Plasma deposition of amorphous metal alloys

DOEpatents

Hays, Auda K.

1986-01-01

Amorphous metal alloy coatings are plasma-deposited by dissociation of vapors of organometallic compounds and metalloid hydrides in the presence of a reducing gas, using a glow discharge. Tetracarbonylnickel, phosphine, and hydrogen constitute a typical reaction mixture of the invention, yielding a NiPC alloy.

Plasma deposition of amorphous metal alloys

DOEpatents

Hays, A.K.

1979-07-18

Amorphous metal alloy coatings are plasma-deposited by dissociation of vapors of organometallic compounds and metalloid hydrides in the presence of a reducing gas, using a glow discharge. Tetracarbonylnickel, phosphine, and hydrogen constitute a typical reaction mixture of the invention, yielding a NiPC alloy.

Formation of amorphous metal alloys by chemical vapor deposition

DOEpatents

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.

Vapor-deposited organic glasses exhibit enhanced stability against photodegradation.

PubMed

Qiu, Yue; Dalal, Shakeel S; Ediger, M D

2018-04-18

Photochemically stable solids are in demand for applications in organic electronics. Previous work has established the importance of the molecular packing environment by demonstrating that different crystal polymorphs of the same compound react at different rates when illuminated. Here we show, for the first time, that different amorphous packing arrangements of the same compound photodegrade at different rates. For these experiments, we utilize the ability of physical vapor deposition to prepare glasses with an unprecedented range of densities and kinetic stabilities. Indomethacin, a pharmaceutical molecule that can undergo photodecarboxylation when irradiated by UV light, is studied as a model system. Photodegradation is assessed through light-induced changes in the mass of glassy thin films due to the loss of CO2, as measured by a quartz crystal microbalance (QCM). Glasses prepared by physical vapor deposition degraded more slowly under UV illumination than did the liquid-cooled glass, with the difference as large as a factor of 2. Resistance to photodegradation correlated with glass density, with the vapor-deposited glasses being up to 1.3% more dense than the liquid-cooled glass. High density glasses apparently limit the local structural changes required for photodegradation.

Communication: Disorder-suppressed vibrational relaxation in vapor-deposited high-density amorphous ice

NASA Astrophysics Data System (ADS)

Shalit, Andrey; Perakis, Fivos; Hamm, Peter

2014-04-01

We apply two-dimensional infrared spectroscopy to differentiate between the two polyamorphous forms of glassy water, low-density (LDA) and high-density (HDA) amorphous ices, that were obtained by slow vapor deposition at 80 and 11 K, respectively. Both the vibrational lifetime and the bandwidth of the 1-2 transition of the isolated OD stretch vibration of HDO in H2O exhibit characteristic differences when comparing hexagonal (Ih), LDA, and HDA ices, which we attribute to the different local structures - in particular the presence of interstitial waters in HDA ice - that cause different delocalization lengths of intermolecular phonon degrees of freedom. Moreover, temperature dependent measurements show that the vibrational lifetime closely follows the structural transition between HDA and LDA phases.

High rate chemical vapor deposition of carbon films using fluorinated gases

DOEpatents

Stafford, Byron L.; Tracy, C. Edwin; Benson, David K.; Nelson, Arthur J.

1993-01-01

A high rate, low-temperature deposition of amorphous carbon films is produced by PE-CVD in the presence of a fluorinated or other halide gas. The deposition can be performed at less than 100.degree. C., including ambient room temperature, with a radio frequency plasma assisted chemical vapor deposition process. With less than 6.5 atomic percent fluorine incorporated into the amorphous carbon film, the characteristics of the carbon film, including index of refraction, mass density, optical clarity, and chemical resistance are within fifteen percent (15%) of those characteristics for pure amorphous carbon films, but the deposition rates are high.

Importance of oxygen in the metal-free catalytic growth of single-walled carbon nanotubes from SiO(x) by a vapor-solid-solid mechanism.

PubMed

Liu, Bilu; Tang, Dai-Ming; Sun, Chenghua; Liu, Chang; Ren, Wencai; Li, Feng; Yu, Wan-Jing; Yin, Li-Chang; Zhang, Lili; Jiang, Chuanbin; Cheng, Hui-Ming

2011-01-19

To understand in-depth the nature of the catalyst and the growth mechanism of single-walled carbon nanotubes (SWCNTs) on a newly developed silica catalyst, we performed this combined experimental and theoretical study. In situ transmission electron microscopy (TEM) observations revealed that the active catalyst for the SWCNT growth is solid and amorphous SiO(x) nanoparticles (NPs), suggesting a vapor-solid-solid growth mechanism. From in situ TEM and chemical vapor deposition growth experiments, we found that oxygen plays a crucial role in SWCNT growth in addition to the well-known catalyst size effect. Density functional theory calculations showed that oxygen atoms can enhance the capture of -CH(x) and consequently facilitate the growth of SWCNTs on oxygen-containing SiO(x) NPs.

Structural analysis of ion-implanted chemical-vapor-deposited diamond by transmission electron microscope

NASA Astrophysics Data System (ADS)

Jiang, N.; Deguchi, M.; Wang, C. L.; Won, J. H.; Jeon, H. M.; Mori, Y.; Hatta, A.; Kitabatake, M.; Ito, T.; Hirao, T.; Sasaki, T.; Hiraki, A.

1997-04-01

A transmission electron microscope (TEM) study of ion-implanted chemical-vapor-deposited (CVD) diamond is presented. CVD diamond used for transmission electron microscope observation was directly deposited onto Mo TEM grids. As-deposited specimens were irradiated by C (100 keV) ions at room temperature with a wide range of implantation doses (10 12-10 17/cm 2). Transmission electron diffraction (TED) patterns indicate that there exists a critical dose ( Dc) for the onset of amorphization of CVD diamond as a result of ion induced damage and the value of critical dose is confirmed to be about 3 × 10 15/cm 2. The ion-induced transformation process is clearly revealed by high resolution electron microscope (HREM) images. For a higher dose implantation (7 × 10 15/cm 2) a large amount of diamond phase is transformed into amorphous carbon and many tiny misoriented diamond blocks are found to be left in the amorphous solid. The average size of these misoriented diamond blocks is only about 1-2 nm. Further bombardment (10 17/cm 2) almost kills all of the diamond phase within the irradiated volume and moreover leads to local formation of micropolycrystalline graphite.

Physical vapor deposition and metalorganic chemical vapor deposition of yttria-stabilized zirconia thin films

NASA Astrophysics Data System (ADS)

Kaufman, David Y.

Two vapor deposition techniques, dual magnetron oblique sputtering (DMOS) and metalorganic chemical vapor deposition (MOCVD), have been developed to produce yttria-stabilized zirconia (YSZ) films with unique microstructures. In particular, biaxially textured thin films on amorphous substrates and dense thin films on porous substrates have been fabricated by DMOS and MOCVD, respectively. DMOS YSZ thin films were deposited by reactive sputtering onto Si (native oxide surface) substrates positioned equidistant between two magnetron sources such that the fluxes arrived at oblique angles with respect to the substrate normal. Incident fluxes from two complimentary oblique directions were necessary for the development of biaxial texture. The films displayed a strong [001] out-of-plane orientation with the <110> direction in the film aligned with the incident flux. Biaxial texture improved with increasing oblique angle and film thickness, and was stronger for films deposited with Ne than with Ar. The films displayed a columnar microstructure with grain bundling perpendicular to the projected flux direction, the degree of which increased with oblique angle and thickness. The texture decreased by sputtering at pressures at which the flux of sputtered atoms was thermalized. These results suggested that grain alignment is due to directed impingement of both sputtered atoms and reflected energetic neutrals. The best texture, a {111} phi FWHM of 23°, was obtained in a 4.8 mum thick film deposited at an oblique angle of 56°. MOCVD YSZ thin films were deposited in a vertical cold-wall reactor using Zr(tmhd)4 and Y(tmhd)3 precursors. Fully stabilized YSZ films with 9 mol% could be deposited by controlling the bubbler temperatures. YSZ films on Si substrates displayed a transition at 525°C from surface kinetic limited growth, with an activation energy of 5.5 kJ/mole, to mass transport limited growth. Modifying the reactor by lowering the inlet height and introducing an Ar baffle

Crystallization of amorphous silicon thin films deposited by PECVD on nickel-metalized porous silicon.

PubMed

Ben Slama, Sonia; Hajji, Messaoud; Ezzaouia, Hatem

2012-08-17

Porous silicon layers were elaborated by electrochemical etching of heavily doped p-type silicon substrates. Metallization of porous silicon was carried out by immersion of substrates in diluted aqueous solution of nickel. Amorphous silicon thin films were deposited by plasma-enhanced chemical vapor deposition on metalized porous layers. Deposited amorphous thin films were crystallized under vacuum at 750°C. Obtained results from structural, optical, and electrical characterizations show that thermal annealing of amorphous silicon deposited on Ni-metalized porous silicon leads to an enhancement in the crystalline quality and physical properties of the silicon thin films. The improvement in the quality of the film is due to the crystallization of the amorphous film during annealing. This simple and easy method can be used to produce silicon thin films with high quality suitable for thin film solar cell applications.

Crystallization of amorphous silicon thin films deposited by PECVD on nickel-metalized porous silicon

PubMed Central

2012-01-01

Porous silicon layers were elaborated by electrochemical etching of heavily doped p-type silicon substrates. Metallization of porous silicon was carried out by immersion of substrates in diluted aqueous solution of nickel. Amorphous silicon thin films were deposited by plasma-enhanced chemical vapor deposition on metalized porous layers. Deposited amorphous thin films were crystallized under vacuum at 750°C. Obtained results from structural, optical, and electrical characterizations show that thermal annealing of amorphous silicon deposited on Ni-metalized porous silicon leads to an enhancement in the crystalline quality and physical properties of the silicon thin films. The improvement in the quality of the film is due to the crystallization of the amorphous film during annealing. This simple and easy method can be used to produce silicon thin films with high quality suitable for thin film solar cell applications. PMID:22901341

Amorphous lithium lanthanum titanate for solid-state microbatteries

DOE PAGES

Lee, Jungwoo Z.; Wang, Ziying; Xin, Huolin L.; ...

2016-12-16

Lithium lanthanum titanate (LLTO) is a promising solid state electrolyte for solid state batteries due to its demonstrated high bulk ionic conductivity. However, crystalline LLTO has a relatively low grain boundary conductivity, limiting the overall material conductivity. In this work, we investigate amorphous LLTO (a-LLTO) thin films grown by pulsed laser deposition (PLD). By controlling the background pressure and temperature we are able to optimize the ionic conductivity to 3 × 10 –4 S/cm and electronic conductivity to 5 × 10 –11 S/cm. XRD, TEM, and STEM/EELS analysis confirm that the films are amorphous and indicate that oxygen background gasmore » is necessary during the PLD process to decrease the oxygen vacancy concentration, decreasing the electrical conductivity. Amorphous LLTO is deposited onto high voltage LiNi 0.5Mn 1.5O 4 (LNMO) spinel cathode thin films and cycled up to 4.8 V vs. Li showing excellent capacity retention. Finally, these results demonstrate that a-LLTO has the potential to be integrated into high voltage thin film batteries.« less

Influence of Molecular Shape on Molecular Orientation and Stability of Vapor-Deposited Organic Semiconductors

NASA Astrophysics Data System (ADS)

Walters, Diane M.; Johnson, Noah D.; Ediger, M. D.

Physical vapor deposition is commonly used to prepare active layers in organic electronics. Recently, it has been shown that molecular orientation and packing can be tuned by changing the substrate temperature during deposition, while still producing macroscopically homogeneous films. These amorphous materials can be highly anisotropic when prepared with low substrate temperatures, and they can exhibit exceptional kinetic stability; films retain their favorable packing when heated to high temperatures. Here, we study the influence of molecular shape on molecular orientation and stability. We investigate disc-shaped molecules, such as TCTA and m-MTDATA, nearly spherical molecules, such as Alq3, and linear molecules covering a broad range of aspect ratios, such as p-TTP and BSB-Cz. Disc-shaped molecules have preferential horizontal orientation when deposited at low substrate temperatures, and their orientation can be tuned by changing the substrate temperature. Alq3 forms stable, amorphous films that are optically isotropic when vapor deposited over a broad range of substrate temperatures. This work may guide the choice of material and deposition conditions for vapor-deposited films used in organic electronics and allow for more efficient devices to be fabricated.

Understanding the Reaction Chemistry of 2,2':5',2''-Terthiophene Films with Vapor-Deposited Ag, Al, and Ca

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

Sang, Lingzi; Matz, Dallas L.; Pemberton, Jeanne E.

The reaction chemistry of vapor-deposited 2,2':5',2''-terthiophene (α-3T) solid-state thin films with postdeposited Ag, Al, and Ca is investigated in ultrahigh vacuum using Raman spectroscopy. Vapor-deposited Ag forms nanoparticles on these films and induces considerable surface enhanced Raman scattering (SERS) along with a change in molecular symmetry of adjacent α-3T and formation of Ag–S bonds; no other reaction chemistry is observed. Vapor-deposited Al and Ca undergo chemical reaction with α-3T initiated by metal-to-α-3T electron transfer. For Al, the resulting product is predominantly amorphous carbon through initial radical formation and subsequent decomposition reactions. For Ca, the spectral evidence suggests two pathways: onemore » leading to α-3T polymerization and the other resulting in thiophene ring opening, both initiated by radical formation through Ca-to-α-3T electron transfer. These interfacial reactions reflect the complex chemistry that can occur between low work function metals and thiophene-based oligomers. This reactivity is strongly correlated with metal work function.« less

Understanding the Reaction Chemistry of 2,2':5',2"-Terthiophene Films with Vapor-Deposited Ag, Al, and Ca

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

Sang, Lingzi; Matz, Dallas L.; Pemberton, Jeanne E.

The reaction chemistry of vapor-deposited 2,2':5',2''-terthiophene (α-3T) solid-state thin films with postdeposited Ag, Al, and Ca is investigated in ultrahigh vacuum using Raman spectroscopy. Vapor-deposited Ag forms nanoparticles on these films and induces considerable surface enhanced Raman scattering (SERS) along with a change in molecular symmetry of adjacent α-3T and formation of Ag–S bonds; no other reaction chemistry is observed. Vapor-deposited Al and Ca undergo chemical reaction with α-3T initiated by metal-to-α-3T electron transfer. For Al, the resulting product is predominantly amorphous carbon through initial radical formation and subsequent decomposition reactions. For Ca, the spectral evidence suggests two pathways: onemore » leading to α-3T polymerization and the other resulting in thiophene ring opening, both initiated by radical formation through Ca-to-α-3T electron transfer. These interfacial reactions reflect the complex chemistry that can occur between low work function metals and thiophene-based oligomers. This reactivity is strongly correlated with metal work function.« less

A Self Consistent RF Discharge, Plasma Chemistry and Surface Model for Plasma Enhanced Chemical Vapor Deposition

DTIC Science & Technology

1988-06-30

consists of three submodels for the electron kinetics, plasma chemistry , and surface deposition kinetics for a-Si:H deposited from radio frequency...properties. Plasma enhanced, Chemical vapor deposition, amorphous silicon, Modeling, Electron kinetics, Plasma chemistry , Deposition kinetics, Rf discharge, Silane, Film properties, Silicon.

Si substrates texturing and vapor-solid-solid Si nanowhiskers growth using pure hydrogen as source gas

NASA Astrophysics Data System (ADS)

Nordmark, H.; Nagayoshi, H.; Matsumoto, N.; Nishimura, S.; Terashima, K.; Marioara, C. D.; Walmsley, J. C.; Holmestad, R.; Ulyashin, A.

2009-02-01

Scanning and transmission electron microscopies have been used to study silicon substrate texturing and whisker growth on Si substrates using pure hydrogen source gas in a tungsten hot filament reactor. Substrate texturing, in the nanometer to micrometer range of mono- and as-cut multicrystalline silicon, was observed after deposition of WSi2 particles that acted as a mask for subsequent hydrogen radical etching. Simultaneous Si whisker growth was observed for long residence time of the source gas and low H2 flow rate with high pressure. The whiskers formed via vapor-solid-solid growth, in which the deposited WSi2 particles acted as catalysts for a subsequent metal-induced layer exchange process well below the eutectic temperature. In this process, SiHx species, formed by substrate etching by the H radicals, diffuse through the metal particles. This leads to growth of crystalline Si whiskers via metal-induced solid-phase crystallization. Transmission electron microscopy, electron diffraction, and x-ray energy dispersive spectroscopy were used to study the WSi2 particles and the structure of the Si substrates in detail. It has been established that the whiskers are partly crystalline and partly amorphous, consisting of pure Si with WSi2 particles on their tips as well as sometimes being incorporated into their structure.

Vapor deposition of water on graphitic surfaces: formation of amorphous ice, bilayer ice, ice I, and liquid water.

PubMed

Lupi, Laura; Kastelowitz, Noah; Molinero, Valeria

2014-11-14

Carbonaceous surfaces are a major source of atmospheric particles and could play an important role in the formation of ice. Here we investigate through molecular simulations the stability, metastability, and molecular pathways of deposition of amorphous ice, bilayer ice, and ice I from water vapor on graphitic and atomless Lennard-Jones surfaces as a function of temperature. We find that bilayer ice is the most stable ice polymorph for small cluster sizes, nevertheless it can grow metastable well above its region of thermodynamic stability. In agreement with experiments, the simulations predict that on increasing temperature the outcome of water deposition is amorphous ice, bilayer ice, ice I, and liquid water. The deposition nucleation of bilayer ice and ice I is preceded by the formation of small liquid clusters, which have two wetting states: bilayer pancake-like (wetting) at small cluster size and droplet-like (non-wetting) at larger cluster size. The wetting state of liquid clusters determines which ice polymorph is nucleated: bilayer ice nucleates from wetting bilayer liquid clusters and ice I from non-wetting liquid clusters. The maximum temperature for nucleation of bilayer ice on flat surfaces, T(B)(max) is given by the maximum temperature for which liquid water clusters reach the equilibrium melting line of bilayer ice as wetting bilayer clusters. Increasing water-surface attraction stabilizes the pancake-like wetting state of liquid clusters leading to larger T(B)(max) for the flat non-hydrogen bonding surfaces of this study. The findings of this study should be of relevance for the understanding of ice formation by deposition mode on carbonaceous atmospheric particles, including soot.

Characterization of molecular disorder in vapor-deposited thin films of aluminum tris(quinoline-8-olate) by one-dimensional 27Al NMR under magic angle spinning.

PubMed

Utz, Marcel; Nandagopal, Magesh; Mathai, Mathew; Papadimitrakopoulos, Fotios

2006-01-21

Aluminum tris (quinoline-8-olate) (Alq3) is used as an electron-transport layer in organic light-emitting diodes. The material can be obtained in a wide range of different solid phases, both crystalline and amorphous, by deposition from the vapor phase or from solution under controlled conditions. While the structure of the crystalline polymorphs of Alq3 has been investigated thoroughly by x-ray diffraction as well as solid-state NMR, very little information is currently available on the amount of structural disorder in the amorphous forms of Alq3. In the present contribution, we report the use of 27Al NMR spectroscopy in the solid state under magic angle spinning to extract such information from amorphous vapor deposits of Alq3. The NMR spectra obtained from these samples exhibit different degrees of broadening, reflecting distributions of the electric-field gradient tensor at the site of the aluminum ion. These distributions can be obtained from the NMR spectra by solving the corresponding inverse problem. From these results, the magnitude of structural disorder in terms of molecular geometry has been estimated by density-functional theory calculations. It was found that the electric-field gradient anisotropy delta follows a bimodal distribution. Its majority component is centered around delta values comparable to the meridianal alpha crystal polymorph and has a width of about 10%, corresponding to distortions of the molecular geometry of a few degrees in the orientation of the ligands. Alq3 samples obtained at higher deposition rates exhibit higher degrees of disorder. The minor component, present at about 7%, has a much smaller anisotropy, suggesting that it may be due to the facial isomer of Alq3.

Tunable carbon nanotube-tungsten carbide nanoparticles heterostructures by vapor deposition

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

Xia, Min; Guo, Hongyan; Ge, Changchun

2014-05-14

A simple, versatile route for the synthesis of carbon nanotube (CNT)-tungsten carbide nanoparticles heterostructures was set up via vapor deposition process. For the first time, amorphous CNTs (α-CNTs) were used to immobilized tungsten carbide nanoparticles. By adjusting the synthesis and annealing temperature, α-CNTs/amorphous tungsten carbide, α-CNTs/W{sub 2}C, and CNTs/W{sub 2}C/WC heterostructures were prepared. This approach provides an efficient method to attach other metal carbides and other nanoparticles to carbon nanotubes with tunable properties.

Physical vapor deposition as a route to hidden amorphous states

PubMed Central

Dawson, Kevin J.; Kearns, Kenneth L.; Yu, Lian; Steffen, Werner; Ediger, M. D.

2009-01-01

Stable glasses of indomethacin (IMC) were prepared by using physical vapor deposition. Wide-angle X-ray scattering measurements were performed to characterize the average local structure. IMC glasses prepared at a substrate temperature of 0.84 Tg (where Tg is the glass transition temperature) and a deposition rate of 0.2 nm/s show a broad, high-intensity peak at low q values that is not present in the supercooled liquid or melt-quenched glasses. When annealed slightly above Tg, the new WAXS pattern transforms into the melt-quenched glass pattern, but only after very long annealing times. For a series of samples prepared at the lowest deposition rate, the new local packing arrangement is present only for deposition temperatures below Tg −20 K, suggesting an underlying first-order liquid-to-liquid phase transition. PMID:19666494

Rapid vapor deposition of highly conformal silica nanolaminates.

PubMed

Hausmann, Dennis; Becker, Jill; Wang, Shenglong; Gordon, Roy G

2002-10-11

Highly uniform and conformal coatings can be made by the alternating exposures of a surface to vapors of two reactants, in a process commonly called atomic layer deposition (ALD). The application of ALD has, however, been limited because of slow deposition rates, with a theoretical maximum of one monolayer per cycle. We show that alternating exposure of a surface to vapors of trimethylaluminum and tris(tert-butoxy)silanol deposits highly conformal layers of amorphous silicon dioxide and aluminum oxide nanolaminates at rates of 12 nanometers (more than 32 monolayers) per cycle. This process allows for the uniform lining or filling of long, narrow holes. We propose that these ALD layers grow by a previously unknown catalytic mechanism that also operates during the rapid ALD of many other metal silicates. This process should allow improved production of many devices, such as trench insulation between transistors in microelectronics, planar waveguides, microelectromechanical structures, multilayer optical filters, and protective layers against diffusion, oxidation, or corrosion.

