B‑H, N‑H y B-N. La concentración de especies B-H y N-H está por debajo del nivel de detección mediante IR en las pel

  4. Interface properties of the amorphous silicon/crystalline silicon heterojunction photovoltaic cell

    Science.gov (United States)

    Halliop, Basia

    Amorphous-crystalline silicon (a-Si:H/c-Si) heterojunctions have the potential of being a very high efficiency silicon photovoltaic platform technology with accompanying cost and energy budget reductions. In this research a heterojunction cell structure based on a-Si:H deposited using a DC saddle field plasma enhanced vapour deposition (DCSF PECVD) technique is studied, and the a-Si:H/c-Si and indium tin oxide/a-Si:H interfaces are examined using several characterization methods. Photocarrier radiometry (PCR) is used for the first time to probe the a-Si:H/c-Si junction. PCR is demonstrated as a carrier lifetime measurement technique -- specifically, confirming carrier lifetimes above 1 ms for 1-5 Ocm phosphorous-doped c-Si wafers passivated on both sides with 30 nm of i-a-Si:H. PCR is also used to determine surface recombination velocity and mobility, and to probe recombination at the a-Si:H/c-Si interface, distinguishing interface recombination from recombination within the a-Si:H layer or at the a-Si:H surface. A complementary technique, lateral conductivity is applied over a temperature range of 140 K to 430 K to construct energy band diagrams of a-Si:H/c-Si junctions. Boron doped a-Si:H films on glass are shown to have activation energies of 0.3 to 0.35 eV, tuneable by adjusting the diborane to silane gas ratio during deposition. Heterojunction samples show evidence of a strong hole inversion layer and a valence band offset of approximately 0.4 eV; carrier concentration in the inversion layer is reduced in p-a-Si:H/i-a-Si:H/ c-Si structures as intrinsic layer thickness increases, while carrier lifetime is increased. The indium tin oxide/amorphous silicon interface is also examined. Optimal ITO films were prepared with a sheet resistance of 17.3 O/[special character omitted] and AM1.5 averaged transmittance of 92.1%., for a film thickness of approximately 85 nm, using temperatures below 200°C. Two different heat treatments are found to cause crystallization of

  5. Design and fabrication of a novel self-powered solid-state neutron detector

    Science.gov (United States)

    LiCausi, Nicholas

    key advantages of the novel devices are theoretical neutron detection efficiency of ˜48%, a self-passivating structure that reduces leakage current and detector operation with no bias resulting in extremely low device noise. Processes required to fabricate the 3D type detector were explored and developed in this thesis. The detector capacitance and processing steps have been simulated with MEDICI and TSuprem-4, respectively. Lithography masks were then designed using Cadence. The fabrication process development was conducted in line with standard CMOS grade integrated circuit processing to allow for simple integration with existing fabrication facilities. A number of new processes were developed including the low pressure chemical vapor deposition of conformal boron films using diborane on very high aspect-ratio trenches and holes. Development also included methods for "wet" chemical etching and "dry" reactive ion etching of the deposited boron films. Fabricated detectors were characterized with the transmission line method, 4-point probe, I-V measurements and C-V measurements. Finally the detector response to thermal neutrons was studied. Characterization has shown significant reduction in reverse leakage current density to ˜8x10-8 A/cm2 (nearly 4 orders of magnitude over the previously published data). Results show that the fabrication process developed is capable of producing efficient (˜22.5%) solid-state thermal neutron detectors.

  6. Interlayer utilization (including metal borides) for subsequent deposition of NSD films via microwave plasma CVD on 316 and 440C stainless steels

    Science.gov (United States)

    Ballinger, Jared

    . Surface boriding was implemented using the novel method of microwave plasma CVD with a mixture of hydrogen and diborane gases. On 440C bearings, dual phase boride layers of Fe2B and FeB were formed which supported adhered nanostructured diamond films. Continuity of the films was not seamless with limited regions remaining uncoated potentially corresponding to delamination of the film as evidenced by the presence of tubular structures presumably composed of sp2 bonded carbon. Surface boriding of 316 stainless steel discs was conducted at various powers and pressures to achieve temperatures ranging from 550-800 °C. The substrate boriding temperature was found to substantially influence the resultant interlayer by altering the metal boride(s) present. The lowest temperatures produced an interlayer where CrB was the single detected phase, higher temperatures yielded the presence of only Fe2B, and a combination of the two phases resulted from an intermediate boriding temperature. Compared with the more common, commercialized boriding methods, this a profound result given the problems posed by the FeB phase in addition to other advantages offered by CVD processes and microwave generated plasmas in general. Indentation testing of the boride layers revealed excellent adhesion strength for all borided interlayers, and above all, no evidence of cracking was observed for a sole Fe2B phase. As with boriding of 440C bearings, subsequent diamond deposition was achieved on these interlayers with substantially improved adhesion strength relative to diamond coated TiN interlayers. Both XRD and Raman spectroscopy confirmed a nanostructured diamond film with interfacial chromium carbides responsible for enhanced adhesion strength. Interlayers consisting solely of Fe2B have displayed an ability to support fully continuous nanostructured diamond films, yet additional study is required for consistent reproduction. This is in good agreement with initial work on pack borided high alloy steels

  7. Deposition of thin layers of boron nitrides and hydrogenated microcrystalline silicon assisted by high current direct current arc plasma; Deposition assistee par un plasma a arc a haut courant continu de couches minces de Nitrure de Bore et de Silicium microcristallin hydrogene

    Energy Technology Data Exchange (ETDEWEB)

    Franz, D. [Ecole Polytechnique Federale de Lausanne, Centre de Recherches en Physique des Plasmas (CRPP), CH-1015 Lausanne (Switzerland)