A three-dimensional phase field model for nanowire growth by the vapor-liquid-solid mechanism

NASA Astrophysics Data System (ADS)

Wang, Yanming; Ryu, Seunghwa; McIntyre, Paul C.; Cai, Wei

2014-07-01

We present a three-dimensional multi-phase field model for catalyzed nanowire (NW) growth by the vapor-liquid-solid (VLS) mechanism. The equation of motion contains both a Ginzburg-Landau term for deposition and a diffusion (Cahn-Hilliard) term for interface relaxation without deposition. Direct deposition from vapor to solid, which competes with NW crystal growth through the molten catalyst droplet, is suppressed by assigning a very small kinetic coefficient at the solid-vapor interface. The thermodynamic self-consistency of the model is demonstrated by its ability to reproduce the equilibrium contact angles at the VLS junction. The incorporation of orientation dependent gradient energy leads to faceting of the solid-liquid and solid-vapor interfaces. The model successfully captures the curved shape of the NW base and the Gibbs-Thomson effect on growth velocity.

Improved amorphous/crystalline silicon interface passivation for heterojunction solar cells by low-temperature chemical vapor deposition and post-annealing treatment.

PubMed

Wang, Fengyou; Zhang, Xiaodan; Wang, Liguo; Jiang, Yuanjian; Wei, Changchun; Xu, Shengzhi; Zhao, Ying

2014-10-07

In this study, hydrogenated amorphous silicon (a-Si:H) thin films are deposited using a radio-frequency plasma-enhanced chemical vapor deposition (RF-PECVD) system. The Si-H configuration of the a-Si:H/c-Si interface is regulated by optimizing the deposition temperature and post-annealing duration to improve the minority carrier lifetime (τeff) of a commercial Czochralski (Cz) silicon wafer. The mechanism of this improvement involves saturation of the microstructural defects with hydrogen evolved within the a-Si:H films due to the transformation from SiH2 into SiH during the annealing process. The post-annealing temperature is controlled to ∼180 °C so that silicon heterojunction solar cells (SHJ) could be prepared without an additional annealing step. To achieve better performance of the SHJ solar cells, we also optimize the thickness of the a-Si:H passivation layer. Finally, complete SHJ solar cells are fabricated using different temperatures for the a-Si:H film deposition to study the influence of the deposition temperature on the solar cell parameters. For the optimized a-Si:H deposition conditions, an efficiency of 18.41% is achieved on a textured Cz silicon wafer.

Deposition of amorphous carbon thin films by aerosol-assisted CVD method

NASA Astrophysics Data System (ADS)

Fadzilah, A. N.; Dayana, K.; Rusop, M.

2018-05-01

This paper reports on the deposition of amorphous carbon (a-C) by Aerosol-assisted Chemical Vapor Deposition (AACVD) using natural source of camphor oil as the precursor material. 4 samples were deposited at 4 different deposition flow rate from 15 sccm to 20 sccm, with 5 sccm interval for each sample. The analysis includes the electrical, optical and structural analysis of the data. The a-C structure which came from the manipulation of synthesis parameter was characterized by the solar simulator system, UV-VIS-NIR, Raman spectroscope and AFM. The properties of a-C are highly dependent on the deposition techniques and deposition parameters; hence the influences of gas flow rate were studied.

Plasma deposited stability enhancement coating for amorphous ketoprofen.

PubMed

Bosselmann, Stephanie; Owens, Donald E; Kennedy, Rachel L; Herpin, Matthew J; Williams, Robert O

2011-05-01

A hydrophobic fluorocarbon coating deposited onto amorphous ketoprofen via pulsed plasma-enhanced chemical vapor deposition (PPECVD) significantly prolonged the onset of recrystallization compared to uncoated drug. Rapid freezing (RF) employed to produce amorphous ketoprofen was followed by PPECVD of perfluorohexane. The effect of coating thickness on the recrystallization and dissolution behavior of ketoprofen was investigated. Samples were stored in open containers at 40°C and 75% relative humidity, and the onset of recrystallization was monitored by DSC. An increase in coating thickness provided enhanced stability against recrystallization for up to 6 months at accelerated storage conditions (longest time of observation) when compared to three days for uncoated ketoprofen. Results from XPS analysis demonstrated that an increase in coating thickness was associated with improved surface coverage thus enabling superior protection. Dissolution testing showed that at least 80% of ketoprofen was released in buffer pH 6.8 from all coated samples. Overall, an increase in coating thickness resulted in a more complete drug release due to decreased adhesion of the coating to the substrate. Copyright © 2010 Elsevier B.V. All rights reserved.

Semiconducting Properties of Nanostructured Amorphous Carbon Thin Films Incorporated with Iodine by Thermal Chemical Vapor Deposition

NASA Astrophysics Data System (ADS)

Kamaruzaman, Dayana; Ahmad, Nurfadzilah; Annuar, Ishak; Rusop, Mohamad

2013-11-01

Nanostructured iodine-post doped amorphous carbon (a-C:I) thin films were prepared from camphor oil using a thermal chemical vapor deposition (TCVD) technique at different doping temperatures. The structural properties of the films were studied by field-emission scanning electron microscopy (FESEM), energy-dispersive spectroscopy (EDS), Raman, and Fourier transform infrared (FTIR) studies. FESEM and EDS studies showed successful iodine doping. FTIR and Raman studies showed that the a-C:I thin films consisted of a mixture of sp2- and sp3-bonded carbon atoms. The optical and electrical properties of a-C:I thin films were determined by UV-vis-NIR spectroscopy and current-voltage (I-V) measurement respectively. The optical band gap of a-C thin films decreased upon iodine doping. The highest electrical conductivity was found at 400 °C doping. Heterojunctions are confirmed by rectifying the I-V characteristics of an a-C:I/n-Si junction.

Degradation by water vapor of hydrogenated amorphous silicon oxynitride films grown at low temperature.

PubMed

Lee, Hyung-Ik; Park, Jong-Bong; Xianyu, Wenxu; Kim, Kihong; Chung, Jae Gwan; Kyoung, Yong Koo; Byun, Sunjung; Yang, Woo Young; Park, Yong Young; Kim, Seong Min; Cho, Eunae; Shin, Jai Kwang

2017-10-26

We report on the degradation process by water vapor of hydrogenated amorphous silicon oxynitride (SiON:H) films deposited by plasma-enhanced chemical vapor deposition at low temperature. The stability of the films was investigated as a function of the oxygen content and deposition temperature. Degradation by defects such as pinholes was not observed with transmission electron microscopy. However, we observed that SiON:H film degrades by reacting with water vapor through only interstitial paths and nano-defects. To monitor the degradation process, the atomic composition, mass density, and fully oxidized thickness were measured by using high-resolution Rutherford backscattering spectroscopy and X-ray reflectometry. The film rapidly degraded above an oxygen composition of ~27 at%, below a deposition temperature of ~150 °C, and below an mass density of ~2.15 g/cm 3 . This trend can be explained by the extents of porosity and percolation channel based on the ring model of the network structure. In the case of a high oxygen composition or low temperature, the SiON:H film becomes more porous because the film consists of network channels of rings with a low energy barrier.

The Vapor Deposition Model of Space Weathering: A Strawman Paradigm for the Moon

NASA Astrophysics Data System (ADS)

Hapke, Bruce W.

1998-01-01

Understanding space weathering on the lunar surface is essential to solving a number of major problems, including correctly interpreting lunar remote-sensing observations, understanding physical and chemical processes in the lunar regolith, and extrapolating to other bodies, especially Mercury, the asteroids, and the parent bodies of the ordinary chondrites. Hence, it is of great importance to correctly identify the process or processes that dominate lunar space weathering. The vapor deposition model postulates that lunar space weathering occurs as a result of the production of submicrscopic metallic iron (SMFe, also called superparamagnetic iron and nanophase iron) particles in the regolith by the intrinsic differentiation that accompanies the deposition of silicate vapor produced by both solar wind sputtering and micrometeorite impacts. This is the only process that has been demonstrated repeatedly by laboratory experiments to be capable of selectively producing SMFe. Hence, at present, it must be regarded as the leading contender for the correct model of lunar space weathering. This paper reviews the features of the vapor deposition model. The basic mechanism of the model relies on the fact that the porous microrelief of the lunar regolith allows most of the vapor produced by sputtering and impacts to be retained in the soil, rather than escaping from the Moon. As the individual vapor atoms impact the soil grain surfaces, they are first weakly bound by physical adsorption processes, and so have a finite probability of desorbing and escaping. Since the O is the most volatile, it escapes preferentially. The remaining atoms become chemically bound and form amorphous coatings on lunar soil grains. Because Fe is the most easily reduced of the major cations in the soil, the O deficiency manifests itself in the form of interstitial Fe0 in the glass deposits. Subsequent heating by impacts allows the Feo atoms to congregate together by solid-state diffusion to form SMFe

Water-Assisted Vapor Deposition of PEDOT Thin Film.

PubMed

Goktas, Hilal; Wang, Xiaoxue; Ugur, Asli; Gleason, Karen K

2015-07-01

The synthesis and characterization of poly(3,4-ethylenedioxythiophene) (PEDOT) using water-assisted vapor phase polymerization (VPP) and oxidative chemical vapor deposition (oCVD) are reported. For the VPP PEDOT, the oxidant, FeCl3 , is sublimated onto the substrate from a heated crucible in the reactor chamber and subsequently exposed to 3,4-ethylenedioxythiophene (EDOT) monomer and water vapor in the same reactor. The oCVD PEDOT was produced by introducing the oxidant, EDOT monomer, and water vapor simultaneously to the reactor. The enhancement of doping and crystallinity is observed in the water-assisted oCVD thin films. The high doping level observed at UV-vis-NIR spectra for the oCVD PEDOT, suggests that water acts as a solubilizing agent for oxidant and its byproducts. Although the VPP produced PEDOT thin films are fully amorphous, their conductivities are comparable with that of the oCVD produced ones. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Clathrate hydrate formation in amorphous cometary ice analogs in vacuo

NASA Technical Reports Server (NTRS)

Blake, David; Allamandola, Louis; Sandford, Scott; Hudgins, Doug; Freund, Friedemann

1991-01-01

Experiments conducted in clathrate hydrates with a modified electron microscope have demonstrated the possibility of such compounds' formation during the warming of vapor-deposited amorphous ices in vacuo, through rearrangements in the solid state. Subsolidus crystallization of compositionally complex amorphous ices may therefore be a general and ubiquitous process. Phase separations and microporous textures thus formed may be able to account for such anomalous cometary phenomena as the release of gas at large radial distances from the sun and the retention of volatiles to elevated temperatures.

Amorphous silicon ionizing particle detectors

DOEpatents

Street, Robert A.; Mendez, Victor P.; Kaplan, Selig N.

1988-01-01

Amorphous silicon ionizing particle detectors having a hydrogenated amorphous silicon (a--Si:H) thin film deposited via plasma assisted chemical vapor deposition techniques are utilized to detect the presence, position and counting of high energy ionizing particles, such as electrons, x-rays, alpha particles, beta particles and gamma radiation.

Influence of Molecular Shape on the Thermal Stability and Molecular Orientation of Vapor-Deposited Organic Semiconductors

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

Walters, Diane M; Antony, Lucas; de Pablo, Juan

High thermal stability and anisotropic molecular orientation enhance the performance of vapor-deposited organic semiconductors, but controlling these properties is a challenge in amorphous materials. To understand the influence of molecular shape on these properties, vapor-deposited glasses of three disk-shaped molecules were prepared. For all three systems, enhanced thermal stability is observed for glasses prepared over a wide range of substrate temperatures and anisotropic molecular orientation is observed at lower substrate temperatures. For two of the disk-shaped molecules, atomistic simulations of thin films were also performed and anisotropic molecular orientation was observed at the equilibrium liquid surface. We find that themore » structure and thermal stability of these vapor-deposited glasses results from high surface mobility and partial equilibration toward the structure of the equilibrium liquid surface during the deposition process. For the three molecules studied, molecular shape is a dominant factor in determining the anisotropy of vapor-deposited glasses.« less

Role of Co-Vapors in Vapor Deposition Polymerization

PubMed Central

Lee, Ji Eun; Lee, Younghee; Ahn, Ki-Jin; Huh, Jinyoung; Shim, Hyeon Woo; Sampath, Gayathri; Im, Won Bin; Huh, Yang–Il; Yoon, Hyeonseok

2015-01-01

Polypyrrole (PPy)/cellulose (PPCL) composite papers were fabricated by vapor phase polymerization. Importantly, the vapor-phase deposition of PPy onto cellulose was assisted by employing different co-vapors namely methanol, ethanol, benzene, water, toluene and hexane, in addition to pyrrole. The resulting PPCL papers possessed high mechanical flexibility, large surface-to-volume ratio, and good redox properties. Their main properties were highly influenced by the nature of the co-vaporized solvent. The morphology and oxidation level of deposited PPy were tuned by employing co-vapors during the polymerization, which in turn led to change in the electrochemical properties of the PPCL papers. When methanol and ethanol were used as co-vapors, the conductivities of PPCL papers were found to have improved five times, which was likely due to the enhanced orientation of PPy chain by the polar co-vapors with high dipole moment. The specific capacitance of PPCL papers obtained using benzene, toluene, water and hexane co-vapors was higher than those of the others, which is attributed to the enlarged effective surface area of the electrode material. The results indicate that the judicious choice and combination of co-vapors in vapor-deposition polymerization (VDP) offers the possibility of tuning the morphological, electrical, and electrochemical properties of deposited conducting polymers. PMID:25673422

Amorphous silicon ionizing particle detectors

DOEpatents

Street, R.A.; Mendez, V.P.; Kaplan, S.N.

1988-11-15

Amorphous silicon ionizing particle detectors having a hydrogenated amorphous silicon (a--Si:H) thin film deposited via plasma assisted chemical vapor deposition techniques are utilized to detect the presence, position and counting of high energy ionizing particles, such as electrons, x-rays, alpha particles, beta particles and gamma radiation. 15 figs.

Amorphous silicon-carbon nanospheres synthesized by chemical vapor deposition using cheap methyltrichlorosilane as improved anode materials for Li-ion batteries.

PubMed

Zhang, Zailei; Zhang, Meiju; Wang, Yanhong; Tan, Qiangqiang; Lv, Xiao; Zhong, Ziyi; Li, Hong; Su, Fabing

2013-06-21

We report the preparation and characterization of amorphous silicon-carbon (Si-C) nanospheres as anode materials in Li-ion batteries. These nanospheres were synthesized by a chemical vapor deposition at 900 °C using methyltrichlorosilane (CH3SiCl3) as both the Si and C precursor, which is a cheap byproduct in the organosilane industry. The samples were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, nitrogen adsorption, thermal gravimetric analysis, Raman spectroscopy, and X-ray photoelectron spectroscopy. It was found that the synthesized Si-C nanospheres composed of amorphous C (about 60 wt%) and Si (about 40 wt%) had a diameter of 400-600 nm and a surface area of 43.8 m(2) g(-1). Their charge capacities were 483.6, 331.7, 298.6, 180.6, and 344.2 mA h g(-1) at 50, 200, 500, 1000, and 50 mA g(-1) after 50 cycles, higher than that of the commercial graphite anode. The Si-C amorphous structure could absorb a large volume change of Si during Li insertion and extraction reactions and hinder the cracking or crumbling of the electrode, thus resulting in the improved reversible capacity and cycling stability. The work opens a new way to fabricate low cost Si-C anode materials for Li-ion batteries.

Solid-state diffusion in amorphous zirconolite

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

Yang, C.; Dove, M. T.; Trachenko, K.

2014-11-14

We discuss how structural disorder and amorphization affect solid-state diffusion, and consider zirconolite as a currently important case study. By performing extensive molecular dynamics simulations, we disentangle the effects of amorphization and density, and show that a profound increase of solid-state diffusion takes place as a result of amorphization. Importantly, this can take place at the same density as in the crystal, representing an interesting general insight regarding solid-state diffusion. We find that decreasing the density in the amorphous system increases pre-factors of diffusion constants, but does not change the activation energy in the density range considered. We also findmore » that atomic species in zirconolite are affected differently by amorphization and density change. Our microscopic insights are relevant for understanding how solid-state diffusion changes due to disorder and for building predictive models of operation of materials to be used to encapsulate nuclear waste.« less

Optical and Structural Properties of Microcrystalline GaN on an Amorphous Substrate Prepared by a Combination of Molecular Beam Epitaxy and Metal-Organic Chemical Vapor Deposition

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

Min, Jung-Wook; Hwang, Hyeong-Yong; Kang, Eun-Kyu

2016-05-01

Microscale platelet-shaped GaN grains were grown on amorphous substrates by a combined epitaxial growth method of molecular beam epitaxy (MBE) and metal-organic chemical vapor deposition (MOCVD). First, MBE GaN was grown on an amorphous substrate as a pre-orienting layer and its structural properties were investigated. Second, MOCVD grown GaN samples using the different growth techniques of planar and selective area growth (SAG) were comparatively investigated by transmission electron microscopy (TEM), cathodoluminescence (CL), and photoluminescence (PL). In MOCVD planar GaN, strong bound exciton peaks dominated despite the high density of the threading dislocations (TDs). In MOCVD SAG GaN, on the othermore » hand, TDs were clearly reduced with bending, but basal stacking fault (BSF) PL peaks were observed at 3.42 eV. The combined epitaxial method not only provides a deep understanding of the growth behavior but also suggests an alternative approach for the growth of GaN on amorphous substances.« less

Thin film solar cells with Si nanocrystallites embedded in amorphous intrinsic layers by hot-wire chemical vapor deposition.

PubMed

Park, Seungil; Parida, Bhaskar; Kim, Keunjoo

2013-05-01

We investigated the thin film growths of hydrogenated silicon by hot-wire chemical vapor deposition with different flow rates of SiH4 and H2 mixture ambient and fabricated thin film solar cells by implementing the intrinsic layers to SiC/Si heterojunction p-i-n structures. The film samples showed the different infrared absorption spectra of 2,000 and 2,100 cm(-1), which are corresponding to the chemical bonds of SiH and SiH2, respectively. The a-Si:H sample with the relatively high silane concentration provides the absorption peak of SiH bond, but the microc-Si:H sample with the relatively low silane concentration provides the absorption peak of SiH2 bond as well as SiH bond. Furthermore, the microc-Si:H sample showed the Raman spectral shift of 520 cm(-1) for crystalline phase Si bonds as well as the 480 cm(-1) for the amorphous phase Si bonds. These bonding structures are very consistent with the further analysis of the long-wavelength photoconduction tail and the formation of nanocrystalline Si structures. The microc-Si:H thin film solar cell has the photovoltaic behavior of open circuit voltage similar to crystalline silicon thin film solar cell, indicating that microc-Si:H thin film with the mixed phase of amorphous and nanocrystalline structures show the carrier transportation through the channel of nanocrystallites.

Structural and optical characterization of self-assembled Ge nanocrystal layers grown by plasma-enhanced chemical vapor deposition.

PubMed

Saeed, Saba; Buters, Frank; Dohnalova, Katerina; Wosinski, Lech; Gregorkiewicz, Tom

2014-10-10

We present a structural and optical study of solid-state dispersions of Ge nanocrystals prepared by plasma-enhanced chemical vapor deposition. Structural analysis shows the presence of nanocrystalline germanium inclusions embedded in an amorphous matrix of Si-rich SiO(2).Optical characterization reveals two prominent emission bands centered around 2.6 eV and 3.4 eV, and tunable by excitation energy. In addition, the lower energy band shows an excitation power-dependent blue shift of up to 0.3 eV. Decay dynamics of the observed emission contains fast (nanosecond) and slow (microseconds) components, indicating contributions of several relaxation channels. Based on these material characteristics, a possible microscopic origin of the individual emission bands is discussed.

Preparation of hydrogenated amorphous carbon films using a microsecond-pulsed DC capacitive-coupled plasma chemical vapor deposition system operated at high frequency up to 400 kHz

NASA Astrophysics Data System (ADS)

Mamun, Md Abdullah Al; Furuta, Hiroshi; Hatta, Akimitsu

2018-06-01

Hydrogenated amorphous carbon (a-C:H) films are deposited on silicon (Si) substrates using a high-repetition microsecond-pulsed DC plasma chemical vapor deposition (CVD) system from acetylene (C2H2) at a gas pressure of 15 Pa inside a custom-made vacuum chamber. The plasma discharge characteristics, hydrocarbon species, and the microstructure of the resulting films are examined at various pulse repetition rates from 50 to 400 kHz and a fixed duty cycle of 50%. The optical emission spectra confirmed the increase in electron excitation energy from 1.09 to 1.82 eV and the decrease in the intensity ratio of CH/C2 from 1.04 to 0.75 with increasing pulse frequency, indicating the enhanced electron impact dissociation of C2H2 gas. With increasing pulse frequency, the deposition rate gradually increased, reaching a maximum rate of 60 nm/min at 200 kHz, after which a progressive decrease was noted, whereas the deposition area was almost uniform for all the prepared films. Clear trends of increasing sp3 content (amorphization) and decreasing hydrogen (H) content in the films were observed as the pulse repetition rate increased, while most of the hydrogen atoms bonded to carbon atoms by sp3 hybridization rather than by sp2 hybridization.

Amorphous indium-gallium-zinc-oxide thin-film transistors using organic-inorganic hybrid films deposited by low-temperature plasma-enhanced chemical vapor deposition for all dielectric layers

NASA Astrophysics Data System (ADS)

Hsu, Chao-Jui; Chang, Ching-Hsiang; Chang, Kuei-Ming; Wu, Chung-Chih

2017-01-01

We investigated the deposition of high-performance organic-inorganic hybrid dielectric films by low-temperature (close to room temperature) inductively coupled plasma chemical vapor deposition (ICP-CVD) with hexamethyldisiloxane (HMDSO)/O2 precursor gas. The hybrid films exhibited low leakage currents and high breakdown fields, suitable for thin-film transistor (TFT) applications. They were successfully integrated into the gate insulator, the etch-stop layer, and the passivation layer for bottom-gate staggered amorphous In-Ga-Zn-O (a-IGZO) TFTs having the etch-stop configuration. With the double-active-layer configuration having a buffer a-IGZO back-channel layer grown in oxygen-rich atmosphere for better immunity against plasma damage, the etch-stop-type bottom-gate staggered a-IGZO TFTs with good TFT characteristics were successfully demonstrated. The TFTs showed good field-effect mobility (μFE), threshold voltage (V th), subthreshold swing (SS), and on/off ratio (I on/off) of 7.5 cm2 V-1 s-1, 2.38 V, 0.38 V/decade, and 2.2 × 108, respectively, manifesting their usefulness for a-IGZO TFTs.

Hybrid gas-to-particle conversion and chemical vapor deposition for production of high-surface area films

NASA Astrophysics Data System (ADS)

Nguyen, Quynh Tan

A hybrid process, based upon gas-to-particle conversion and chemical vapor deposition, is presented as an alternative technique for producing porous films with the main advantages of solvent-free, low-substrate temperature operation. Starting from solid precursors, nanoparticles were produced in the vapor phase. Downstream of this reaction zone, these nanoparticles were collected via thermophoresis onto a cooled substrate forming a porous film. Initially, alumina (Al2O3) films were produced. Later, multi-component processing was explored by incorporating platinum (Pt) nanoparticles into the Al2O3 matrix leading to the production of Pt/Al 2O3 films by two routes: simultaneous precursor injection processing or by a layer-by-layer approach. In single component processing, the formation of nanoparticle aggregates was evident within the amorphous Al2O3 films. Aggregates, composed of these particles, are likely held together by relatively weak van der Waals forces leading to the observed poor physical cohesion. In multi-component processing, reasonable control of composition and distribution of species is possible with Pt nanoparticles appearing to be co-agglomerated with alumina. Deposited crystalline Pt nanoparticles may encourage the crystallization of the amorphous Al2O3. Finally, from chemisorption results, the produced sample appears to have potentially greater catalytic activity than a commercially available standard. A model is in development to study nanoparticle interactions with a gas and deposition occurring in stagnation flow onto the cooled horizontal substrate within the tubular reactor. Using velocity and temperature fields generated from numerical solutions to the Navier-Stokes and energy equations, particle trajectories were calculated from the summation of drag, gravitational, thermophoretic, and Brownian forces. In rectangular coordinates, cooling stage width to reactor diameter ratio, deposition stage temperature, and initial velocity were the

Interactions between glycine and amorphous solid water nanoscale films

NASA Astrophysics Data System (ADS)

Tzvetkov, George; Koller, Georg; Netzer, Falko P.

2012-12-01

The interactions of glycine (Gly) with amorphous solid water (ASW) nanolayers (≤ 100 ML), vapor-deposited on single crystalline AlOx surfaces at 100 K, have been investigated by near-edge X-ray absorption fine structure spectroscopy (NEXAFS) at the oxygen K-edge, temperature-programmed thermal desorption (TPD), X-ray photoelectron spectroscopy (XPS), and temperature-dependent work function measurements. Gly-on-ASW, ASW-on-Gly, and Gly on top of ASW-on-Gly ultrathin films have been fabricated. In contrast to the uniform ASW films grown directly on the hydrophilic AlOx, water molecules adsorb on the hydrophobic Gly films in the form of 3D ASW clusters. This leads to significant differences in the NEXAFS and work function data obtained from ASW-on-AlOx and ASW-on-Gly films, respectively. Furthermore, these structural differences influence the chemical state of Gly molecules (neutral vs. zwitterionic) adsorbed on top of ASW films. N1s XPS measurements revealed an increased amount of neutral Gly molecules in the film top-deposited on the ASW-on-Gly structure in comparison to the neutral Gly in the films directly condensed on AlOx or grown on the ASW substrate. H2O TPD spectra demonstrate that the crystallization and desorption processes of ASW are affected in a different way by the Gly layers, top-deposited on to ASW-on-AlOx and ASW-on-Gly films. At the same time, Gly adlayers sink into the ASW film during crystallization/desorption of the latter and land softly on the alumina surface in the form of zwitterionic clusters.

The effect of grooves in amorphous substrates on the orientation of metal deposits. I - Carbon substrates

NASA Technical Reports Server (NTRS)

Anton, R.; Poppa, H.; Flanders, D. C.

1982-01-01

The graphoepitaxial alignment of vapor-deposited discrete metal crystallites is investigated in the nucleation and growth stages and during annealing by in situ UHV/TEM techniques. Various stages of nucleation, growth and coalescence of vapor deposits of Au, Ag, Pb, Sn, and Bi on amorphous, topographically structured C substrates are analyzed by advanced dark-field techniques to detect preferred local orientations. It is found that the topography-induced orientation of metal crystallites depends strongly on their mobility and their respective tendency to develop pronounced crystallographic shapes. Lowering of the average surface free energies and increasing the crystallographic surface energy anisotropies cause generally improved graphoepitaxial alignments.

Production and reactions of silicon atoms in hot wire deposition of amorphous silicon

NASA Astrophysics Data System (ADS)

Zheng, Wengang; Gallagher, Alan

2003-10-01

Decomposing silane and hydrogen molecules on a hot tungsten filament is an alternative method of depositing hydrogenated microcrystal and amorphous Si for thin-film semmiconductor devices. This "hot-wire" method can have significant advantages, such as high film deposition rates. The deposition chemistry involves Si and H atoms released from the filament, followed by their reactions with the vapor and surfaces. To establish these deposition pathways, we measure radicals at the substrate with a home built, threshold ionization mass spectrometer. The design and operation of this mass spectrometer for radical detection, and the behavior of Si atom production and reactions, will be presented. This work is supported by the National Renewable Energy Laboratory, Golden, CO 80401

Different amorphous solid-state forms of roxithromycin: A thermodynamic and morphological study.

PubMed

Milne, Marnus; Liebenberg, Wilna; Aucamp, Marique Elizabeth

2016-02-10

The striking impact that different preparation methods have on the characteristics of amorphous solid-state forms has attracted considerable attention during the last two decades. The pursuit of more extensive knowledge regarding polyamorphism therefore continues. The aim of this study was firstly, to investigate the influence of different preparation techniques to obtain amorphous solid-state forms for the same active pharmaceutical ingredient, namely roxithromycin. The preparation techniques also report on a method utilizing hot air, which although it is based on a melt intermediary step, is considered a novel preparation method. Secondly, to conduct an in-depth investigation into any physico-chemical differences between the resulting amorphous forms and thirdly, to bring our findings into context with that of previous work done, whilst simultaneously discussing a well-defined interpretation for the term polyamorphism and propose a discernment between true polyamorphism and pseudo-polyamorphism/atypical-polyamorphism. The preparation techniques included melt, solution, and a combination of solution-mechanical disruption as intermediary steps. The resulting amorphous forms were investigated using differential scanning calorimetry, X-ray powder diffraction, hot-stage microscopy, scanning electron microscopy, and vapor sorption. Clear and significant thermodynamic differences were determined between the four amorphous forms. It was also deduced from this study that different preparation techniques have a mentionable impact on the morphological properties of the resulting amorphous roxithromycin powders. Thermodynamic properties as well as the physical characteristics of the amorphous forms greatly governed other physico-chemical properties i.e. solubility and dissolution. Copyright © 2015 Elsevier B.V. All rights reserved.

Hybrid deposition of thin film solid oxide fuel cells and electrolyzers

DOEpatents

Jankowski, A.F.; Makowiecki, D.M.; Rambach, G.D.; Randich, E.

1998-05-19

The use of vapor deposition techniques enables synthesis of the basic components of a solid oxide fuel cell (SOFC); namely, the electrolyte layer, the two electrodes, and the electrolyte-electrode interfaces. Such vapor deposition techniques provide solutions to each of the three critical steps of material synthesis to produce a thin film solid oxide fuel cell (TFSOFC). The electrolyte is formed by reactive deposition of essentially any ion conducting oxide, such as defect free, yttria stabilized zirconia (YSZ) by planar magnetron sputtering. The electrodes are formed from ceramic powders sputter coated with an appropriate metal and sintered to a porous compact. The electrolyte-electrode interface is formed by chemical vapor deposition of zirconia compounds onto the porous electrodes to provide a dense, smooth surface on which to continue the growth of the defect-free electrolyte, whereby a single fuel cell or multiple cells may be fabricated. 8 figs.

Hybrid deposition of thin film solid oxide fuel cells and electrolyzers

DOEpatents

Jankowski, Alan F.; Makowiecki, Daniel M.; Rambach, Glenn D.; Randich, Erik

1999-01-01

The use of vapor deposition techniques enables synthesis of the basic components of a solid oxide fuel cell (SOFC); namely, the electrolyte layer, the two electrodes, and the electrolyte-electrode interfaces. Such vapor deposition techniques provide solutions to each of the three critical steps of material synthesis to produce a thin film solid oxide fuel cell (TFSOFC). The electrolyte is formed by reactive deposition of essentially any ion conducting oxide, such as defect free, yttria stabilized zirconia (YSZ) by planar magnetron sputtering. The electrodes are formed from ceramic powders sputter coated with an appropriate metal and sintered to a porous compact. The electrolyte-electrode interface is formed by chemical vapor deposition of zirconia compounds onto the porous electrodes to provide a dense, smooth surface on which to continue the growth of the defect-free electrolyte, whereby a single fuel cell or multiple cells may be fabricated.

Hybrid deposition of thin film solid oxide fuel cells and electrolyzers

DOEpatents

Jankowski, Alan F.; Makowiecki, Daniel M.; Rambach, Glenn D.; Randich, Erik

1998-01-01

The use of vapor deposition techniques enables synthesis of the basic components of a solid oxide fuel cell (SOFC); namely, the electrolyte layer, the two electrodes, and the electrolyte-electrode interfaces. Such vapor deposition techniques provide solutions to each of the three critical steps of material synthesis to produce a thin film solid oxide fuel cell (TFSOFC). The electrolyte is formed by reactive deposition of essentially any ion conducting oxide, such as defect free, yttria stabilized zirconia (YSZ) by planar magnetron sputtering. The electrodes are formed from ceramic powders sputter coated with an appropriate metal and sintered to a porous compact. The electrolyte-electrode interface is formed by chemical vapor deposition of zirconia compounds onto the porous electrodes to provide a dense, smooth surface on which to continue the growth of the defect-free electrolyte, whereby a single fuel cell or multiple cells may be fabricated.

Metal organic chemical vapor deposition of environmental barrier coatings for the inhibition of solid deposit formation from heated jet fuel

NASA Astrophysics Data System (ADS)

Mohan, Arun Ram

Solid deposit formation from jet fuel compromises the fuel handling system of an aviation turbine engine and increases the maintenance downtime of an aircraft. The deposit formation process depends upon the composition of the fuel, the nature of metal surfaces that come in contact with the heated fuel and the operating conditions of the engine. The objective of the study is to investigate the effect of substrate surfaces on the amount and nature of solid deposits in the intermediate regime where both autoxidation and pyrolysis play an important role in deposit formation. A particular focus has been directed to examining the effectiveness of barrier coatings produced by metal organic chemical vapor deposition (MOCVD) on metal surfaces for inhibiting the solid deposit formation from jet fuel degradation. In the first part of the experimental study, a commercial Jet-A sample was stressed in a flow reactor on seven different metal surfaces: AISI316, AISI 321, AISI 304, AISI 347, Inconel 600, Inconel 718, Inconel 750X and FecrAlloy. Examination of deposits by thermal and microscopic analysis shows that the solid deposit formation is influenced by the interaction of organosulfur compounds and autoxidation products with the metal surfaces. The nature of metal sulfides was predicted by Fe-Ni-S ternary phase diagram. Thermal stressing on uncoated surfaces produced coke deposits with varying degree of structural order. They are hydrogen-rich and structurally disordered deposits, spherulitic deposits, small carbon particles with relatively ordered structures and large platelets of ordered carbon structures formed by metal catalysis. In the second part of the study, environmental barrier coatings were deposited on tube surfaces to inhibit solid deposit formation from the heated fuel. A new CVD system was configured by the proper choice of components for mass flow, pressure and temperature control in the reactor. A bubbler was designed to deliver the precursor into the reactor

Moisture-Induced Amorphous Phase Separation of Amorphous Solid Dispersions: Molecular Mechanism, Microstructure, and Its Impact on Dissolution Performance.

PubMed

Chen, Huijun; Pui, Yipshu; Liu, Chengyu; Chen, Zhen; Su, Ching-Chiang; Hageman, Michael; Hussain, Munir; Haskell, Roy; Stefanski, Kevin; Foster, Kimberly; Gudmundsson, Olafur; Qian, Feng

2018-01-01

Amorphous phase separation (APS) is commonly observed in amorphous solid dispersions (ASD) when exposed to moisture. The objective of this study was to investigate: (1) the phase behavior of amorphous solid dispersions composed of a poorly water-soluble drug with extremely low crystallization propensity, BMS-817399, and PVP, following exposure to different relative humidity (RH), and (2) the impact of phase separation on the intrinsic dissolution rate of amorphous solid dispersion. Drug-polymer interaction was confirmed in ASDs at different drug loading using infrared (IR) spectroscopy and water vapor sorption analysis. It was found that the drug-polymer interaction could persist at low RH (≤75% RH) but was disrupted after exposure to high RH, with the advent of phase separation. Surface morphology and composition of 40/60 ASD at micro-/nano-scale before and after exposure to 95% RH were also compared. It was found that hydrophobic drug enriched on the surface of ASD after APS. However, for the 40/60 ASD system, the intrinsic dissolution rate of amorphous drug was hardly affected by the phase behavior of ASD, which may be partially attributed to the low crystallization tendency of amorphous BMS-817399 and enriched drug amount on the surface of ASD. Intrinsic dissolution rate of PVP decreased resulting from APS, leading to a lower concentration in the dissolution medium, but supersaturation maintenance was not anticipated to be altered after phase separation due to the limited ability of PVP to inhibit drug precipitation and prolong the supersaturation of drug in solution. This study indicated that for compounds with low crystallization propensity and high hydrophobicity, the risk of moisture-induced APS is high but such phase separation may not have profound impact on the drug dissolution performance of ASDs. Therefore, application of ASD technology on slow crystallizers could incur low risks not only in physical stability but also in dissolution performance

Characterization of melt-quenched and milled amorphous solids of gatifloxacin.

PubMed

Hattori, Yusuke; Suzuki, Ayumi; Otsuka, Makoto

2016-11-01

The objectives of this study were to characterize and investigate the differences in amorphous states of gatifloxacin. We prepared two types of gatifloxacin amorphous solids coded as M and MQ using milling and melt-quenching methods, respectively. The amorphous solids were characterized via X-ray diffraction (XRD), nonisothermal differential scanning calorimetry (DSC) and time-resolved near-infrared (NIR) spectroscopy. Both the solids displayed halo XRD patterns, the characteristic of amorphous solids; however, in the non-isothermal DSC profiles, these amorphous solids were distinguished by their crystallization and melting temperatures. The Kissinger-Akahira-Sunose plots of non-isothermal crystallization temperatures at various heating rates indicated a lower activation energy of crystallization for the amorphous solid M than that of MQ. These results support the differentiation between two amorphous states with different physical and chemical properties.

Long-term stable water vapor permeation barrier properties of SiN/SiCN/SiN nanolaminated multilayers grown by plasma-enhanced chemical vapor deposition at extremely low pressures

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

Choi, Bum Ho, E-mail: bhchoi@kitech.re.kr; Lee, Jong Ho

2014-08-04

We investigated the water vapor permeation barrier properties of 30-nm-thick SiN/SiCN/SiN nanolaminated multilayer structures grown by plasma enhanced chemical vapor deposition at 7 mTorr. The derived water vapor transmission rate was 1.12 × 10{sup −6} g/(m{sup 2} day) at 85 °C and 85% relative humidity, and this value was maintained up to 15 000 h of aging time. The X-ray diffraction patterns revealed that the nanolaminated film was composed of an amorphous phase. A mixed phase was observed upon performing high resolution transmission electron microscope analysis, which indicated that a thermodynamically stable structure was formed. It was revealed amorphous SiN/SiCN/SiN multilayer structures that are freemore » from intermixed interface defects effectively block water vapor permeation into active layer.« less

Solid-phase crystallization of amorphous Si films on glass and Si wafer

NASA Astrophysics Data System (ADS)

Lee, Dong Nyung

2011-11-01

When amorphous silicon films deposited on glass by physical or chemical vapor deposition are annealed, they undergo crystallization by nucleation and growth. The growth rate of Si crystallites is the highest in their <111> directions along or nearly along the film surface. The directed crystallization is likely to develop the <110>//ND or <111>//ND oriented Si crystallites. As the annealing temperature increases, the equiaxed crystallization increases, which in turn increases the random orientation. When amorphous Si is under a stress of the order of 0.1 GPa at about 540 °C, the tensile stress increases the growth rate of Si grains, whereas the compressive stress decreases the growth rate. However, the crystal growth rate increases with the increasing hydrostatic pressure, when the pressure is of the order of GPa at 530-540 °C. These phenomena have been discussed based on the directed crystallization model advanced before, which has been further elaborated.

Advanced deposition model for thermal activated chemical vapor deposition

NASA Astrophysics Data System (ADS)

Cai, Dang

Thermal Activated Chemical Vapor Deposition (TACVD) is defined as the formation of a stable solid product on a heated substrate surface from chemical reactions and/or dissociation of gaseous reactants in an activated environment. It has become an essential process for producing solid film, bulk material, coating, fibers, powders and monolithic components. Global market of CVD products has reached multi billions dollars for each year. In the recent years CVD process has been extensively used to manufacture semiconductors and other electronic components such as polysilicon, AlN and GaN. Extensive research effort has been directed to improve deposition quality and throughput. To obtain fast and high quality deposition, operational conditions such as temperature, pressure, fluid velocity and species concentration and geometry conditions such as source-substrate distance need to be well controlled in a CVD system. This thesis will focus on design of CVD processes through understanding the transport and reaction phenomena in the growth reactor. Since the in situ monitor is almost impossible for CVD reactor, many industrial resources have been expended to determine the optimum design by semi-empirical methods and trial-and-error procedures. This approach has allowed the achievement of improvements in the deposition sequence, but begins to show its limitations, as this method cannot always fulfill the more and more stringent specifications of the industry. To resolve this problem, numerical simulation is widely used in studying the growth techniques. The difficulty of numerical simulation of TACVD crystal growth process lies in the simulation of gas phase and surface reactions, especially the latter one, due to the fact that very limited kinetic information is available in the open literature. In this thesis, an advanced deposition model was developed to study the multi-component fluid flow, homogeneous gas phase reactions inside the reactor chamber, heterogeneous surface

Electron emission from chemical vapor deposited diamond and amorphous carbon films observed with a simple field emission device

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

Feng, Z.; Brown, I.G.; Ager, J.W. III

Electron emission from chemical vapor deposited (CVD) diamond and amorphous carbon (a-C) films was observed with a simple field emission device (FED). Both diamond and a-C films were prepared with microwave plasma-enhanced CVD techniques. Electron emission in the field strength range +10 to {minus}10 MVm{sup {minus}1} was studied, and the field emission source was confirmed by a diode characteristic of the {ital I}-{ital V} curve, a straight line in the Fowler--Nordheim (F-N) plot, and direct observation of light emission from a fluorescent screen. The turn-on field strength was {similar_to}5 MVm{sup {minus}1}, which was similar for both kinds of carbon films.more » The highest current density for diamond films, observed at a field strength of 10 MVm{sup {minus}1}, was {similar_to}15 {mu}A cm{sup {minus}2}. Diamond films yielded a higher emission current than a-C films. The reasons for the observed field emission are discussed.« less

Vapor-Deposited Glasses with Long-Range Columnar Liquid Crystalline Order

DOE PAGES

Gujral, Ankit; Gomez, Jaritza; Ruan, Shigang; ...

2017-10-04

Anisotropic molecular packing, particularly in highly ordered liquid crystalline arrangements, has the potential for optimizing performance in organic electronic and optoelectronic applications. Here we show that physical vapor deposition can be used to prepare highly organized glassy solids of discotic liquid crystalline systems. Using grazing incidence X-ray scattering, atomic force microscopy, and UV–vis spectroscopy, we compare three systems: a rectangular columnar liquid crystal, a hexagonal columnar liquid crystal, and a nonmesogen. The packing motifs accessible by vapor deposition are highly organized for the liquid crystalline systems with columns propagating either in-plane or out-of-plane depending upon the substrate temperature during deposition.more » As a result, the structures formed at a given substrate temperature can be understood as resulting from partial equilibration toward the structure of the equilibrium liquid crystal surface during the deposition process.« less

Vapor-Deposited Glasses with Long-Range Columnar Liquid Crystalline Order

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

Gujral, Ankit; Gomez, Jaritza; Ruan, Shigang

Anisotropic molecular packing, particularly in highly ordered liquid crystalline arrangements, has the potential for optimizing performance in organic electronic and optoelectronic applications. Here we show that physical vapor deposition can be used to prepare highly organized glassy solids of discotic liquid crystalline systems. Using grazing incidence X-ray scattering, atomic force microscopy, and UV–vis spectroscopy, we compare three systems: a rectangular columnar liquid crystal, a hexagonal columnar liquid crystal, and a nonmesogen. The packing motifs accessible by vapor deposition are highly organized for the liquid crystalline systems with columns propagating either in-plane or out-of-plane depending upon the substrate temperature during deposition.more » As a result, the structures formed at a given substrate temperature can be understood as resulting from partial equilibration toward the structure of the equilibrium liquid crystal surface during the deposition process.« less

Structure, growth kinetics, and ledge flow during vapor-solid-solid growth of copper-catalyzed silicon nanowires.

PubMed

Wen, C-Y; Reuter, M C; Tersoff, J; Stach, E A; Ross, F M

2010-02-10

We use real-time observations of the growth of copper-catalyzed silicon nanowires to determine the nanowire growth mechanism directly and to quantify the growth kinetics of individual wires. Nanowires were grown in a transmission electron microscope using chemical vapor deposition on a copper-coated Si substrate. We show that the initial reaction is the formation of a silicide, eta'-Cu(3)Si, and that this solid silicide remains on the wire tips during growth so that growth is by the vapor-solid-solid mechanism. Individual wire directions and growth rates are related to the details of orientation relation and catalyst shape, leading to a rich morphology compared to vapor-liquid-solid grown nanowires. Furthermore, growth occurs by ledge propagation at the silicide/silicon interface, and the ledge propagation kinetics suggest that the solubility of precursor atoms in the catalyst is small, which is relevant to the fabrication of abrupt heterojunctions in nanowires.

Influences of ultrathin amorphous buffer layers on GaAs/Si grown by metal-organic chemical vapor deposition

NASA Astrophysics Data System (ADS)

Hu, Haiyang; Wang, Jun; Cheng, Zhuo; Yang, Zeyuan; Yin, Haiying; Fan, Yibing; Ma, Xing; Huang, Yongqing; Ren, Xiaomin

2018-04-01

In this work, a technique for the growth of GaAs epilayers on Si, combining an ultrathin amorphous Si buffer layer and a three-step growth method, has been developed to achieve high crystalline quality for monolithic integration. The influences of the combined technique for the crystalline quality of GaAs on Si are researched in this article. The crystalline quality of GaAs epilayer on Si with the combined technique is investigated by scanning electron microscopy, double crystal X-ray diffraction (DCXRD), photoluminescence, and transmission electron microscopy measurements. By means of this technique, a 1.8-µm-thick high-quality GaAs/Si epilayer was grown by metal-organic chemical vapor deposition. The full-width at half-maximum of the DCXRD rocking curve in the (400) reflection obtained from the GaAs/Si epilayers is about 163 arcsec. Compared with only using three-step growth method, the current technique reduces etch pit density from 3 × 106 cm-2 to 1.5 × 105 cm-2. The results demonstrate that the combined technique is an effective approach for reducing dislocation density in GaAs epilayers on Si.