    1999-09-01

    of plasma. Diborane dissociation, the different reactions and new species created in the gas phase, such as aminoborane, containing boron-nitrogen bonds, reveals a rich chemistry in the plasma phase. A large amount of atomic hydrogen is necessary to deposit hydrogenated microcrystalline silicon coatings. The study of HCDCA regarding the deposition of diamond has shown that this arc efficiently dissociates molecular hydrogen by way of intermediate vibrationally excited states. This efficient dissociation has allowed the fast deposition (up to 0.6 microns per minute) of highly crystalline silicon films, even without any addition of molecular hydrogen, where the atomic hydrogen was created by the molecular dissociation of silane (SiH{sub 4}). The nature of the deposition precursors is highly dependent on the magnetic field used to confine the arc. At low field, the deposition of hydrogenated silicon radicals created in the plasma leads to columnar growth, whereas with an increase of the magnetic field, the film growth is probably dominated by the deposition of crystallites created in the plasma phase, whose size increases with the field. Moreover, a strong dependence of the film morphology on the deposition parameters has been observed, in particular, regarding the substrate temperature, the hydrogen dilution and the magnetic field. This new deposition technique of hydrogenated microcrystalline silicon is promising for industrial applications. (author)

  8. Final Report: DE- FC36-05GO15063, Fundamental Studies of Advanced High-Capacity, Reversible Metal Hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Jensen, Craig [Univ. of Hawaii, Honolulu, HI (United States); McGrady, Sean [Univ. of New Brunswick, Fredericton NB (Canada); Severa, Godwin [Univ. of Hawaii, Honolulu, HI (United States); Eliseo, Jennifer [Univ. of Hawaii, Honolulu, HI (United States); Chong, Marina [Univ. of Hawaii, Honolulu, HI (United States)

    2013-05-31

    The project was component of the US DOE, Metal Hydride Center of Excellence (MHCoE). The Sandia National Laboratory led center was established to conduct highly collaborative and multi-disciplinary applied R&D to develop new reversible hydrogen storage materials that meet or exceed DOE/FreedomCAR 2010 and 2015 system targets for hydrogen storage materials. Our approach entailed a wide variety of activities ranging from synthesis, characterization, and evaluation of new candidate hydrogen storage materials; screening of catalysts for high capacity materials requiring kinetics enhancement; development of low temperature methods for nano-confinement of hydrides and determining its effects on the kinetics and thermodynamics of hydrides; and development of novel processes for the direct re-hydrogenation of materials. These efforts have resulted in several advancements the development of hydrogen storage materials. We have greatly extended the fundamental knowledge about the highly promising hydrogen storage carrier, alane (AlH3), by carrying out the first crystal structure determinations and the first determination of the heats of dehydrogenation of β–AlH3 and γ-AlD3. A low-temperature homogenous organometallic approach to incorporation of Al and Mg based hydrides into carbon aerogels has been developed that that allows high loadings without degradation of the nano-porous scaffold. Nano-confinement was found to significantly improve the dehydrogenation kinetics but not effect the enthalpy of dehydrogenation. We conceived, characterized, and synthesized a novel class of potential hydrogen storage materials, bimetallic borohydrides. These novel compounds were found to have many favorable properties including release of significant amounts of hydrogen at moderate temperatures (75-190 º C). However, in situ IR studies in tandem with thermal gravimetric analysis have shown that about 0.5 equivalents of diborane are released during the

  9. Discovery of Novel Complex Metal Hydrides for Hydrogen Storage through Molecular Modeling and Combinatorial Methods

    Energy Technology Data Exchange (ETDEWEB)

    Lesch, David A; Adriaan Sachtler, J.W. J.; Low, John J; Jensen, Craig M; Ozolins, Vidvuds; Siegel, Don; Harmon, Laurel

    2011-02-14

    alanate from alkali hydride, Al and hydrogen, was hampering reversibility. The reverse reaction was then studied for the same phase diagram, starting with LiH, NaH, and MgH2, and Al. The study was extended to phase diagrams including KH and CaH2 as well. The observed hydrogen storage capacity in the Al hexahydrides was less than 4 wt. %, well short of DOE targets. The HT assay came on line and after certification with studies on NaAlH4, was first applied to the LiNH2 - LiBH4 - MgH2 phase diagram. The 60-point study elucidated trends within the system locating an optimum material of 0.6 LiNH2 0.3 MgH2 0.1 LiBH4 that stored about 4 wt. % H2 reversibly and operated below 220 °C. Also present was the phase Li4(NH2)3BH4, which had been discovered in the LiNH2 -LiBH4 system. This new ternary formulation performed much better than the well-known 2 LiNH2MgH2 system by 50 °C in the HT assay. The Li4(NH2)3BH4 is a low melting ionic liquid under our test conditions and facilitates the phase transformations required in the hydrogen storage reaction, which no longer relies on a higher energy solid state reaction pathway. Further study showed that the 0.6 LiNH2 0.3 MgH2 0.1 LiBH4 formulation was very stable with respect to ammonia and diborane desorption, the observed desorption was from hydrogen. This result could not have been anticipated and was made possible by the efficiency of HT combinatorial methods. Investigation of the analogous LiNH2 LiBH4 CaH2 phase diagram revealed new reversible hydrogen storage materials 0.625 LiBH4 + 0.375 CaH2 and 0.375 LiNH2 + 0.25 LiBH4 + 0.375 CaH2 operating at 1 wt. % reversible hydrogen below 175 °C. Powder x-ray diffraction revealed a new structure for the spent materials which had not been previously observed. While the storage capacity was not impressive, an important aspect is that it boron appears to participate in a low temperature reversible reaction. The last major area of study also focused on activating boron-based materials in