Effects of gas residence time of CH4/H2 on sp2 fraction of amorphous carbon films and dissociated methyl density during radical-injection plasma-enhanced chemical vapor deposition

NASA Astrophysics Data System (ADS)

Sugiura, Hirotsugu; Jia, Lingyun; Kondo, Hiroki; Ishikawa, Kenji; Tsutsumi, Takayoshi; Hayashi, Toshio; Takeda, Keigo; Sekine, Makoto; Hori, Masaru

2018-06-01

Quadruple mass spectrometric measurements of CH3 density during radical-injection plasma-enhanced chemical vapor deposition to consider the sp2 fraction of amorphous carbon (a-C) films were performed. The sp2 fraction of the a-C films reached a minimum of 46%, where the CH3 density was maximum for a residence time of 6 ms. The sp2 fraction of the a-C films was tailored with the gaseous phase CH3 density during the deposition. This knowledge is useful for understanding the formation mechanism of bonding structures in the a-C films, which enables the precise control of their electronic properties.

Vapor deposition routes to conformal polymer thin films

PubMed Central

Moni, Priya; Al-Obeidi, Ahmed

2017-01-01

Vapor phase syntheses, including parylene chemical vapor deposition (CVD) and initiated CVD, enable the deposition of conformal polymer thin films to benefit a diverse array of applications. This short review for nanotechnologists, including those new to vapor deposition methods, covers the basic theory in designing a conformal polymer film vapor deposition, sample preparation and imaging techniques to assess film conformality, and several applications that have benefited from vapor deposited, conformal polymer thin films. PMID:28487816

Small-angle neutron scattering study of micropore collapse in amorphous solid water.

PubMed

Mitterdorfer, Christian; Bauer, Marion; Youngs, Tristan G A; Bowron, Daniel T; Hill, Catherine R; Fraser, Helen J; Finney, John L; Loerting, Thomas

2014-08-14

Vapor-deposited amorphous solid water (ASW) is the most abundant solid molecular material in space, where it plays a direct role in both the formation of more complex chemical species and the aggregation of icy materials in the earliest stages of planet formation. Nevertheless, some of its low temperature physics such as the collapse of the micropore network upon heating are still far from being understood. Here we characterize the nature of the micropores and their collapse using neutron scattering of gram-quantities of D2O-ASW of internal surface areas up to 230 ± 10 m(2) g(-1) prepared at 77 K. The model-free interpretation of the small-angle scattering data suggests micropores, which remain stable up to 120-140 K and then experience a sudden collapse. The exact onset temperature to pore collapse depends on the type of flow conditions employed in the preparation of ASW and, thus, the specific surface area of the initial deposit, whereas the onset of crystallization to cubic ice is unaffected by the flow conditions. Analysis of the small-angle neutron scattering signal using the Guinier-Porod model suggests that a sudden transition from three-dimensional cylindrical pores with 15 Å radius of gyration to two-dimensional lamellae is the mechanism underlying the pore collapse. The rather high temperature of about 120-140 K of micropore collapse and the 3D-to-2D type of the transition unraveled in this study have implications for our understanding of the processing and evolution of ices in various astrophysical environments.

Vapor Wall Deposition in Chambers: Theoretical Considerations

NASA Astrophysics Data System (ADS)

McVay, R.; Cappa, C. D.; Seinfeld, J.

2014-12-01

In order to constrain the effects of vapor wall deposition on measured secondary organic aerosol (SOA) yields in laboratory chambers, Zhang et al. (2014) varied the seed aerosol surface area in toluene oxidation and observed a clear increase in the SOA yield with increasing seed surface area. Using a coupled vapor-particle dynamics model, we examine the extent to which this increase is the result of vapor wall deposition versus kinetic limitations arising from imperfect accommodation of organic species into the particle phase. We show that a seed surface area dependence of the SOA yield is present only when condensation of vapors onto particles is kinetically limited. The existence of kinetic limitation can be predicted by comparing the characteristic timescales of gas-phase reaction, vapor wall deposition, and gas-particle equilibration. The gas-particle equilibration timescale depends on the gas-particle accommodation coefficient αp. Regardless of the extent of kinetic limitation, vapor wall deposition depresses the SOA yield from that in its absence since vapor molecules that might otherwise condense on particles deposit on the walls. To accurately extrapolate chamber-derived yields to atmospheric conditions, both vapor wall deposition and kinetic limitations must be taken into account.

Dependence of electrical and optical properties of amorphous SiC:H thin films grown by rf plasma enhanced chemical vapor deposition on annealing temperature

NASA Astrophysics Data System (ADS)

Park, M. G.; Choi, W. S.; Hong, B.; Kim, Y. T.; Yoon, D. H.

2002-05-01

In this article, we investigated the dependence of optical and electrical properties of hydrogenated amorphous silicon carbide (a-SiC:H) films on annealing temperature (Ta) and radio frequency (rf) power. The substrate temperature (Ts) was 250 °C, the rf power was varied from 30 to 400 W, and the range of Ta was from 400 to 600 °C. The a-SiC:H films were deposited by using the plasma enhanced chemical vapor deposition system on Corning 7059 glasses and p-type Si (100) wafers with a SiH4+CH4 gas mixture. The experimental results have shown that the optical bandgap energy (Eg) of the a-SiC:H thin films changed little on the annealing temperature while Eg increased with the rf power. The Raman spectrum of the thin films annealed at high temperatures showed that graphitization of carbon clusters and microcrystalline silicon occurs. The current-voltage characteristics have shown good electrical properties in relation to the annealed films.

The preparation of in situ doped hydrogenated amorphous silicon by homogeneous chemical vapor deposition

NASA Astrophysics Data System (ADS)

Meyerson, B. S.; Scott, B. A.; Wolford, D. J.

1983-03-01

Raman scattering, infrared absorption, conductivity measurements, electron microprobe, and secondary ion mass spectrometry (SIMS) were used to characterize boron and phosphorus doped hydrogenated amorphous silicon (a-Si:H) films prepared by Homogeneous Chemical Vapor Deposition (HOMOCVD). HOMOCVD is a thermal process which relies upon the gas phase pyrolysis of a source (silane containing up to 1.0% diborane or phosphine) to generate activated species for deposition upon a cooled substrate. Doped films prepared at 275 °C by this process were found to contain ˜12-at. % hydrogen as determined by infrared absorption. We examined dopant incorporation from the gas phase, obtaining values for a distribution coefficient CD (film dopant content/gas phase dopant concentration, atomic basis) of 0.33≤CD ≤0.63 for boron, while 0.4≤CD ≤10.75 in the limits 3.3×10-5≤PH3/SiH4≤0.004. We interpret the data as indicative of the formation of an unstable phosphorus/silicon intermediate in the gas phase, leading to the observed enhancements in CD at high gas phase phosphine content. HOMOCVD films doped at least as efficiently as their prepared counterparts, but tended to achieve higher conductivities [σ≥0.1 (Ω cm)-1 for 4.0% incorporated phosphorus] in the limit of heavy doping. Raman spectra showed no evidence of crystallinity in the doped films. Film properties (conductivity, activation energy of of conduction) have not saturated at the doping levels investigated here, making the attainment of higher ``active'' dopant levels a possibility. We attribute the observation that HOMOCVD appears more amenable to high ``active'' dopant levels than plasma techniques to the low (˜0.1 eV) thermal energy at which HOMOCVD proceeds, versus ˜10-100 eV for plasma techniques. Low substrate temperature (75 °C) doped films were prepared with initial results showing these films to dope as readily as those prepared at high temperature (T˜275 °C).

Magnetomechanical coupling in thermal amorphous solids

NASA Astrophysics Data System (ADS)

Hentschel, H. George E.; Ilyin, Valery; Mondal, Chandana; Procaccia, Itamar

2018-05-01

Standard approaches to magnetomechanical interactions in thermal magnetic crystalline solids involve Landau functionals in which the lattice anisotropy and the resulting magnetization easy axes are taken explicitly into account. In glassy systems one needs to develop a theory in which the amorphous structure precludes the existence of an easy axis, and in which the constituent particles are free to respond to their local amorphous surroundings and the resulting forces. We present a theory of all the mixed responses of an amorphous solid to mechanical strains and magnetic fields. Atomistic models are proposed in which we test the predictions of magnetostriction for both bulk and nanofilm amorphous samples in the paramagnetic phase. The application to nanofilms with emergent self-affine free interfaces requires a careful definition of the film "width" and its change due to the magnetostriction effect.

High-Throughput Characterization of Vapor-Deposited Organic Glasses

NASA Astrophysics Data System (ADS)

Dalal, Shakeel S.

Glasses are non-equilibrium materials which on short timescales behave like solids, and on long timescales betray their liquid-like structure. The most common way of preparing a glass is to cool the liquid faster than it can structurally rearrange. Until recently, most preparation schemes for a glass were considered to result in materials with undifferentiable structure and properties. This thesis utilizes a particular preparation method, physical vapor deposition, in order to prepare glasses of organic molecules with properties otherwise considered to be unobtainable. The glasses are characterized using spectroscopic ellipsometry, both as a dilatometric technique and as a reporter of molecular packing. The results reported here develop ellipsometry as a dilatometric technique on a pair of model glass formers, alpha,alpha,beta-trisnaphthylbenzene and indomethacin. It is found that the molecular orientation, as measured by birefringence, can be tuned by changing the substrate temperature during the deposition. In order to efficiently characterize the properties of vapor-deposited indomethacin as a function of substrate temperature, a high-throughput method is developed to capture the entire interesting range of substrate temperatures in just a few experiments. This high-throughput method is then leveraged to describe molecular mobility in vapor-deposited indomethacin. It is also used to demonstrate that the behavior of organic semiconducting molecules agrees with indomethacin quantitatively, and this agreement has implications for emerging technologies such as light-emitting diodes, photovoltaics and thin-film transistors made from organic molecules.

Deposition of amorphous silicon using a tubular reactor with concentric-electrode confinement

NASA Astrophysics Data System (ADS)

Conde, J. P.; Chan, K. K.; Blum, J. M.; Arienzo, M.; Cuomo, J. J.

1992-04-01

High-quality, hydrogenated amorphous silicon (a-Si:H) is deposited at room temperature by rf glow discharge at a high deposition rate using a tubular reactor with cylindrical symmetry (concentric-electrode plasma-enhanced chemical vapor deposition, CE-PECVD). Using the novel CE-PECVD design, room-temperature deposition of a-Si:H with growth rates up to 14 Å s-1, low hydrogen concentration (≲10%), and the bonded hydrogen in the Si-H monohydride configuration, is achieved for the first time using an rf glow-discharge technique. The influence of the deposition parameters (silane flow rate, pressure, and power density) on the growth rate, optical band gap, and silicon-hydrogen bonding configuration, is quantitatively predicted using a deposition mechanism based on the additive contribution of three growth precursors, SiH2, SiH3, and Si2H6, with decreasing sticking coefficients of 0.7, 0.1, and 0.001, respectively. The low hydrogen concentration is due to the enhanced ion bombardment resulting from the concentric electrode design.

Preparation Of Sources For Plasma Vapor Deposition

NASA Technical Reports Server (NTRS)

Waters, William J.; Sliney, Hal; Kowalski, D.

1993-01-01

Multicomponent metal targets serving as sources of vapor for plasma vapor deposition made in modified pressureless-sintering process. By use of targets made in modified process, one coats components with materials previously plasma-sprayed or sintered but not plasma-vapor-deposited.

One step growth of GaN/SiO2 core/shell nanowire in vapor-liquid-solid route by chemical vapor deposition technique

NASA Astrophysics Data System (ADS)

Barick, B. K.; Yadav, Shivesh; Dhar, S.

2017-11-01

GaN/SiO2 core/shell nanowires are grown by cobalt phthalocyanine catalyst assisted vapor-liquid-solid route, in which Si wafer coated with a mixture of gallium and indium is used as the source for Ga and Si and ammonia is used as the precursor for nitrogen and hydrogen. Gallium in the presence of indium and hydrogen, which results from the dissociation of ammonia, forms Si-Ga-In alloy at the growth temperature ∼910 °C. This alloy acts as the source of Si, Ga and In. A detailed study using a variety of characterization tools reveals that these wires, which are several tens of micron long, has a diameter distribution of the core ranging from 20 to 50 nm, while the thickness of the amorphous SiO2 shell layer is about 10 nm. These wires grow along [ 1 0 1 bar 0 ] direction. It has also been observed that the average diameter of these wires decreases, while their density increases as the gallium proportion in the Ga-In mixture is increased.

A review-application of physical vapor deposition (PVD) and related methods in the textile industry

NASA Astrophysics Data System (ADS)

Shahidi, Sheila; Moazzenchi, Bahareh; Ghoranneviss, Mahmood

2015-09-01

Physical vapor deposition (PVD) is a coating process in which thin films are deposited by the condensation of a vaporized form of the desired film material onto the substrate. The PVD process is carried out in a vacuum. PVD processes include different types, such as: cathode arc deposition, electron beam physical vapor deposition, evaporative deposition, sputtering, ion plating and enhanced sputtering. In the PVD method, the solid coating material is evaporated by heat or by bombardment with ions (sputtering). At the same time, a reactive gas is also introduced; it forms a compound with the metal vapor and is deposited on the substrate as a thin film with highly adherent coating. Such coatings are used in a wide range of applications such as aerospace, automotive, surgical, medical, dyes and molds for all manner of material processing, cutting tools, firearms, optics, thin films and textiles. The objective of this work is to give a comprehensive description and review of the science and technology related to physical vapor deposition with particular emphasis on their potential use in the textile industry. Physical vapor deposition has opened up new possibilities in the modification of textile materials and is an exciting prospect for usage in textile design and technical textiles. The basic principle of PVD is explained and the major applications, particularly sputter coatings in the modification and functionalization of textiles, are introduced in this research.

Critical detonation thickness in vapor-deposited hexanitroazobenzene (HNAB) films with different preparation conditions

NASA Astrophysics Data System (ADS)

Tappan, Alexander; Knepper, Robert; Marquez, Michael; Ball, J.; Miller, Jill

2013-06-01

At Sandia National Laboratories, we have coined the term ``microenergetics'' to describe sub-millimeter energetic material studies aimed at gaining knowledge of combustion and detonation behavior at the mesoscale. Films of the high explosive hexanitroazobenzene (HNAB) have been deposited through physical vapor deposition. HNAB deposits in an amorphous state that crystallizes over time and modest heating accelerates this crystallization. HNAB films were prepared under different crystallization temperatures, and characterized with surface profilometry and scanning electron microscopy. The critical detonation thickness for HNAB at different crystallization conditions was determined in a configuration where charge width was large compared to film thickness, and thus side losses did not play a role in detonation propagation. The results of these experiments will be discussed in the context of small sample geometry, deposited film morphology, crystal structure, and density.

Polymeric Amorphous Solid Dispersions: A Review of Amorphization, Crystallization, Stabilization, Solid-State Characterization, and Aqueous Solubilization of Biopharmaceutical Classification System Class II Drugs.

PubMed

Baghel, Shrawan; Cathcart, Helen; O'Reilly, Niall J

2016-09-01

Poor water solubility of many drugs has emerged as one of the major challenges in the pharmaceutical world. Polymer-based amorphous solid dispersions have been considered as the major advancement in overcoming limited aqueous solubility and oral absorption issues. The principle drawback of this approach is that they can lack necessary stability and revert to the crystalline form on storage. Significant upfront development is, therefore, required to generate stable amorphous formulations. A thorough understanding of the processes occurring at a molecular level is imperative for the rational design of amorphous solid dispersion products. This review attempts to address the critical molecular and thermodynamic aspects governing the physicochemical properties of such systems. A brief introduction to Biopharmaceutical Classification System, solid dispersions, glass transition, and solubility advantage of amorphous drugs is provided. The objective of this review is to weigh the current understanding of solid dispersion chemistry and to critically review the theoretical, technical, and molecular aspects of solid dispersions (amorphization and crystallization) and potential advantage of polymers (stabilization and solubilization) as inert, hydrophilic, pharmaceutical carrier matrices. In addition, different preformulation tools for the rational selection of polymers, state-of-the-art techniques for preparation and characterization of polymeric amorphous solid dispersions, and drug supersaturation in gastric media are also discussed. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Design of Amorphous Manganese Oxide@Multiwalled Carbon Nanotube Fiber for Robust Solid-State Supercapacitor.

PubMed

Shi, Peipei; Li, Li; Hua, Li; Qian, Qianqian; Wang, Pengfei; Zhou, Jinyuan; Sun, Gengzhi; Huang, Wei

2017-01-24

Solid-state fiber-based supercapacitors have been considered promising energy storage devices for wearable electronics due to their lightweight and amenability to be woven into textiles. Efforts have been made to fabricate a high performance fiber electrode by depositing pseudocapacitive materials on the outer surface of carbonaceous fiber, for example, crystalline manganese oxide/multiwalled carbon nanotubes (MnO 2 /MWCNTs). However, a key challenge remaining is to achieve high specific capacitance and energy density without compromising the high rate capability and cycling stability. In addition, amorphous MnO 2 is actually preferred due to its disordered structure and has been proven to exhibit superior electrochemical performance over the crystalline one. Herein, by incorporating amorphous MnO 2 onto a well-aligned MWCNT sheet followed by twisting, we design an amorphous MnO 2 @MWCNT fiber, in which amorphous MnO 2 nanoparticles are distributed in MWCNT fiber uniformly. The proposed structure gives the amorphous MnO 2 @MWCNT fiber good mechanical reliability, high electrical conductivity, and fast ion-diffusion. Solid-state supercapacitor based on amorphous MnO 2 @MWCNT fibers exhibits improved energy density, superior rate capability, exceptional cycling stability, and excellent flexibility. This study provides a strategy to design a high performance fiber electrode with microstructure control for wearable energy storage devices.

What controls deposition rate in electron-beam chemical vapor deposition?

PubMed

White, William B; Rykaczewski, Konrad; Fedorov, Andrei G

2006-08-25

The key physical processes governing electron-beam-assisted chemical vapor deposition are analyzed via a combination of theoretical modeling and supporting experiments. The scaling laws that define growth of the nanoscale deposits are developed and verified using carefully designed experiments of carbon deposition from methane onto a silicon substrate. The results suggest that the chamber-scale continuous transport of the precursor gas is the rate controlling process in electron-beam chemical vapor deposition.

Vapor Deposition Rig

NASA Image and Video Library

2015-01-27

The Plasma Spray-Physical Vapor Deposition (PS-PVD) Rig at NASA Glenn Research Center. The rig helps develop coatings for next-generation aircraft turbine components and create more efficient engines.

Metal (Ag/Ti)-Containing Hydrogenated Amorphous Carbon Nanocomposite Films with Enhanced Nanoscratch Resistance: Hybrid PECVD/PVD System and Microstructural Characteristics.

PubMed

Constantinou, Marios; Nikolaou, Petros; Koutsokeras, Loukas; Avgeropoulos, Apostolos; Moschovas, Dimitrios; Varotsis, Constantinos; Patsalas, Panos; Kelires, Pantelis; Constantinides, Georgios

2018-03-30

This study aimed to develop hydrogenated amorphous carbon thin films with embedded metallic nanoparticles (a-C:H:Me) of controlled size and concentration. Towards this end, a novel hybrid deposition system is presented that uses a combination of Plasma Enhanced Chemical Vapor Deposition (PECVD) and Physical Vapor Deposition (PVD) technologies. The a-C:H matrix was deposited through the acceleration of carbon ions generated through a radio-frequency (RF) plasma source by cracking methane, whereas metallic nanoparticles were generated and deposited using terminated gas condensation (TGC) technology. The resulting material was a hydrogenated amorphous carbon film with controlled physical properties and evenly dispersed metallic nanoparticles (here Ag or Ti). The physical, chemical, morphological and mechanical characteristics of the films were investigated through X-ray reflectivity (XRR), Raman spectroscopy, Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), Transmission Electron Microscopy (TEM) and nanoscratch testing. The resulting amorphous carbon metal nanocomposite films (a-C:H:Ag and a-C:H:Ti) exhibited enhanced nanoscratch resistance (up to +50%) and low values of friction coefficient (<0.05), properties desirable for protective coatings and/or solid lubricant applications. The ability to form nanocomposite structures with tunable coating performance by potentially controlling the carbon bonding, hydrogen content, and the type/size/percent of metallic nanoparticles opens new avenues for a broad range of applications in which mechanical, physical, biological and/or combinatorial properties are required.

Recrystallization of nifedipine and felodipine from amorphous molecular level solid dispersions containing poly(vinylpyrrolidone) and sorbed water.

PubMed

Marsac, Patrick J; Konno, Hajime; Rumondor, Alfred C F; Taylor, Lynne S

2008-03-01

To compare the physical stability of amorphous molecular level solid dispersions of nifedipine and felodipine, in the presence of poly(vinylpyrrolidone) (PVP) and small amounts of moisture. Thin amorphous films of nifedipine and felodipine and amorphous molecular level solid dispersions with PVP were stored at various relative humidities (RH) and the nucleation rate was measured. The amount of water sorbed at each RH was measured using isothermal vapor sorption and glass transition temperatures (Tg) were determined using differential scanning calorimetry. The solubility of each compound in methyl pyrrolidone was measured as a function of water content. Nifedipine crystallizes more easily than felodipine at any given polymer concentration and in the presence of moisture. The glass transition temperatures of each compound, alone and in the presence of PVP, are statistically equivalent at any given water content. The nifedipine systems are significantly more hygroscopic than the corresponding felodipine systems. Variations in the physical stability of the two compounds could not be explained by differences in Tg. However, the relative physical stability is consistent with differences in the degree of supersaturation of each drug in the solid dispersion, treating the polymer and water as a co-solvent system for each drug compound.

Chemical vapor deposition growth

NASA Technical Reports Server (NTRS)

Ruth, R. P.; Manasevit, H. M.; Kenty, J. L.; Moudy, L. A.; Simpson, W. I.; Yang, J. J.

1976-01-01

A chemical vapor deposition (CVD) reactor system with a vertical deposition chamber was used for the growth of Si films on glass, glass-ceramic, and polycrystalline ceramic substrates. Silicon vapor was produced by pyrolysis of SiH4 in a H2 or He carrier gas. Preliminary deposition experiments with two of the available glasses were not encouraging. Moderately encouraging results, however, were obtained with fired polycrystalline alumina substrates, which were used for Si deposition at temperatures above 1,000 C. The surfaces of both the substrates and the films were characterized by X-ray diffraction, reflection electron diffraction, scanning electron microscopy optical microscopy, and surface profilometric techniques. Several experiments were conducted to establish baseline performance data for the reactor system, including temperature distributions on the sample pedestal, effects of carrier gas flow rate on temperature and film thickness, and Si film growth rate as a function of temperature.

Vapor deposition of hardened niobium

DOEpatents

Blocher, Jr., John M.; Veigel, Neil D.; Landrigan, Richard B.

1983-04-19

A method of coating ceramic nuclear fuel particles containing a major amount of an actinide ceramic in which the particles are placed in a fluidized bed maintained at ca. 800.degree. to ca. 900.degree. C., and niobium pentachloride vapor and carbon tetrachloride vapor are led into the bed, whereby niobium metal is deposited on the particles and carbon is deposited interstitially within the niobium. Coating apparatus used in the method is also disclosed.

Amorphous alumina thin films deposited on titanium: Interfacial chemistry and thermal oxidation barrier properties

DOE PAGES

Baggetto, Loic; Charvillat, Cedric; Thebault, Yannick; ...

2015-12-02

Ti/Al 2O 3 bilayer stacks are used as model systems to investigate the role of atomic layer deposition (ALD) and chemical vapor deposition (CVD) to prepare 30-180 nm thick amorphous alumina films as protective barriers for the medium temperature oxidation (500-600⁰C) of titanium, which is employed in aeronautic applications. X-ray diffraction (XRD), transmission electron microscopy (TEM) with selected area electron diffraction (SAED), and X-ray photoelectron spectroscopy (XPS) results show that the films produced from the direct liquid injection (DLI) CVD of aluminum tri-isopropoxide (ATI) are poor oxygen barriers. The films processed using the ALD of trimethylaluminum (TMA) show good barriermore » properties but an extensive intermixing with Ti which subsequently oxidizes. In contrast, the films prepared from dimethyl aluminum isopropoxide (DMAI) by CVD are excellent oxygen barriers and show little intermixing with Ti. Overall, these measurements correlate the effect of the alumina coating thickness, morphology, and stoichiometry resulting from the preparation method to the oxidation barrier properties, and show that compact and stoichiometric amorphous alumina films offer superior barrier properties.« less

Modeling physical vapor deposition of energetic materials

DOE PAGES

Shirvan, Koroush; Forrest, Eric C.

2018-03-28

Morphology and microstructure of organic explosive films formed using physical vapor deposition (PVD) processes strongly depends on local surface temperature during deposition. Currently, there is no accurate means of quantifying the local surface temperature during PVD processes in the deposition chambers. This study focuses on using a multiphysics computational fluid dynamics tool, STARCCM+, to simulate pentaerythritol tetranitrate (PETN) deposition. The PETN vapor and solid phase were simulated using the volume of fluid method and its deposition in the vacuum chamber on spinning silicon wafers was modeled. The model also included the spinning copper cooling block where the wafers are placedmore » along with the chiller operating with forced convection refrigerant. Implicit time-dependent simulations in two- and three-dimensional were performed to derive insights in the governing physics for PETN thin film formation. PETN is deposited at the rate of 14 nm/s at 142.9 °C on a wafer with an initial temperature of 22 °C. The deposition of PETN on the wafers was calculated at an assumed heat transfer coefficient (HTC) of 400 W/m 2 K. This HTC proved to be the most sensitive parameter in determining the local surface temperature during deposition. Previous experimental work found noticeable microstructural changes with 0.5 mm fused silica wafers in place of silicon during the PETN deposition. This work showed that fused silica slows initial wafer cool down and results in ~10 °C difference for the surface temperature at 500 μm PETN film thickness. It was also found that the deposition surface temperature is insensitive to the cooling power of the copper block due to the copper block's very large heat capacity and thermal conductivity relative to the heat input from the PVD process. Future work should incorporate the addition of local stress during PETN deposition. Lastly, based on simulation results, it is also recommended to investigate the impact of wafer

Modeling physical vapor deposition of energetic materials

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

Shirvan, Koroush; Forrest, Eric C.

Morphology and microstructure of organic explosive films formed using physical vapor deposition (PVD) processes strongly depends on local surface temperature during deposition. Currently, there is no accurate means of quantifying the local surface temperature during PVD processes in the deposition chambers. This study focuses on using a multiphysics computational fluid dynamics tool, STARCCM+, to simulate pentaerythritol tetranitrate (PETN) deposition. The PETN vapor and solid phase were simulated using the volume of fluid method and its deposition in the vacuum chamber on spinning silicon wafers was modeled. The model also included the spinning copper cooling block where the wafers are placedmore » along with the chiller operating with forced convection refrigerant. Implicit time-dependent simulations in two- and three-dimensional were performed to derive insights in the governing physics for PETN thin film formation. PETN is deposited at the rate of 14 nm/s at 142.9 °C on a wafer with an initial temperature of 22 °C. The deposition of PETN on the wafers was calculated at an assumed heat transfer coefficient (HTC) of 400 W/m 2 K. This HTC proved to be the most sensitive parameter in determining the local surface temperature during deposition. Previous experimental work found noticeable microstructural changes with 0.5 mm fused silica wafers in place of silicon during the PETN deposition. This work showed that fused silica slows initial wafer cool down and results in ~10 °C difference for the surface temperature at 500 μm PETN film thickness. It was also found that the deposition surface temperature is insensitive to the cooling power of the copper block due to the copper block's very large heat capacity and thermal conductivity relative to the heat input from the PVD process. Future work should incorporate the addition of local stress during PETN deposition. Lastly, based on simulation results, it is also recommended to investigate the impact of wafer

Vacuum vapor deposition

NASA Technical Reports Server (NTRS)

Poorman, Richard M. (Inventor); Weeks, Jack L. (Inventor)

1995-01-01

A method and apparatus is described for vapor deposition of a thin metallic film utilizing an ionized gas arc directed onto a source material spaced from a substrate to be coated in a substantial vacuum while providing a pressure differential between the source and the substrate so that, as a portion of the source is vaporized, the vapors are carried to the substrate. The apparatus includes a modified tungsten arc welding torch having a hollow electrode through which a gas, preferably inert, flows and an arc is struck between the electrode and the source. The torch, source, and substrate are confined within a chamber within which a vacuum is drawn. When the arc is struck, a portion of the source is vaporized and the vapors flow rapidly toward the substrate. A reflecting shield is positioned about the torch above the electrode and the source to ensure that the arc is struck between the electrode and the source at startup. The electrode and the source may be confined within a vapor guide housing having a duct opening toward the substrate for directing the vapors onto the substrate.

Deformation-induced localized solid-state amorphization in nanocrystalline nickel.

PubMed

Han, Shuang; Zhao, Lei; Jiang, Qing; Lian, Jianshe

2012-01-01

Although amorphous structures have been widely obtained in various multi-component metallic alloys, amorphization in pure metals has seldom been observed and remains a long-standing scientific curiosity and technological interest. Here we present experimental evidence of localized solid-state amorphization in bulk nanocrystalline nickel introduced by quasi-static compression at room temperature. High-resolution electron microscope observations illustrate that nano-scale amorphous structures present at the regions where severe deformation occurred, e.g. along crack paths or surrounding nano-voids. These findings have indicated that nanocrystalline structures are highly desirable for promoting solid-state amorphization, which may provide new insights for understanding the nature of the crystalline-to-amorphous transformation and suggested a potential method to produce elemental metallic glasses that have hardly been available hitherto through rapid solidification.

Deformation-induced localized solid-state amorphization in nanocrystalline nickel

PubMed Central

Han, Shuang; Zhao, Lei; Jiang, Qing; Lian, Jianshe

2012-01-01

Although amorphous structures have been widely obtained in various multi-component metallic alloys, amorphization in pure metals has seldom been observed and remains a long-standing scientific curiosity and technological interest. Here we present experimental evidence of localized solid-state amorphization in bulk nanocrystalline nickel introduced by quasi-static compression at room temperature. High-resolution electron microscope observations illustrate that nano-scale amorphous structures present at the regions where severe deformation occurred, e.g. along crack paths or surrounding nano-voids. These findings have indicated that nanocrystalline structures are highly desirable for promoting solid-state amorphization, which may provide new insights for understanding the nature of the crystalline-to-amorphous transformation and suggested a potential method to produce elemental metallic glasses that have hardly been available hitherto through rapid solidification. PMID:22768383

Structural properties of nitrogenated amorphous carbon films: Influence of deposition temperature and radiofrequency discharge power

NASA Astrophysics Data System (ADS)

Lazar, G.; Bouchet-Fabre, B.; Zellama, K.; Clin, M.; Ballutaud, D.; Godet, C.

2008-10-01

The structural properties of nitrogenated amorphous carbon deposited by radiofrequency magnetron sputtering of graphite in pure N2 plasma are investigated as a function of the substrate temperature and radiofrequency discharge power. The film composition is derived from x-ray photoemission spectroscopy, nuclear reaction analysis and elastic recoil detection measurements and the film microstructure is discussed using infrared, Raman, x-ray photoemission and near edge x-ray absorption fine structure spectroscopic results. At low deposition temperature and low radiofrequency power, the films are soft, porous, and easily contaminated with water vapor and other atmospheric components. The concentration of nitrogen in the films is very large for low deposition temperatures (˜33.6at.% N at 150°C) but decreases strongly when the synthesis temperature increases (˜15at.% N at 450°C). With increasing deposition temperature and discharge power values, the main observed effects in amorphous carbon nitride alloys are a loss of nitrogen atoms, a smaller hydrogen and oxygen contamination related to the film densification, an increased order of the aromatic sp2 phase, and a strong change in the nitrogen distribution within the carbon matrix. Structural changes are well correlated with modifications of the optical and transport properties.

Highly patterned growth of SnO2 nanowires using a sub-atmospheric vapor-liquid-solid deposition

NASA Astrophysics Data System (ADS)

Akbari, M.; Mohajerzadeh, S.

2017-08-01

We report the realization of tin-oxide nanowires on patterned structures using a vapor-liquid-solid (VLS) process. While gold acts as the catalyst for the growth of wires, a tin-oxide containing sol-gel solution is spin coated on silicon substrate to act as the source for SnO vapor. The growth of tin-oxide nano-structures occurs mostly at the vicinity of the pre-deposited solution. By patterning the gold as the catalyst material, one is able to observe the growth at desired places. The growth of nanowires is highly dense within 100 µm away from such in situ source and their length is of the order of 5 µm. By further distancing from the source, the growth becomes more limited and nanowires become shorter and more sparsely distributed. The growth of nanowires has been studied using scanning and transmission electron microscopy tools while their composition has been investigated using XRD and EDS analyses. As a novel application, we have employed the grown nanowires as electron detection elements to measure the emitted electrons from electron sources. This configuration can be further used as electron detectors for scanning electron microscopes.

Microspheres for the growth of silicon nanowires via vapor-liquid-solid mechanism

DOE PAGES

Gomez-Martinez, Arancha; Marquez, Francisco; Elizalde, Eduardo; ...

2014-01-01

Silicon nanowires have been synthesized by a simple process using a suitable support containing silica and carbon microspheres. Nanowires were grown by thermal chemical vapor deposition via a vapor-liquid-solid mechanism with only the substrate as silicon source. The curved surface of the microsized spheres allows arranging the gold catalyst as nanoparticles with appropriate dimensions to catalyze the growth of nanowires. Here, the resulting material is composed of the microspheres with the silicon nanowires attached on their surface.

Study of Polymer Crystallization by Physical Vapor Deposition

NASA Astrophysics Data System (ADS)

Jeong, Hyuncheol

When a polymer is confined under the submicron length scale, confinement size and interfaces can significantly impact the crystallization kinetics and resulting morphology. The ability to tune the morphology of confined polymer systems is of critical importance for the development of high-performance polymer microelectronics. The wisdom from the research on confined crystallization suggests that it would be beneficial to have a processing route in which the crystallization of polymers is driven by interface and temperature effects at a nanometer-scale confinement. In practice, for atomic and small-molecular systems, physical vapor deposition (PVD) has been recognized as the most successful processing route for the precise control of the film structure at surface utilizing confinement effects. While standard PVD technologies are not generally applicable to the deposition of the chemically fragile macromolecules, the development of matrix-assisted pulsed laser evaporation (MAPLE) now enables the non-destructive PVD of high-molecular weight polymers. In this thesis work, we investigated the use of MAPLE for the precise control of the crystallization of polymer films at a molecular level. We also sought to decipher the rules governing the crystallization of confined polymers, by using MAPLE as a tool to form confined polymer systems onto substrates with a controlled temperature. We first explored the early stages of film growth and crystallization of poly(ethylene oxide) (PEO) at the substrate surface formed by MAPLE. The unique mechanism of film formation in MAPLE, the deposition of submicron-sized polymer droplets, allowed for the manifestation of confinement and substrate effects in the crystallization of MAPLE-deposited PEO. Furthermore, we also focused on the property of the amorphous PEO film formed by MAPLE, showing the dependence of polymer crystallization kinetics on the thermal history of the amorphous phase. Lastly, we probed how MAPLE processing affected

Boron nitride microfibers grown by plasma-assisted laser chemical vapor deposition without a metal catalyst

NASA Astrophysics Data System (ADS)

Komatsu, Shojiro; Kazami, Daisuke; Tanaka, Hironori; Shimizu, Yoshiki; Moriyoshi, Yusuke; Shiratani, Masaharu; Okada, Katsuyuki

2006-04-01

Boron nitride fibers were found to grow on polycrystalline nickel and Si (100) substrates by plasma-assisted laser chemical vapor deposition from B2H6+NH3 using an excimer laser at 193nm. Their diameter was typically a few hundreds of nanometers, while the length was a few tens of micrometers. They were stoichiometric or boron-rich BN in chemical composition. When the substrate was rotated during deposition, spiral fibers were found to grow. We conclude that they grew with the help of laser light by other than the vapor - liquid - solid mechanism.

Solid-state flat panel imager with avalanche amorphous selenium

NASA Astrophysics Data System (ADS)

Scheuermann, James R.; Howansky, Adrian; Goldan, Amir H.; Tousignant, Olivier; Levéille, Sébastien; Tanioka, K.; Zhao, Wei

2016-03-01

Active matrix flat panel imagers (AMFPI) have become the dominant detector technology for digital radiography and fluoroscopy. For low dose imaging, electronic noise from the amorphous silicon thin film transistor (TFT) array degrades imaging performance. We have fabricated the first prototype solid-state AMFPI using a uniform layer of avalanche amorphous selenium (a-Se) photoconductor to amplify the signal to eliminate the effect of electronic noise. We have previously developed a large area solid-state avalanche a-Se sensor structure referred to as High Gain Avalanche Rushing Photoconductor (HARP) capable of achieving gains of 75. In this work we successfully deposited this HARP structure onto a 24 x 30 cm2 TFT array with a pixel pitch of 85 μm. An electric field (ESe) up to 105 Vμm-1 was applied across the a-Se layer without breakdown. Using the HARP layer as a direct detector, an X-ray avalanche gain of 15 +/- 3 was achieved at ESe = 105 Vμm-1. In indirect mode with a 150 μm thick structured CsI scintillator, an optical gain of 76 +/- 5 was measured at ESe = 105 Vμm-1. Image quality at low dose increases with the avalanche gain until the electronic noise is overcome at a constant exposure level of 0.76 mR. We demonstrate the success of a solid-state HARP X-ray imager as well as the largest active area HARP sensor to date.

Plasma deposition of amorphous silicon carbide thin films irradiated with neutrons

NASA Astrophysics Data System (ADS)

Huran, J.; Bohacek, P.; Kucera, M.; Kleinova, A.; Sasinkova, V.; IEE SAS, Bratislava, Slovakia Team; Polymer Institute, SAS, Bratislava, Slovakia Team; Institute of Chemistry, SAS, Bratislava, Slovakia Team

2015-09-01

Amorphous silicon carbide and N-doped silicon carbide thin films were deposited on P-type Si(100) wafer by plasma enhanced chemical vapor deposition (PECVD) technology using silane, methane, ammonium and argon gases. The concentration of elements in the films was determined by RBS and ERDA method. Chemical compositions were analyzed by FTIR spectroscopy. Photoluminescence properties were studied by photoluminescence spectroscopy (PL). Irradiation of samples with various neutron fluencies was performed at room temperature. The films contain silicon, carbon, hydrogen, nitrogen and small amount of oxygen. From the IR spectra, the films contained Si-C, Si-H, C-H, Si-N, N-H and Si-O bonds. No significance effect on the IR spectra after neutron irradiation was observed. PL spectroscopy results of films showed decreasing PL intensity after neutron irradiation and PL intensity decreased with increased neutron fluencies. The measured current of the prepared structures increased after irradiation with neutrons and rise up with neutron fluencies.

Physical Vapor Deposition of Thin Films

NASA Astrophysics Data System (ADS)

Mahan, John E.

2000-01-01

A unified treatment of the theories, data, and technologies underlying physical vapor deposition methods With electronic, optical, and magnetic coating technologies increasingly dominating manufacturing in the high-tech industries, there is a growing need for expertise in physical vapor deposition of thin films. This important new work provides researchers and engineers in this field with the information they need to tackle thin film processes in the real world. Presenting a cohesive, thoroughly developed treatment of both fundamental and applied topics, Physical Vapor Deposition of Thin Films incorporates many critical results from across the literature as it imparts a working knowledge of a variety of present-day techniques. Numerous worked examples, extensive references, and more than 100 illustrations and photographs accompany coverage of: * Thermal evaporation, sputtering, and pulsed laser deposition techniques * Key theories and phenomena, including the kinetic theory of gases, adsorption and condensation, high-vacuum pumping dynamics, and sputtering discharges * Trends in sputter yield data and a new simplified collisional model of sputter yield for pure element targets * Quantitative models for film deposition rate, thickness profiles, and thermalization of the sputtered beam

Scaling behavior of columnar structure during physical vapor deposition

NASA Astrophysics Data System (ADS)

Meese, W. J.; Lu, T.-M.

2018-02-01

The statistical effects of different conditions in physical vapor deposition, such as sputter deposition, have on thin film morphology has long been the subject of interest. One notable effect is that of column development due to differential chamber pressure in the well-known empirical model called the Thornton's Structure Zone Model. The model is qualitative in nature and theoretical understanding with quantitative predictions of the morphology is still lacking due, in part, to the absence of a quantitative description of the incident flux distribution on the growth front. In this work, we propose an incident Gaussian flux model developed from a series of binary hard-sphere collisions and simulate its effects using Monte Carlo methods and a solid-on-solid growth scheme. We also propose an approximate cosine-power distribution for faster Monte Carlo sampling. With this model, it is observed that higher chamber pressures widen the average deposition angle, and similarly increase the growth of column diameters (or lateral correlation length) and the column-to-column separation (film surface wavelength). We treat both the column diameter and the surface wavelength as power laws. It is seen that both the column diameter exponent and the wavelength exponent are very sensitive to changes in pressure for low pressures (0.13 Pa to 0.80 Pa); meanwhile, both exponents saturate for higher pressures (0.80 Pa to 6.7 Pa) around a value of 0.6. These predictions will serve as guides to future experiments for quantitative description of the film morphology under a wide range of vapor pressure.

Vapor-Phase Deposition and Modification of Metal-Organic Frameworks: State-of-the-Art and Future Directions.

PubMed

Stassen, Ivo; De Vos, Dirk; Ameloot, Rob

2016-10-04

Materials processing, and thin-film deposition in particular, is decisive in the implementation of functional materials in industry and real-world applications. Vapor processing of materials plays a central role in manufacturing, especially in electronics. Metal-organic frameworks (MOFs) are a class of nanoporous crystalline materials on the brink of breakthrough in many application areas. Vapor deposition of MOF thin films will facilitate their implementation in micro- and nanofabrication research and industries. In addition, vapor-solid modification can be used for postsynthetic tailoring of MOF properties. In this context, we review the recent progress in vapor processing of MOFs, summarize the underpinning chemistry and principles, and highlight promising directions for future research. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid coatings deposited from liquid methyl methacrylate via Plasma Polymerization

NASA Astrophysics Data System (ADS)

Wurlitzer, Lisa; Maus-Friedrichs, Wolfgang; Dahle, Sebastian

2016-09-01

The polymerization of methyl methacrylate via plasma discharges is well known today. Usually, plasma-enhanced chemical vapor deposition (PECVD) is used to deposit polymer coatings. Solid coatings are formed out of the liquid phase from methyl methacrylate via dielectric barrier discharge. The formation of the coating proceeds in the gas and the liquid phase. To learn more about the reactions in the two phases, the coatings from MMA monomer will be compared to those from MMA resin. Finally, attenuated total reflection infrared spectroscopy, confocal laser scanning microscopy and X-ray photoelectron spectroscopy are employed to characterize the solid coatings. In conclusion, the plasma enhanced chemical solution deposition is compared to the classical thermal polymerization of MMA.

Porosity effects on crystallization kinetics of Amorphous Solid Water: Implications for cold icy objects in the Outer Solar System

NASA Astrophysics Data System (ADS)

Mitchell, Emily H.; Raut, Ujjwal; Baragiola, Raul A.

2015-11-01

Crystalline ice has been identified on the cold surfaces of most icy satellites and TNOs [1]. This is surprising since accretion of water vapor at temperatures (T < 100 K) should result in the amorphous phase [2]. There are several possible explanations for the unexpected presence of crystalline ice on cold bodies, including cryovolcanism [3] and pulsed heating by micrometeoritic impacts [4].A salient feature of ice films condensed at low T is microporosity, known to increase with deposition angle [5]. Here we investigate the dependence of the crystallization rate on the ice porosity, which could contribute to the observed variation in crystallization time τc reported in the literature [2]. Such dependence is noted in other porous materials such as zeolites and titania [6, 7].Amorphous ice films were deposited on a CsI substrate from a collimated water vapor source at 10 K at incidences varying from 0 to 70°, as well as from an omnidirectional water vapor source. The films were heated to temperatures between 130 and 140 K following deposition. The isothermal transition from amorphous to fully crystalline phase was characterized by analyzing the time-dependent evolution of the OH-stretch absorption band using transmission infrared spectroscopy. Our initial results show that τc decreases with increasing porosity; for instance, a film deposited at 45° was observed to crystallize ~6 times faster than a film deposited at 0°. The preliminary estimate of the porosity of the 45° film is ~50% higher than that of the film deposited at normal incidence. Our findings can explain the reported variation in temperature-dependent τc [2] and contribute to the understanding of crystalline ice on cold bodies in the Outer Solar System.1. Mastrapa, R.M.E. et al. In: Gudipati, M.S. & Castillo-Rogez, J., Eds, The Science of Solar System Ices, Springer, New York, 2013.2. Baragiola, R.A. In: Devlin & Buch, Eds, Water in Confining Geometries, Springer-Verlag, 2003.3. Jewitt, D

Fabricating amorphous silicon solar cells by varying the temperature _of the substrate during deposition of the amorphous silicon layer

DOEpatents

Carlson, David E.

1982-01-01

An improved process for fabricating amorphous silicon solar cells in which the temperature of the substrate is varied during the deposition of the amorphous silicon layer is described. Solar cells manufactured in accordance with this process are shown to have increased efficiencies and fill factors when compared to solar cells manufactured with a constant substrate temperature during deposition of the amorphous silicon layer.

Amorphous stabilization and dissolution enhancement of amorphous ternary solid dispersions: combination of polymers showing drug-polymer interaction for synergistic effects.

PubMed

Prasad, Dev; Chauhan, Harsh; Atef, Eman

2014-11-01

The purpose of this study was to understand the combined effect of two polymers showing drug-polymer interactions on amorphous stabilization and dissolution enhancement of indomethacin (IND) in amorphous ternary solid dispersions. The mechanism responsible for the enhanced stability and dissolution of IND in amorphous ternary systems was studied by exploring the miscibility and intermolecular interactions between IND and polymers through thermal and spectroscopic analysis. Eudragit E100 and PVP K90 at low concentrations (2.5%-40%, w/w) were used to prepare amorphous binary and ternary solid dispersions by solvent evaporation. Stability results showed that amorphous ternary solid dispersions have better stability compared with amorphous binary solid dispersions. The dissolution of IND from the ternary dispersion was substantially higher than the binary dispersions as well as amorphous drug. Melting point depression of physical mixtures reveals that the drug was miscible in both the polymers; however, greater miscibility was observed in ternary physical mixtures. The IR analysis confirmed intermolecular interactions between IND and individual polymers. These interactions were found to be intact in ternary systems. These results suggest that the combination of two polymers showing drug-polymer interaction offers synergistic enhancement in amorphous stability and dissolution in ternary solid dispersions. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association.

Optical, mechanical and surface properties of amorphous carbonaceous thin films obtained by plasma enhanced chemical vapor deposition and plasma immersion ion implantation and deposition

NASA Astrophysics Data System (ADS)

Turri, Rafael G.; Santos, Ricardo M.; Rangel, Elidiane C.; da Cruz, Nilson C.; Bortoleto, José R. R.; Dias da Silva, José H.; Antonio, César Augusto; Durrant, Steven F.

2013-09-01

Diverse amorphous hydrogenated carbon-based films (a-C:H, a-C:H:F, a-C:H:N, a-C:H:Cl and a-C:H:Si:O) were obtained by radiofrequency plasma enhanced chemical vapor deposition (PECVD) and plasma immersion ion implantation and deposition (PIIID). The same precursors were used in the production of each pair of each type of film, such as a-C:H, using both PECVD and PIIID. Optical properties, namely the refractive index, n, absorption coefficient, α, and optical gap, ETauc, of these films were obtained via transmission spectra in the ultraviolet-visible near-infrared range (wavelengths from 300 to 3300 nm). Film hardness, elastic modulus and stiffness were obtained as a function of depth using nano-indentation. Surface energy values were calculated from liquid drop contact angle data. Film roughness and morphology were assessed using atomic force microscopy (AFM). The PIIID films were usually thinner and possessed higher refractive indices than the PECVD films. Determined refractive indices are consistent with literature values for similar types of films. Values of ETauc were increased in the PIIID films compared to the PECVD films. An exception was the a-C:H:Si:O films, for which that obtained by PIIID was thicker and exhibited a decreased ETauc. The mechanical properties - hardness, elastic modulus and stiffness - of films produced by PECVD and PIIID generally present small differences. An interesting effect is the increase in the hardness of a-C:H:Cl films from 1.0 to 3.0 GPa when ion implantation is employed. Surface energy correlates well with surface roughness. The implanted films are usually smoother than those obtained by PECVD.

Vapor Phase Deposition Using Plasma Spray-PVD™

NASA Astrophysics Data System (ADS)

von Niessen, K.; Gindrat, M.; Refke, A.

2010-01-01

Plasma spray—physical vapor deposition (PS-PVD) is a low pressure plasma spray technology to deposit coatings out of the vapor phase. PS-PVD is a part of the family of new hybrid processes recently developed by Sulzer Metco AG (Switzerland) on the basis of the well-established low pressure plasma spraying (LPPS) technology. Included in this new process family are plasma spray—chemical vapor deposition (PS-CVD) and plasma spray—thin film (PS-TF) processes. In comparison to conventional vacuum plasma spraying and LPPS, these new processes use a high energy plasma gun operated at a work pressure below 2 mbar. This leads to unconventional plasma jet characteristics which can be used to obtain specific and unique coatings. An important new feature of PS-PVD is the possibility to deposit a coating not only by melting the feed stock material which builds up a layer from liquid splats, but also by vaporizing the injected material. Therefore, the PS-PVD process fills the gap between the conventional PVD technologies and standard thermal spray processes. The possibility to vaporize feedstock material and to produce layers out of the vapor phase results in new and unique coating microstructures. The properties of such coatings are superior to those of thermal spray and EB-PVD coatings. This paper reports on the progress made at Sulzer Metco to develop functional coatings build up from vapor phase of oxide ceramics and metals.

Automatic chemical vapor deposition

NASA Technical Reports Server (NTRS)

Kennedy, B. W.

1981-01-01

Report reviews chemical vapor deposition (CVD) for processing integrated circuits and describes fully automatic machine for CVD. CVD proceeds at relatively low temperature, allows wide choice of film compositions (including graded or abruptly changing compositions), and deposits uniform films of controllable thickness at fairly high growth rate. Report gives overview of hardware, reactants, and temperature ranges used with CVD machine.

Vapor deposition of thin films

DOEpatents

Smith, David C.; Pattillo, Stevan G.; Laia, Jr., Joseph R.; Sattelberger, Alfred P.

1992-01-01

A highly pure thin metal film having a nanocrystalline structure and a process of preparing such highly pure thin metal films of, e.g., rhodium, iridium, molybdenum, tungsten, rhenium, platinum, or palladium by plasma assisted chemical vapor deposition of, e.g., rhodium(allyl).sub.3, iridium(allyl).sub.3, molybdenum(allyl).sub.4, tungsten(allyl).sub.4, rhenium(allyl).sub.4, platinum(allyl).sub.2, or palladium(allyl).sub.2 are disclosed. Additionally, a general process of reducing the carbon content of a metallic film prepared from one or more organometallic precursor compounds by plasma assisted chemical vapor deposition is disclosed.

Gallium assisted plasma enhanced chemical vapor deposition of silicon nanowires.

PubMed

Zardo, I; Yu, L; Conesa-Boj, S; Estradé, S; Alet, Pierre Jean; Rössler, J; Frimmer, M; Roca I Cabarrocas, P; Peiró, F; Arbiol, J; Morante, J R; Fontcuberta I Morral, A

2009-04-15

Silicon nanowires have been grown with gallium as catalyst by plasma enhanced chemical vapor deposition. The morphology and crystalline structure has been studied by electron microscopy and Raman spectroscopy as a function of growth temperature and catalyst thickness. We observe that the crystalline quality of the wires increases with the temperature at which they have been synthesized. The crystalline growth direction has been found to vary between <111> and <112>, depending on both the growth temperature and catalyst thickness. Gallium has been found at the end of the nanowires, as expected from the vapor-liquid-solid growth mechanism. These results represent good progress towards finding alternative catalysts to gold for the synthesis of nanowires.

Resolving the nanostructure of plasma-enhanced chemical vapor deposited nanocrystalline SiOx layers for application in solar cells

NASA Astrophysics Data System (ADS)

Klingsporn, M.; Kirner, S.; Villringer, C.; Abou-Ras, D.; Costina, I.; Lehmann, M.; Stannowski, B.

2016-06-01

Nanocrystalline silicon suboxides (nc-SiOx) have attracted attention during the past years for the use in thin-film silicon solar cells. We investigated the relationships between the nanostructure as well as the chemical, electrical, and optical properties of phosphorous, doped, nc-SiO0.8:H fabricated by plasma-enhanced chemical vapor deposition. The nanostructure was varied through the sample series by changing the deposition pressure from 533 to 1067 Pa. The samples were then characterized by X-ray photoelectron spectroscopy, spectroscopic ellipsometry, Raman spectroscopy, aberration-corrected high-resolution transmission electron microscopy, selected-area electron diffraction, and a specialized plasmon imaging method. We found that the material changed with increasing pressure from predominantly amorphous silicon monoxide to silicon dioxide containing nanocrystalline silicon. The nanostructure changed from amorphous silicon filaments to nanocrystalline silicon filaments, which were found to cause anisotropic electron transport.

Carbon nanotubes synthesized by Ni-assisted atmospheric pressure thermal chemical vapor deposition

NASA Astrophysics Data System (ADS)

Choi, G. S.; Cho, Y. S.; Hong, S. Y.; Park, J. B.; Son, K. H.; Kim, D. J.

2002-03-01

A detailed systematic study on the growth morphology of carbon nanotubes (CNTs) on Si in atmospheric pressure thermal chemical vapor deposition was undertaken. The role of NH3 for vertical alignment of CNTs was investigated. The direct cause for the alignment was a dense distribution of the catalytic metal particles, but that the particles are maintained catalytically active under amorphous carbon deposits was established by NH3. It allows a dense nucleation of the CNTs, and consequently, assists vertical alignment through entanglement and mechanical leaning among the tubes. The CNTs grew in a base growth mode. Since Ni is consumed both by silicide reaction and by capture into the growing tube, the growth stops when Ni is totally depleted. It occurs earlier for smaller particles, and thus a long time of growth results in a thin bottom with poor adhesion.

Qualification of a sublimation tool applied to the case of metalorganic chemical vapor deposition of In{sub 2}O{sub 3} from In(tmhd){sub 3} as a solid precursor

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

Szkutnik, P. D., E-mail: pierre.szkutnik@cea.fr; Jiménez, C.; Angélidès, L.

2016-02-15

A solid delivery system consisting of a source canister, a gas management, and temperature controlled enclosure designed and manufactured by Air Liquide Electronics Systems was tested in the context of gas-phase delivery of the In(tmhd){sub 3} solid precursor. The precursor stream was delivered to a thermal metalorganic chemical vapor deposition reactor to quantify deposition yield under various conditions of carrier gas flow and sublimation temperature. The data collected allowed the determination of characteristic parameters such as the maximum precursor flow rate (18.2 mg min{sup −1} in specified conditions) and the critical mass (defined as the minimum amount of precursor ablemore » to attain the maximum flow rate) found to be about 2.4 g, as well as an understanding of the influence of powder distribution inside the canister. Furthermore, this qualification enabled the determination of optimal delivery conditions which allowed for stable and reproducible precursor flow rates over long deposition times (equivalent to more than 47 h of experiment). The resulting In{sub 2}O{sub 3} layers was compared with those elaborated via pulsed liquid injection obtained in the same chemical vapor deposition chamber and under the same deposition conditions.« less

Continuum limit of the vibrational properties of amorphous solids.

PubMed

Mizuno, Hideyuki; Shiba, Hayato; Ikeda, Atsushi

2017-11-14

The low-frequency vibrational and low-temperature thermal properties of amorphous solids are markedly different from those of crystalline solids. This situation is counterintuitive because all solid materials are expected to behave as a homogeneous elastic body in the continuum limit, in which vibrational modes are phonons that follow the Debye law. A number of phenomenological explanations for this situation have been proposed, which assume elastic heterogeneities, soft localized vibrations, and so on. Microscopic mean-field theories have recently been developed to predict the universal non-Debye scaling law. Considering these theoretical arguments, it is absolutely necessary to directly observe the nature of the low-frequency vibrations of amorphous solids and determine the laws that such vibrations obey. Herein, we perform an extremely large-scale vibrational mode analysis of a model amorphous solid. We find that the scaling law predicted by the mean-field theory is violated at low frequency, and in the continuum limit, the vibrational modes converge to a mixture of phonon modes that follow the Debye law and soft localized modes that follow another universal non-Debye scaling law.

Structure, mechanical, and frictional properties of hydrogenated fullerene-like amorphous carbon film prepared by direct current plasma enhanced chemical vapor deposition

NASA Astrophysics Data System (ADS)

Wang, Yongfu; Gao, Kaixiong; Zhang, Junyan

2016-07-01

In this study, fullerene like carbon (FL-C) is introduced in hydrogenated amorphous carbon (a-C:H) film by employing a direct current plasma enhanced chemical vapor deposition. The film has a low friction and wear, such as 0.011 and 2.3 × 10-9mm3/N m in the N2, and 0.014 and 8.4 × 10-8mm3/N m in the humid air, and high hardness and elasticity (25.8 GPa and 83.1%), to make further engineering applications in practice. It has several nanometers ordered domains consisting of less frequently cross-linked graphitic sheet stacks. We provide new evidences for understanding the reported Raman fit model involving four vibrational frequencies from five, six, and seven C-atom rings of FL-C structures, and discuss the structure evolution before or after friction according to the change in the 1200 cm-1 Raman band intensity caused by five- and seven-carbon rings. Friction inevitably facilitates the transformation of carbon into FL-C nanostructures, namely, the ultra low friction comes from both such structures within the carbon film and the sliding induced at friction interface.

Ruthenium films by digital chemical vapor deposition: Selectivity, nanostructure, and work function

NASA Astrophysics Data System (ADS)

Dey, Sandwip K.; Goswami, Jaydeb; Gu, Diefeng; de Waard, Henk; Marcus, Steve; Werkhoven, Chris

2004-03-01

Ruthenium electrodes were selectively deposited on photoresist-patterned HfO2 surface [deposited on a SiOx/Si wafer by atomic layer deposition (ALD)] by a manufacturable, digital chemical vapor deposition (DCVD) technique. DCVD of Ru was carried out at 280-320 °C using an alternate delivery of Bis (2,2,6,6-tetramethyl-3,5-heptanedionato)(1,5-cyclooctadiene)Ru (dissolved in tetrahydrofuran) and oxygen. The as-deposited Ru films were polycrystalline, dense, and conducting (resistivity ˜20.6 μΩ cm). However, Rutherford backscattering spectroscopy, x-ray photoelectron spectroscopy, and high-resolution electron microscopy results indicate the presence of an amorphous RuOx at the Ru grain boundaries and at the DCVD-Ru/ALD-HfO2 interface. The estimated work function of DCVD-Ru on ALD-HfO2 was ˜5.1 eV. Moreover, the equivalent oxide thickness, hysteresis in capacitance-voltage, and leakage current density at -2 V of the HfO2/SiOx dielectric, after forming gas (95% N2+5% H2) annealing at 450 °C for 30 min, were 1.4 nm, 20 mV, and 7.4×10-7 A cm-2, respectively.

Method and apparatus for conducting variable thickness vapor deposition

DOEpatents

Nesslage, G.V.

1984-08-03

A method of vapor depositing metal on a substrate in variable thickness comprises conducting the deposition continuously without interruption to avoid formation of grain boundaries. To achieve reduced deposition in specific regions a thin wire or ribbon blocking body is placed between source and substrate to partially block vapors from depositing in the region immediately below.

Effects of argon addition on a-CNx film deposition by hot carbon filament chemical vapor deposition

NASA Astrophysics Data System (ADS)

Watanabe, Yoshihisa; Aono, Masami; Yamazaki, Ayumi; Kitazawa, Nobuaki; Nakamura, Yoshikazu

2002-07-01

Using a carbon filament which supplies carbon and heat, amorphous carbon nitride (a-CNx) films were prepared on Si (100) substrates by hot filament chemical vapor deposition. Deposition was performed in a low-pressure atmosphere of pure nitrogen and a gas mixture of nitrogen and argon. Effects of argon additions to the nitrogen atmosphere on the film microstructure and interface composition between the film and substrate were studied by field-emission scanning electron microscopy (FESEM) and x-ray photoelectron spectroscopy (XPS). FESEM observations reveal that the film prepared in a pure nitrogen atmosphere has uniform nucleation and a densely packed columnar pieces structure. The film prepared in the nitrogen and argon gas mixture exhibits preferential nucleation and a tapered structure with macroscopic voids. Depth analyses using XPS reveal that the film prepared in pure nitrogen possesses a broad interface, which includes silicon carbide as well as a-CNx, whereas a sharp interface is discerned in the film prepared in the mixed nitrogen and argon gas. We observed that silicon carbide formation is suppressed by an argon addition to the nitrogen atmosphere during deposition. copyright 2002 American Vacuum Society.

Continuum limit of the vibrational properties of amorphous solids

PubMed Central

Mizuno, Hideyuki; Ikeda, Atsushi

2017-01-01

The low-frequency vibrational and low-temperature thermal properties of amorphous solids are markedly different from those of crystalline solids. This situation is counterintuitive because all solid materials are expected to behave as a homogeneous elastic body in the continuum limit, in which vibrational modes are phonons that follow the Debye law. A number of phenomenological explanations for this situation have been proposed, which assume elastic heterogeneities, soft localized vibrations, and so on. Microscopic mean-field theories have recently been developed to predict the universal non-Debye scaling law. Considering these theoretical arguments, it is absolutely necessary to directly observe the nature of the low-frequency vibrations of amorphous solids and determine the laws that such vibrations obey. Herein, we perform an extremely large-scale vibrational mode analysis of a model amorphous solid. We find that the scaling law predicted by the mean-field theory is violated at low frequency, and in the continuum limit, the vibrational modes converge to a mixture of phonon modes that follow the Debye law and soft localized modes that follow another universal non-Debye scaling law. PMID:29087941

Metal organic chemical vapor deposition of 111-v compounds on silicon

DOEpatents

Vernon, Stanley M.

1986-01-01

Expitaxial composite comprising thin films of a Group III-V compound semiconductor such as gallium arsenide (GaAs) or gallium aluminum arsenide (GaAlAs) on single crystal silicon substrates are disclosed. Also disclosed is a process for manufacturing, by chemical deposition from the vapor phase, epitaxial composites as above described, and to semiconductor devices based on such epitaxial composites. The composites have particular utility for use in making light sensitive solid state solar cells.

Amorphization of itraconazole by inorganic pharmaceutical excipients: comparison of excipients and processing methods.

PubMed

Grobelny, Pawel; Kazakevich, Irina; Zhang, Dan; Bogner, Robin

2015-01-01

The aim of this study was to investigate the effects of solid carriers and processing routes on the properties of amorphous solid dispersions of itraconazole. Three solid carriers with a range of surface properties were studied, (1) a mesoporous silicate, magnesium aluminum silicate (Neusilin US2), (2) a nonporous silicate of corresponding composition (Veegum) and (3) a non-silicate, inorganic excipient, calcium phosphate dibasic anhydrous (A-TAB). The drug was incorporated via either solvent-deposition or ball milling. Both the maximum drug deposited by solvent-based method that produced an amorphous composite and the time for complete amorphization by co-milling was determined by X-ray powder diffraction (XRPD). Changes in the drug and excipients were monitored by nitrogen adsorption and wettability of the powder. The ability of the excipients to amorphize the drug and enhance its dissolution was related to the powder characteristics. Neusilin provided the fastest amorphization time in the mill and highest drug loading by solvent-deposition, compared with the other two excipients. Solvent-deposition provided greater dissolution enhancement than milling, due to the reduction in Neusilin porosity during high energy milling.This study confirms that substrates as well as the processing routes have notable influence on the drug deposition, amorphization, physical stability and drug in vitro release.

Deposition of single and layered amorphous fluorocarbon films by C8F18 PECVD

NASA Astrophysics Data System (ADS)

Yamauchi, Tatsuya; Mizuno, Kouichiro; Sugawara, Hirotake

2008-10-01

Amorphous fluorocarbon films were deposited by plasma-enhanced chemical vapor deposition (PECVD) using C8F18 in closed system at C8F18 pressures 0.1--0.3 Torr, deposition times 1--30 min and plasma powers 20--200 W@. The layered films were composed by repeated PECVD processes. We compared `two-layered' and `intermittently deposited' films, which were made by the PECVD, respectively, with and without renewal of the gas after the deposition of the first layer. The interlayer boundary was observed in the layered films, and that of the intermittently deposited films showed a tendency to be clearer when the deposition time until the interruption of the PECVD was shorter. The film thickness increased linearly in the beginning of the PECVD and it turned down after 10--15 min, that was similar between the single and intermittently deposited films. It was considered that large precursors made at a low decomposition degree of C8F18 contributed to the film deposition in the early phase and that the downturn was due to the development of the C8F18 decomposition. This explanation on the deposition mechanism agrees qualitatively with our experimental data of pressure change and optical emission spectra during the deposition. This work is supported by Grant-in-Aid from Japan Society for the Promotion of Science.

Disseminated flake graphite and amorphous graphite deposit types. An analysis using grade and tonnage models

USGS Publications Warehouse

Sutphin, David M.; Bliss, James D.

1990-01-01

On the basis of differences derived from genetic, descriptive, and grade-tonnage data, graphite deposits are classified here into three deposit types: disseminated flake, amorphous (microcrystalline), or graphite veins. Descriptive models have been constructed for each of these deposit types, and grade-tonnage models are constructed for disseminated flake and amorphous deposit types. Grade and tonnage data are used also to construct grade-tonnage models that assist in predicting the size and grade of undiscovered graphite deposits. The median tonnage and carbon grade of disseminated flake deposits are 240 000 tonnes and 9% carbon and for amorphous deposits, 130 000 tonnes and 40% carbon. The differences in grade between disseminated flake and amorphous deposit types are statistically significant, whereas the differences in amount of contained carbon are not.

Preparing highly ordered glasses of discotic liquid crystalline systems by vapor deposition

NASA Astrophysics Data System (ADS)

Gujral, Ankit; Gomez, Jaritza; Bishop, Camille E.; Toney, Michael F.; Ediger, M. D.

Anisotropic molecular packing, particularly in highly ordered liquid-crystalline arrangements, has the potential for optimizing performance in organic electronic and optoelectronic applications. Here we show that physical vapor deposition can be used to prepare highly organized out-of-equilibrium (glassy) solids of discotic liquid-crystalline (LC) systems. Using grazing incidence x-ray scattering, we compare 3 systems: a rectangular columnar LC, a hexagonal columnar LC and a non-liquid crystal former. The packing motifs accessible by vapor deposition are highly organized and vary from face-on to edge-on columnar arrangements depending upon substrate temperature. A subset of these structures cannot be accessed under equilibrium conditions. The structures formed at a given substrate temperature can be understood as the result of the system partially equilibrating toward the structure of the free surface of the equilibrium liquid crystal. Consistent with this view, the structures formed are independent of the substrate material.

Hybrid Physical Vapor Deposition Instrument for Advanced Functional Multilayers and Materials

DTIC Science & Technology

2016-04-27

Hybrid Physical Vapor Deposition Instrument for Advanced Functional Multilayers and Materials PI Maria received support to construct a physical... vapor deposition (PVD) system that combines electron beam (e- beam) evaporation, magnetron sputtering, pulsed laser ablation, and ion-assisted deposition ...peer-reviewed journals: Number of Papers published in non peer-reviewed journals: Final Report: Hybrid Physical Vapor Deposition Instrument for Advanced

Structure, mechanical, and frictional properties of hydrogenated fullerene-like amorphous carbon film prepared by direct current plasma enhanced chemical vapor deposition

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

Wang, Yongfu; University of Chinese Academy of Sciences, Beijing 100049; Gao, Kaixiong

In this study, fullerene like carbon (FL-C) is introduced in hydrogenated amorphous carbon (a-C:H) film by employing a direct current plasma enhanced chemical vapor deposition. The film has a low friction and wear, such as 0.011 and 2.3 × 10{sup −9}mm{sup 3}/N m in the N{sub 2}, and 0.014 and 8.4 × 10{sup −8}mm{sup 3}/N m in the humid air, and high hardness and elasticity (25.8 GPa and 83.1%), to make further engineering applications in practice. It has several nanometers ordered domains consisting of less frequently cross-linked graphitic sheet stacks. We provide new evidences for understanding the reported Raman fit model involving four vibrational frequenciesmore » from five, six, and seven C-atom rings of FL-C structures, and discuss the structure evolution before or after friction according to the change in the 1200 cm{sup −1} Raman band intensity caused by five- and seven-carbon rings. Friction inevitably facilitates the transformation of carbon into FL-C nanostructures, namely, the ultra low friction comes from both such structures within the carbon film and the sliding induced at friction interface.« less

Solid state amorphization kinetic of alpha lactose upon mechanical milling.

PubMed

Caron, Vincent; Willart, Jean-François; Lefort, Ronan; Derollez, Patrick; Danède, Florence; Descamps, Marc

2011-11-29

It has been previously reported that α-lactose could be totally amorphized by ball milling. In this paper we report a detailed investigation of the structural and microstructural changes by which this solid state amorphization takes place. The investigations have been performed by Powder X-ray Diffraction, Solid State Nuclear Magnetic Resonance ((13)C CP-MAS) and Differential Scanning Calorimetry. The results reveal the structural complexity of the material in the course of its amorphization so that it cannot be considered as a simple mixture made of a decreasing crystalline fraction and an increasing amorphous fraction. Heating this complexity can give rise to a fully nano-crystalline material. The results also show that chemical degradations upon heating are strongly connected to the melting process. Copyright © 2011 Elsevier Ltd. All rights reserved.

Solid-State NMR Investigation of Drug-Excipient Interactions and Phase Behavior in Indomethacin-Eudragit E Amorphous Solid Dispersions.

PubMed

Lubach, Joseph W; Hau, Jonathan

2018-02-20

To investigate the nature of drug-excipient interactions between indomethacin (IMC) and methacrylate copolymer Eudragit® E (EE) in the amorphous state, and evaluate the effects on formulation and stability of these amorphous systems. Amorphous solid dispersions containing IMC and EE were spray dried with drug loadings from 20% to 90%. PXRD was used to confirm the amorphous nature of the dispersions, and DSC was used to measure glass transition temperatures (T g ). 13 C and 15 N solid-state NMR was utilized to investigate changes in local structure and protonation state, while 1 H T 1 and T 1ρ relaxation measurements were used to probe miscibility and phase behavior of the dispersions. T g values for IMC-EE solid dispersions showed significant positive deviations from predicted values in the drug loading range of 40-90%, indicating a relatively strong drug-excipient interaction. 15 N solid-state NMR exhibited a change in protonation state of the EE basic amine, with two distinct populations for the EE amine at -360.7 ppm (unprotonated) and -344.4 ppm (protonated). Additionally, 1 H relaxation measurements showed phase separation at high drug load, indicating an amorphous ionic complex and free IMC-rich phase. PXRD data showed all ASDs up to 90% drug load remained physically stable after 2 years. 15 N solid-state NMR experiments show a change in protonation state of EE, indicating that an ionic complex indeed forms between IMC and EE in amorphous solid dispersions. Phase behavior was determined to exhibit nanoscale phase separation at high drug load between the amorphous ionic complex and excess free IMC.

Structural Characterization of Vapor-deposited Organic Glasses

NASA Astrophysics Data System (ADS)

Gujral, Ankit

Physical vapor deposition, a common route of thin film fabrication for organic electronic devices, has recently been shown to produce organic glassy films with enhanced kinetic stability and anisotropic structure. Anisotropic structures are of interest in the organic electronics community as it has been shown that certain structures lead to enhanced device performance, such as higher carrier mobility and better light outcoupling. A mechanism proposed to explain the origin of the stability and anisotropy of vapor-deposited glasses relies on two parameters: 1) enhanced molecular mobility at the free surface (vacuum interface) of a glass, and 2) anisotropic molecular packing at the free surface of the supercooled liquid of the glass-forming system. By vapor-depositing onto a substrate maintained at Tsubstrate < Tg (where Tg is the glass transition temperature), the enhanced molecular mobility at the free surface allows every molecule that lands on the surface to at least partially equilibrate to the preferred anisotropic molecular packing motifs before being buried by further deposition. The extent of equilibration depends on the mobility at the surface, controlled by Tsubstrate, and the residence time on the free surface, controlled by the rate of deposition. This body of work deals with the optimization of deposition conditions and system chemistry to prepare and characterize films with functional anisotropic structures. Here, we show that structural anisotropy can be attained for a variety of molecular systems including a rod-shaped non-mesogen, TPD, a rod-shaped smectic mesogen, itraconazole, two discotic mesogens, phenanthroperylene-ester and triphenylene-ester, and a disc-shaped non-mesogen, m-MTDATA. Experimental evidence is also provided of the anisotropic molecular packing at the free surface (vacuum interface) for the disc-shaped systems that are consistent with the expectations of the proposed mechanism and the final bulk state of the vapor-deposited

A Molecular-Level View of the Physical Stability of Amorphous Solid Dispersions

NASA Astrophysics Data System (ADS)

Yuan, Xiaoda

Many pharmaceutical compounds being developed in recent years are poorly soluble in water. This has led to insufficient oral bioavailability of many compounds in vitro. The amorphous formulation is one of the promising techniques to increase the oral bioavailability of these poorly water-soluble compounds. However, an amorphous drug substance is inherently unstable because it is a high energy form. In order to increase the physical stability, the amorphous drug is often formulated with a suitable polymer to form an amorphous solid dispersion. Previous research has suggested that the formation of an intimately mixed drug-polymer mixture contributes to the stabilization of the amorphous drug compound. The goal of this research is to better understand the role of miscibility, molecular interactions and mobility on the physical stability of amorphous solid dispersions. Methods were developed to detect different degrees of miscibility on nanometer scale and to quantify the extent of hydrogen-bonding interactions between the drug and the polymer. Miscibility, hydrogen-bonding interactions and molecular mobility were correlated with physical stability during a six-month period using three model systems. Overall, this research provides molecular-level insights into many factors that govern the physical stability of amorphous solid dispersions which can lead to a more effective design of stable amorphous formulations.

Chemical-Vapor-Deposited Diamond Film

NASA Technical Reports Server (NTRS)

Miyoshi, Kazuhisa

1999-01-01

This chapter describes the nature of clean and contaminated diamond surfaces, Chemical-vapor-deposited (CVD) diamond film deposition technology, analytical techniques and the results of research on CVD diamond films, and the general properties of CVD diamond films. Further, it describes the friction and wear properties of CVD diamond films in the atmosphere, in a controlled nitrogen environment, and in an ultra-high-vacuum environment.

Effect of milling conditions on solid-state amorphization of glipizide, and characterization and stability of solid forms.

PubMed

Xu, Kailin; Xiong, Xinnuo; Zhai, Yuanming; Wang, Lili; Li, Shanshan; Yan, Jin; Wu, Di; Ma, Xiaoli; Li, Hui

2016-09-10

In this study, the amorphization of glipizide was systematically investigated through high-energy ball milling at different temperatures. The results of solid-state amorphization through milling indicated that glipizide underwent direct crystal-to-glass transformation at 15 and 25°C and crystal-to-glass-to-crystal conversion at 35°C; hence, milling time and temperature had significant effects on the amorphization of glipizide, which should be effectively controlled to obtain totally amorphous glipizide. Solid forms of glipizide were detailedly characterized through analyses of X-ray powder diffraction, morphology, thermal curves, vibrational spectra, and solid-state nuclear magnetic resonance. The physical stability of solid forms was investigated under different levels of relative humidity (RH) at 25°C. Forms I and III are kinetically stable and do not form any new solid-state forms at various RH levels. By contrast, Form II is kinetically unstable, undergoing direct glass-to-crystal transformation when RH levels higher than 32.8%. Therefore, stability investigation indicated that Form II should be stored under relatively dry conditions to prevent rapid crystallization. High temperatures can also induce the solid-state transformation of Form II; the conversion rate increased with increasing temperature. Copyright © 2016 Elsevier B.V. All rights reserved.

Magmatic-vapor expansion and the formation of high-sulfidation gold deposits: Chemical controls on alteration and mineralization

USGS Publications Warehouse

Henley, R.W.; Berger, B.R.

2011-01-01

Large bulk-tonnage high-sulfidation gold deposits, such as Yanacocha, Peru, are the surface expression of structurally-controlled lode gold deposits, such as El Indio, Chile. Both formed in active andesite-dacite volcanic terranes. Fluid inclusion, stable isotope and geologic data show that lode deposits formed within 1500. m of the paleo-surface as a consequence of the expansion of low-salinity, low-density magmatic vapor with very limited, if any, groundwater mixing. They are characterized by an initial 'Sulfate' Stage of advanced argillic wallrock alteration ?? alunite commonly with intense silicification followed by a 'Sulfide' Stage - a succession of discrete sulfide-sulfosalt veins that may be ore grade in gold and silver. Fluid inclusions in quartz formed during wallrock alteration have homogenization temperatures between 100 and over 500 ??C and preserve a record of a vapor-rich environment. Recent data for El Indio and similar deposits show that at the commencement of the Sulfide Stage, 'condensation' of Cu-As-S sulfosalt melts with trace concentrations of Sb, Te, Bi, Ag and Au occurred at > 600 ??C following pyrite deposition. Euhedral quartz crystals were simultaneously deposited from the vapor phase during crystallization of the vapor-saturated melt occurs to Fe-tennantite with progressive non-equilibrium fractionation of heavy metals between melt-vapor and solid. Vugs containing a range of sulfides, sulfosalts and gold record the changing composition of the vapor. Published fluid inclusion and mineralogical data are reviewed in the context of geological relationships to establish boundary conditions through which to trace the expansion of magmatic vapor from source to surface and consequent alteration and mineralization. Initially heat loss from the vapor is high resulting in the formation of acid condensate permeating through the wallrock. This Sulfate Stage alteration effectively isolates the expansion of magmatic vapor in subsurface fracture arrays

Suppressed beta relaxations and reduced heat capacity in ultrastable organic glasses prepared by physical vapor deposition

NASA Astrophysics Data System (ADS)

Ediger, Mark

Glasses play an important role in technology as a result of their macroscopic homogeneity (e.g., the clarity of window glass) and our ability to tune properties through composition changes. A problem with liquid-cooled glasses is that they exhibit marginal kinetic stability and slowly evolve towards lower energy glasses and crystalline states. In contrast, we have shown that physical vapor deposition can prepare glasses with very high kinetic stability. These materials have properties expected for ``million-year-old'' glasses, including high density, low enthalpy, and high mechanical moduli. We have used nanocalorimetry to show that these high stability glasses have lower heat capacities than liquid-cooled glasses for a number of molecular systems. Dielectric relaxation has been used to show that the beta relaxation can be suppressed by nearly a factor of four in vapor-deposited toluene glasses, indicating a very tight packing environment. Consistent with this view, computer simulations of high stability glasses indicate reduced Debye-Waller factors. These high stability materials raise interesting questions about the limiting properties of amorphous packing arrangements.

Resolving the nanostructure of plasma-enhanced chemical vapor deposited nanocrystalline SiO{sub x} layers for application in solar cells

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

Klingsporn, M.; Costina, I.; Kirner, S.

2016-06-14

Nanocrystalline silicon suboxides (nc-SiO{sub x}) have attracted attention during the past years for the use in thin-film silicon solar cells. We investigated the relationships between the nanostructure as well as the chemical, electrical, and optical properties of phosphorous, doped, nc-SiO{sub 0.8}:H fabricated by plasma-enhanced chemical vapor deposition. The nanostructure was varied through the sample series by changing the deposition pressure from 533 to 1067 Pa. The samples were then characterized by X-ray photoelectron spectroscopy, spectroscopic ellipsometry, Raman spectroscopy, aberration-corrected high-resolution transmission electron microscopy, selected-area electron diffraction, and a specialized plasmon imaging method. We found that the material changed with increasing pressuremore » from predominantly amorphous silicon monoxide to silicon dioxide containing nanocrystalline silicon. The nanostructure changed from amorphous silicon filaments to nanocrystalline silicon filaments, which were found to cause anisotropic electron transport.« less

Deposition of device quality low H content, amorphous silicon films

DOEpatents

Mahan, A.H.; Carapella, J.C.; Gallagher, A.C.

1995-03-14

A high quality, low hydrogen content, hydrogenated amorphous silicon (a-Si:H) film is deposited by passing a stream of silane gas (SiH{sub 4}) over a high temperature, 2,000 C, tungsten (W) filament in the proximity of a high temperature, 400 C, substrate within a low pressure, 8 mTorr, deposition chamber. The silane gas is decomposed into atomic hydrogen and silicon, which in turn collides preferably not more than 20--30 times before being deposited on the hot substrate. The hydrogenated amorphous silicon films thus produced have only about one atomic percent hydrogen, yet have device quality electrical, chemical, and structural properties, despite this lowered hydrogen content. 7 figs.

Deposition of device quality low H content, amorphous silicon films

DOEpatents

Mahan, Archie H.; Carapella, Jeffrey C.; Gallagher, Alan C.

1995-01-01

A high quality, low hydrogen content, hydrogenated amorphous silicon (a-Si:H) film is deposited by passing a stream of silane gas (SiH.sub.4) over a high temperature, 2000.degree. C., tungsten (W) filament in the proximity of a high temperature, 400.degree. C., substrate within a low pressure, 8 mTorr, deposition chamber. The silane gas is decomposed into atomic hydrogen and silicon, which in turn collides preferably not more than 20-30 times before being deposited on the hot substrate. The hydrogenated amorphous silicon films thus produced have only about one atomic percent hydrogen, yet have device quality electrical, chemical, and structural properties, despite this lowered hydrogen content.

Vapor-liquid nucleation: the solid touch.

PubMed

Yarom, Michal; Marmur, Abraham

2015-08-01

Vapor-liquid nucleation is a ubiquitous process that has been widely researched in many disciplines. Yet, case studies are quite scattered in the literature, and the implications of some of its basic concepts are not always clearly stated. This is especially noticeable for heterogeneous nucleation, which involves a solid surface in touch with the liquid and vapor. The current review attempts to offer a comprehensive, though concise, thermodynamic discussion of homogeneous and heterogeneous nucleation in vapor-liquid systems. The fundamental concepts of nucleation are detailed, with emphasis on the role of the chemical potential, and on intuitive explanations whenever possible. We review various types of nucleating systems and discuss the effect of the solid geometry on the characteristics of the new phase formation. In addition, we consider the effect of mixing on the vapor-liquid equilibrium. An interesting sub-case is that of a non-volatile solute that modifies the chemical potential of the liquid, but not of the vapor. Finally, we point out topics that need either further research or more exact, accurate presentation. Copyright © 2014 Elsevier B.V. All rights reserved.

Influence of mass diffusion on the stability of thermophoretic growth of a solid from the vapor phase

NASA Technical Reports Server (NTRS)

Castillo, J. L.; Garcia-Ybarra, P. L.; Rosner, D. E.

1991-01-01

The stability of solid planar growth from a binary vapor phase with a condensing species dilute in a carrier gas is examined when the ratio of depositing to carrier species molecular mass is large and the main diffusive transport mechanism is thermal diffusion. It is shown that a deformation of the solid-gas interface induces a deformation of the gas phase isotherms that increases the thermal gradients and thereby the local mass deposition rate at the crests and reduces them at the valleys. The initial surface deformation is enhanced by the modified deposition rates in the absence of appreciable Fick/Brownian diffusion and interfacial energy effects.

Chemical Vapor Deposition of Turbine Thermal Barrier Coatings

NASA Technical Reports Server (NTRS)

Haven, Victor E.

1999-01-01

Ceramic thermal barrier coatings extend the operating temperature range of actively cooled gas turbine components, therefore increasing thermal efficiency. Performance and lifetime of existing ceram ic coatings are limited by spallation during heating and cooling cycles. Spallation of the ceramic is a function of its microstructure, which is determined by the deposition method. This research is investigating metalorganic chemical vapor deposition (MOCVD) of yttria stabilized zirconia to improve performance and reduce costs relative to electron beam physical vapor deposition. Coatings are deposited in an induction-heated, low-pressure reactor at 10 microns per hour. The coating's composition, structure, and response to the turbine environment will be characterized.

The effect of carrier gas flow rate and source cell temperature on low pressure organic vapor phase deposition simulation by direct simulation Monte Carlo method

PubMed Central

Wada, Takao; Ueda, Noriaki

2013-01-01

The process of low pressure organic vapor phase deposition (LP-OVPD) controls the growth of amorphous organic thin films, where the source gases (Alq3 molecule, etc.) are introduced into a hot wall reactor via an injection barrel using an inert carrier gas (N2 molecule). It is possible to control well the following substrate properties such as dopant concentration, deposition rate, and thickness uniformity of the thin film. In this paper, we present LP-OVPD simulation results using direct simulation Monte Carlo-Neutrals (Particle-PLUS neutral module) which is commercial software adopting direct simulation Monte Carlo method. By estimating properly the evaporation rate with experimental vaporization enthalpies, the calculated deposition rates on the substrate agree well with the experimental results that depend on carrier gas flow rate and source cell temperature. PMID:23674843

Chemical-Vapor Deposition Of Silicon Carbide

NASA Technical Reports Server (NTRS)

Cagliostro, D. E.; Riccitiello, S. R.; Ren, J.; Zaghi, F.

1993-01-01

Report describes experiments in chemical-vapor deposition of silicon carbide by pyrolysis of dimethyldichlorosilane in hydrogen and argon carrier gases. Directed toward understanding chemical-kinetic and mass-transport phenomena affecting infiltration of reactants into, and deposition of SiC upon, fabrics. Part of continuing effort to develop method of efficient and more nearly uniform deposition of silicon carbide matrix throughout fabric piles to make improved fabric/SiC-matrix composite materials.

An improved kinetics approach to describe the physical stability of amorphous solid dispersions.

PubMed

Yang, Jiao; Grey, Kristin; Doney, John

2010-01-15

The recrystallization of amorphous solid dispersions may lead to a loss in the dissolution rate, and consequently reduce bioavailability. The purpose of this work is to understand factors governing the recrystallization of amorphous drug-polymer solid dispersions, and develop a kinetics model capable of accurately predicting their physical stability. Recrystallization kinetics was measured using differential scanning calorimetry for initially amorphous efavirenz-polyvinylpyrrolidone solid dispersions stored at controlled temperature and relative humidity. The experimental measurements were fitted by a new kinetic model to estimate the recrystallization rate constant and microscopic geometry of crystal growth. The new kinetics model was used to illustrate the governing factors of amorphous solid dispersions stability. Temperature was found to affect efavirenz recrystallization in an Arrhenius manner, while recrystallization rate constant was shown to increase linearly with relative humidity. Polymer content tremendously inhibited the recrystallization process by increasing the crystallization activation energy and decreasing the equilibrium crystallinity. The new kinetic model was validated by the good agreement between model fits and experiment measurements. A small increase in polyvinylpyrrolidone resulted in substantial stability enhancements of efavirenz amorphous solid dispersion. The new established kinetics model provided more accurate predictions than the Avrami equation.

Preferred orientations of laterally grown silicon films over amorphous substrates using the vapor–liquid–solid technique

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

LeBoeuf, J. L., E-mail: jerome.leboeuf@mail.mcgill.ca; Brodusch, N.; Gauvin, R.

2014-12-28

A novel method has been optimized so that adhesion layers are no longer needed to reliably deposit patterned gold structures on amorphous substrates. Using this technique allows for the fabrication of amorphous oxide templates known as micro-crucibles, which confine a vapor–liquid–solid (VLS) catalyst of nominally pure gold to a specific geometry. Within these confined templates of amorphous materials, faceted silicon crystals have been grown laterally. The novel deposition technique, which enables the nominally pure gold catalyst, involves the undercutting of an initial chromium adhesion layer. Using electron backscatter diffraction it was found that silicon nucleated in these micro-crucibles were 30%more » single crystals, 45% potentially twinned crystals and 25% polycrystals for the experimental conditions used. Single, potentially twinned, and polycrystals all had an aversion to growth with the (1 0 0) surface parallel to the amorphous substrate. Closer analysis of grain boundaries of potentially twinned and polycrystalline samples revealed that the overwhelming majority of them were of the 60° Σ3 coherent twin boundary type. The large amount of coherent twin boundaries present in the grown, two-dimensional silicon crystals suggest that lateral VLS growth occurs very close to thermodynamic equilibrium. It is suggested that free energy fluctuations during growth or cooling, and impurities were the causes for this twinning.« less

Mesoscale modeling of strain induced solid state amorphization in crystalline materials

NASA Astrophysics Data System (ADS)

Lei, Lei

Solid state amorphization, and in particular crystalline to amorphous transformation, can be observed in metallic alloys, semiconductors, intermetallics, minerals, and also molecular crystals when they undergo irradiation, hydrogen gas dissolution, thermal interdiffusion, mechanical alloying, or mechanical milling. Although the amorphization mechanisms may be different, the transformation occurs due to the high level of disorder introduced into the material. Milling induced solid state amorphization is proposed to be the result of accumulation of crystal defects, specifically dislocations, as the material is subjected to large deformations during the high energy process. Thus, understanding the deformation mechanisms of crystalline materials will be the first step in studying solid state amorphization in crystalline materials, which not only has scientific contributions, but also technical consequences. A phase field dislocation dynamics (PFDD) approach is employed in this work to simulate plastic deformation of molecular crystals. This PFDD model has the advantage of tracking all of the dislocations in a material simultaneously. The model takes into account the elastic interaction between dislocations, the lattice resistance to dislocation motion, and the elastic interaction of dislocations with an external stress field. The PFDD model is employed to describe the deformation of molecular crystals with pharmaceutical applications, namely, single crystal sucrose, acetaminophen, gamma-indomethacin, and aspirin. Stress-strain curves are produced that result in expected anisotropic material response due to the activation of different slip systems and yield stresses that agree well with those from experiments. The PFDD model is coupled to a phase transformation model to study the relation between plastic deformation and the solid state amorphization of crystals that undergo milling. This model predicts the amorphous volume fraction in excellent agreement with

Ti-doped hydrogenated diamond like carbon coating deposited by hybrid physical vapor deposition and plasma enhanced chemical vapor deposition

NASA Astrophysics Data System (ADS)

Lee, Na Rae; Sle Jun, Yee; Moon, Kyoung Il; Sunyong Lee, Caroline

2017-03-01

Diamond-like carbon films containing titanium and hydrogen (Ti-doped DLC:H) were synthesized using a hybrid technique based on physical vapor deposition (PVD) and plasma enhanced chemical vapor deposition (PECVD). The film was deposited under a mixture of argon (Ar) and acetylene gas (C2H2). The amount of Ti in the Ti-doped DLC:H film was controlled by varying the DC power of the Ti sputtering target ranging from 0 to 240 W. The composition, microstructure, mechanical and chemical properties of Ti-doped DLC:H films with varying Ti concentrations, were investigated using Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), nano indentation, a ball-on-disk tribometer, a four-point probe system and dynamic anodic testing. As a result, the optimum composition of Ti in Ti-doped DLC:H film using our hybrid method was found to be a Ti content of 18 at. %, having superior electrical conductivity and high corrosion resistance, suitable for bipolar plates. Its hardness value was measured to be 25.6 GPa with a low friction factor.

Metal ions differentially influence the aggregation and deposition of Alzheimer's beta-amyloid on a solid template.

PubMed

Ha, Chanki; Ryu, Jungki; Park, Chan Beum

2007-05-22

The abnormal deposition and aggregation of beta-amyloid (Abeta) on brain tissues are considered to be one of the characteristic neuropathological features of Alzheimer's disease (AD). Environmental conditions such as metal ions, pH, and cell membranes are associated with Abeta deposition and plaque formation. According to the amyloid cascade hypothesis of AD, the deposition of Abeta42 oligomers as diffuse plaques in vivo is an important earliest event, leading to the formation of fibrillar amyloid plaques by the further accumulation of soluble Abeta under certain environmental conditions. In order to characterize the effect of metal ions on amyloid deposition and plaque growth on a solid surface, we prepared a synthetic template by immobilizing Abeta oligomers onto a N-hydroxysuccinimide ester-activated solid surface. According to our study using ex situ atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FT-IR), and thioflavin T (ThT) fluorescence spectroscopy, Cu2+ and Zn2+ ions accelerated both Abeta40 and Abeta42 deposition but resulted only in the formation of "amorphous" aggregates. In contrast, Fe3+ induced the deposition of "fibrillar" amyloid plaques at neutral pH. Under mildly acidic environments, the formation of fibrillar amyloid plaques was not induced by any metal ion tested in this work. Using secondary ion mass spectroscopy (SIMS) analysis, we found that binding Cu ions to Abeta deposits on a solid template occurred by the possible reduction of Cu ions during the interaction of Abeta with Cu2+. Our results may provide insights into the role of metal ions on the formation of fibrillar or amorphous amyloid plaques in AD.

Anisotropic electrical conduction and reduction in dangling-bond density for polycrystalline Si films prepared by catalytic chemical vapor deposition

NASA Astrophysics Data System (ADS)

Niikura, Chisato; Masuda, Atsushi; Matsumura, Hideki

1999-07-01

Polycrystalline Si (poly-Si) films with high crystalline fraction and low dangling-bond density were prepared by catalytic chemical vapor deposition (Cat-CVD), often called hot-wire CVD. Directional anisotropy in electrical conduction, probably due to structural anisotropy, was observed for Cat-CVD poly-Si films. A novel method to separately characterize both crystalline and amorphous phases in poly-Si films using anisotropic electrical conduction was proposed. On the basis of results obtained by the proposed method and electron spin resonance measurements, reduction in dangling-bond density for Cat-CVD poly-Si films was achieved using the condition to make the quality of the included amorphous phase high. The properties of Cat-CVD poly-Si films are found to be promising in solar-cell applications.

The nature of catalyst particles and growth mechanisms of GaN nanowires grown by Ni-assisted metal-organic chemical vapor deposition.

PubMed

Weng, Xiaojun; Burke, Robert A; Redwing, Joan M

2009-02-25

The structure and chemistry of the catalyst particles that terminate GaN nanowires grown by Ni-assisted metal-organic chemical vapor deposition were investigated using a combination of electron diffraction, high-resolution transmission electron microscopy, and x-ray energy dispersive spectrometry. The crystal symmetry, lattice parameter, and chemical composition obtained reveal that the catalyst particles are Ni(3)Ga with an ordered L 1(2) structure. The results suggest that the catalyst is a solid particle during growth and therefore favor a vapor-solid-solid mechanism for the growth of GaN nanowires under these conditions.

Femtosecond pulsed laser deposition of amorphous, ultrahard boride thin films

NASA Astrophysics Data System (ADS)

Stock, Michael; Molian, Pal

2004-05-01

Amorphous thin films (300-500 nm) of ultrahard AlMgB10 with oxygen and carbon impurities were grown on Si (100) substrates at 300 K using a solid target of AlMgB14 containing a spinel phase (MgAl2O4) and using a 120 fs pulsed, 800 nm wavelength Ti:sapphire laser. The films were subsequently annealed in argon gas up to 1373 K for 2 h. Scanning electron microscopy (SEM) was used to examine the particulate formation, atomic force microscopy was employed to characterize the film surface topography, x-ray diffraction and transmission electron microscopy were used to determine the microstructure, x-ray photoelectron spectroscopy was performed to examine the film composition, and nanoindentation was employed to study the hardness of thin films. The as-deposited and postannealed films (up to 1273 K) had a stochiometry of AlMgB10 with a significant amount of oxygen and carbon impurities and exhibited amorphous structures for a maximum hardness of 40+/-3 GPa. However, postannealing at higher temperatures led to crystallization and transformation of the film to SiB6 with a substantial loss in hardness. Results are also compared with our previous study on 23 ns, 248 nm wavelength (KrF excimer) pulsed laser deposition of AlMgB14 reported in this journal [Y. Tian, A. Constant, C. C. H. Lo, J. W. Anderegg, A. M. Russell, J. E. Snyder, and P. A. Molian, J. Vac. Sci. Technol. A 21, 1055 (2003)]. .

Low temperature deposition of nanocrystalline silicon carbide films by plasma enhanced chemical vapor deposition and their structural and optical characterization

NASA Astrophysics Data System (ADS)

Rajagopalan, T.; Wang, X.; Lahlouh, B.; Ramkumar, C.; Dutta, Partha; Gangopadhyay, S.

2003-10-01

Nanocrystalline silicon carbide (SiC) thin films were deposited by plasma enhanced chemical vapor deposition technique at different deposition temperatures (Td) ranging from 80 to 575 °C and different gas flow ratios (GFRs). While diethylsilane was used as the source for the preparation of SiC films, hydrogen, argon and helium were used as dilution gases in different concentrations. The effects of Td, GFR and dilution gases on the structural and optical properties of these films were investigated using high resolution transmission electron microscope (HRTEM), micro-Raman, Fourier transform infrared (FTIR) and ultraviolet-visible optical absorption techniques. Detailed analysis of the FTIR spectra indicates the onset of formation of SiC nanocrystals embedded in the amorphous matrix of the films deposited at a temperature of 300 °C. The degree of crystallization increases with increasing Td and the crystalline fraction (fc) is 65%±2.2% at 575 °C. The fc is the highest for the films deposited with hydrogen dilution in comparison with the films deposited with argon and helium at the same Td. The Raman spectra also confirm the occurrence of crystallization in these films. The HRTEM measurements confirm the existence of nanocrystallites in the amorphous matrix with a wide variation in the crystallite size from 2 to 10 nm. These results are in reasonable agreement with the FTIR and the micro-Raman analysis. The variation of refractive index (n) with Td is found to be quite consistent with the structural evolution of these films. The films deposited with high dilution of H2 have large band gap (Eg) and these values vary from 2.6 to 4.47 eV as Td is increased from 80 to 575 °C. The size dependent shift in the Eg value has also been investigated using effective mass approximation. Thus, the observed large band gap is attributed to the presence of nanocrystallites in the films.

Orally Disintegrating Tablets Containing Melt Extruded Amorphous Solid Dispersion of Tacrolimus for Dissolution Enhancement.

PubMed

Ponnammal, Poovizhi; Kanaujia, Parijat; Yani, Yin; Ng, Wai Kiong; Tan, Reginald B H

2018-03-16

In order to improve the aqueous solubility and dissolution of Tacrolimus (TAC), amorphous solid dispersions of TAC were prepared by hot melt extrusion with three hydrophilic polymers, Polyvinylpyrrolidone vinyl acetate (PVP VA64), Soluplus ® and Hydroxypropyl Cellulose (HPC), at a drug loading of 10% w / w . Molecular modeling was used to determine the miscibility of the drug with the carrier polymers by calculating the Hansen Solubility Parameters. Powder X-ray diffraction and differential scanning calorimetry (DSC) studies of powdered solid dispersions revealed the conversion of crystalline TAC to amorphous form. Fourier transform Infrared (FTIR) spectroscopy results indicated formation of hydrogen bond between TAC and polymers leading to stabilization of TAC in amorphous form. The extrudates were found to be stable under accelerated storage conditions for 3 months with no re-crystallization, indicating that hot melt extrusion is suitable for producing stable amorphous solid dispersions of TAC in PVP VA64, Soluplus ® and HPC. Stable solid dispersions of amorphous TAC exhibited higher dissolution rate, with the solid dispersions releasing more than 80% drug in 15 min compared to the crystalline drug giving 5% drug release in two hours. These stable solid dispersions were incorporated into orally-disintegrating tablets in which the solid dispersion retained its solubility, dissolution and stability advantage.

Orally Disintegrating Tablets Containing Melt Extruded Amorphous Solid Dispersion of Tacrolimus for Dissolution Enhancement

PubMed Central

Ponnammal, Poovizhi; Kanaujia, Parijat; Ng, Wai Kiong; Tan, Reginald B. H.

2018-01-01

In order to improve the aqueous solubility and dissolution of Tacrolimus (TAC), amorphous solid dispersions of TAC were prepared by hot melt extrusion with three hydrophilic polymers, Polyvinylpyrrolidone vinyl acetate (PVP VA64), Soluplus® and Hydroxypropyl Cellulose (HPC), at a drug loading of 10% w/w. Molecular modeling was used to determine the miscibility of the drug with the carrier polymers by calculating the Hansen Solubility Parameters. Powder X-ray diffraction and differential scanning calorimetry (DSC) studies of powdered solid dispersions revealed the conversion of crystalline TAC to amorphous form. Fourier transform Infrared (FTIR) spectroscopy results indicated formation of hydrogen bond between TAC and polymers leading to stabilization of TAC in amorphous form. The extrudates were found to be stable under accelerated storage conditions for 3 months with no re-crystallization, indicating that hot melt extrusion is suitable for producing stable amorphous solid dispersions of TAC in PVP VA64, Soluplus® and HPC. Stable solid dispersions of amorphous TAC exhibited higher dissolution rate, with the solid dispersions releasing more than 80% drug in 15 min compared to the crystalline drug giving 5% drug release in two hours. These stable solid dispersions were incorporated into orally-disintegrating tablets in which the solid dispersion retained its solubility, dissolution and stability advantage. PMID:29547585

On the Plasticity of Amorphous Solids

NASA Astrophysics Data System (ADS)

Lin, Jie

Mechanical behaviors of amorphous materials under external stress are central to various phenomena including earthquakes and landslides. Most amorphous materials possess a well defined yield stress when thermal fluctuations are negligible. Only when the shear stress is above the yield stress, the material can flow as a fluid, otherwise it deforms as a solid. There are accumulating evidences that the yielding transition between the flowing and solid phase is a critical phenomenon, and one evidence is the long ranged correlations of plastic strain during adiabatic shear. In spite of this, we still have not fully understood the associated critical exponents and their scaling relations. In the last decade, it has been widely accepted that the elementary rearrangements in amorphous solids are not well-defined topological defects as crystals, instead they are local irreversible rearrangements of a few particles, denoted as shear transformations. Because a single shear transformation changes the local arrangement of particles, it therefore generates an elastic stress field propagating over the whole system. The resulting changes in the local stresses in other regions of the system may in turn trigger more shear transformations. A central feature that complicates the yielding transition is the long range and anisotropic stress field generated by shear transformations. This peculiar interaction between shear transformations leads to two important characteristics: 1.the mechanical noises generated by plastic deformation are broadly distributed 2.those regions that are undergoing plastic deformation has equal probability to make other parts of the material to be more stable or more unstable, depending on the direction between them. In this thesis, we show that these two important factors leads to a singular density of shear transformations, P( x) xtheta at small x, where x is a local measure of stability, namely, the extra stress one needs to add locally to reach the elastic

Yield stress in amorphous solids: A mode-coupling-theory analysis

NASA Astrophysics Data System (ADS)

Ikeda, Atsushi; Berthier, Ludovic

2013-11-01

The yield stress is a defining feature of amorphous materials which is difficult to analyze theoretically, because it stems from the strongly nonlinear response of an arrested solid to an applied deformation. Mode-coupling theory predicts the flow curves of materials undergoing a glass transition and thus offers predictions for the yield stress of amorphous solids. We use this approach to analyze several classes of disordered solids, using simple models of hard-sphere glasses, soft glasses, and metallic glasses for which the mode-coupling predictions can be directly compared to the outcome of numerical measurements. The theory correctly describes the emergence of a yield stress of entropic nature in hard-sphere glasses, and its rapid growth as density approaches random close packing at qualitative level. By contrast, the emergence of solid behavior in soft and metallic glasses, which originates from direct particle interactions is not well described by the theory. We show that similar shortcomings arise in the description of the caging dynamics of the glass phase at rest. We discuss the range of applicability of mode-coupling theory to understand the yield stress and nonlinear rheology of amorphous materials.

Optical multilayers with an amorphous fluoropolymer

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

Chow, R.; Loomis, G.E.; Lindsey, E.F.

1994-07-01

Multilayered coatings were made by physical vapor deposition (PVD) of a perfluorinated amorphous polymer, Teflon AF2400, together with other optical materials. A high reflector at 1064 run was made with ZnS and AF2400. An all-organic 1064-nm reflector was made from AF2400 and polyethylene. Oxide (HfO{sub 2}, SiO{sub 2}) compatibility was also tested. Each multilayer system adhered to itself. The multilayers were influenced by coating stress and unintentional temperature rises during PVD deposition.

Moire-Fringe Images of Twin Boundaries in Chemical Vapor Deposited Diamond

DTIC Science & Technology

1992-07-10

Moire-Fringe Images of Twin Boundaries in Chemical Vapor Deposited Diamond IJ PERSONAL AUITHOR(S) - D. Shechtman. A. Fldman, M.D. Vaudin, and J.L...micrographs of chemical vapor deposited diamond can be interprete as Moire fringes that occur when viewing twin boundaries that are inclined to the electron...Dist J Special TECHNICAL REPORT No. 14 eca MOIRE-FRINGE IMAGES OF TWIN BOUNDARIES IN CHEMICAL VAPOR DEPOSITED DIAMOND D. Shechtman, A. Feldman, M.D

Comparison of a model vapor deposited glass films to equilibrium glass films

NASA Astrophysics Data System (ADS)

Flenner, Elijah; Berthier, Ludovic; Charbonneau, Patrick; Zamponi, Francesco

Vapor deposition of particles onto a substrate held at around 85% of the glass transition temperature can create glasses with increased density, enthalpy, kinetic stability, and mechanical stability compared to an ordinary glass created by cooling. It is estimated that an ordinary glass would need to age thousands of years to reach the kinetic stability of a vapor deposited glass, and a natural question is how close to the equilibrium is the vapor deposited glass. To understand the process, algorithms akin to vapor deposition are used to create simulated glasses that have a higher kinetic stability than their annealed counterpart, although these glasses may not be well equilibrated either. Here we use novel models optimized for a swap Monte Carlo algorithm in order to create equilibrium glass films and compare their properties with those of glasses obtained from vapor deposition algorithms. This approach allows us to directly assess the non-equilibrium nature of vapor-deposited ultrastable glasses. Simons Collaboration on Cracking the Glass Problem and NSF Grant No. DMR 1608086.

Hybrid Physical Vapor Deposition Instrument for Advanced Functional Multilayers and Materials

DTIC Science & Technology

2016-04-27

Hybrid Physical Vapor Deposition Instrument for Advanced Functional Multilayers and Materials PI Maria received support to construct a physical...vapor deposition (PVD) system that combines electron beam (e- beam) evaporation, magnetron sputtering, pulsed laser ablation, and ion-assisted deposition ...The instrumentation enables clean, uniform, and rapid deposition of a wide variety of metallic, semiconducting, and ceramic thin films with

Instantaneous formation of SiOx nanocomposite for high capacity lithium ion batteries by enhanced disproportionation reaction during plasma spray physical vapor deposition.

PubMed

Tashiro, Tohru; Dougakiuchi, Masashi; Kambara, Makoto

2016-01-01

Nanocomposite SiO x particles have been produced by a single step plasma spray physical vapor deposition (PS-PVD) through rapid condensation of SiO vapors and the subsequent disproportionation reaction. Core-shell nanoparticles, in which 15 nm crystalline Si is embedded within the amorphous SiO x matrix, form under typical PS-PVD conditions, while 10 nm amorphous particles are formed when processed with an increased degree of non-equilibrium effect. Addition of CH 4 promotes reduction in the oxygen content x of SiO x , and thereby increases the Si volume in a nanocomposite particle. As a result, core-shell nanoparticles with x  = 0.46 as anode exhibit increased initial efficiency and the capacity of lithium ion batteries while maintaining cyclability. Furthermore, it is revealed that the disproportionation reaction of SiO is promoted in nanosized particles attaining increased Si diffusivity by two orders of magnitude compared to that in bulk, which facilitates instantaneous composite nanoparticle formation during PS-PVD.

Instantaneous formation of SiOx nanocomposite for high capacity lithium ion batteries by enhanced disproportionation reaction during plasma spray physical vapor deposition

PubMed Central

Tashiro, Tohru; Dougakiuchi, Masashi; Kambara, Makoto

2016-01-01

Abstract Nanocomposite SiOx particles have been produced by a single step plasma spray physical vapor deposition (PS-PVD) through rapid condensation of SiO vapors and the subsequent disproportionation reaction. Core-shell nanoparticles, in which 15 nm crystalline Si is embedded within the amorphous SiOx matrix, form under typical PS-PVD conditions, while 10 nm amorphous particles are formed when processed with an increased degree of non-equilibrium effect. Addition of CH4 promotes reduction in the oxygen content x of SiOx, and thereby increases the Si volume in a nanocomposite particle. As a result, core-shell nanoparticles with x = 0.46 as anode exhibit increased initial efficiency and the capacity of lithium ion batteries while maintaining cyclability. Furthermore, it is revealed that the disproportionation reaction of SiO is promoted in nanosized particles attaining increased Si diffusivity by two orders of magnitude compared to that in bulk, which facilitates instantaneous composite nanoparticle formation during PS-PVD. PMID:27933114

The Effects of Polymer Carrier, Hot Melt Extrusion Process and Downstream Processing Parameters on the Moisture Sorption Properties of Amorphous Solid Dispersions

PubMed Central

Feng, Xin; Vo, Anh; Patil, Hemlata; Tiwari, Roshan V.; Alshetaili, Abdullah S.; Pimparade, Manjeet B.; Repka, Michael A.

2017-01-01

Objective The aim of this study was to evaluate the effect of polymer carrier, hot melt extrusion (HME) and downstream processing parameters on the water uptake properties of amorphous solid dispersions. Methods Three polymers and a model drug were used to prepare amorphous solid dispersions utilizing HME technology. The sorption-desorption isotherms of solid dispersions and their physical mixtures were measured by the Dynamic Vapor Sorption system, and the effect of polymer hydrophobicity, hygroscopicity, molecular weight and the HME process were investigated. FTIR imaging was performed to understand the phase separation driven by the moisture. Key findings Solid dispersions with polymeric carriers with lower hydrophilicity, hygroscopicity, and higher molecular weight could sorb less moisture under the high RH conditions. The water uptake ability of polymer-drug solid dispersion systems were decreased compared to the physical mixture after HME, which might be due to the decreased surface area and porosity. The FTIR imaging indicated the homogeneity of the drug molecularly dispersed within the polymer matrix was changed after exposure to high RH. Conclusion Understanding the effect of formulation and processing on the moisture sorption properties of solid dispersions is essential for the development of drug products with desired physical and chemical stability. PMID:26589107

Solvent Vapor Annealing of Amorphous Carbamazepine Films for Fast Polymorph Screening and Dissolution Alteration.

PubMed

Schrode, Benedikt; Bodak, Brigitta; Riegler, Hans; Zimmer, Andreas; Christian, Paul; Werzer, Oliver

2017-09-30

Solubility enhancement and thus higher bioavailability are of great importance and a constant challenge in pharmaceutical research whereby polymorph screening and selection is one of the most important tasks. A very promising approach for polymorph screening is solvent vapor annealing where a sample is exposed to an atmosphere saturated with molecules of a specific chemical/solvent. In this work, amorphous carbamazepine thin films were prepared by spin coating, and the transformation into crystalline forms under exposure to solvent vapors was investigated. Employing grazing incidence X-ray diffraction, four distinct carbamazepine polymorphs, a solvate, and hydrates could be identified, while optical microscopy showed mainly spherulitic morphologies. In vitro dissolution experiments revealed different carbamazepine release from the various thin-film samples containing distinct polymorphic compositions: heat treatment of amorphous samples at 80 °C results in an immediate release; samples exposed to EtOH vapors show a drug release about 5 times slower than this immediate one; and all the others had intermediate release profiles. Noteworthy, even the sample of slowest release has a manifold faster release compared to a standard powder sample demonstrating the capabilities of thin-film preparation for faster drug release in general. Despite the small number of samples in this screening experiment, the results clearly show how solvent vapor annealing can assist in identifying potential polymorphs and allows for estimating their impact on properties like bioavailability.

Vacuum vapor deposition: A spinoff of space welding development

NASA Technical Reports Server (NTRS)

Poorman, R. M.

1991-01-01

A vapor deposition process has been defined through a spinoff effort of space welding development. In this development for welding in a space environment, a hollow electrode was used to add gas precisely at the welding arc. This provides gas for ionization which carries the welding arc current. During this welding development metal vapor coatings were observed. These coatings are unique in that they are produced by a new process. Some coatings produced and the potential of this new and innovative vapor deposition process are characterized. Advantages over prior art are discussed.

Investigation of aluminosilicate as a solid oxide fuel cell refractory

NASA Astrophysics Data System (ADS)

Gentile, Paul S.; Sofie, Stephen W.

2011-05-01

Aluminosilicate represents a potential low cost alternative to alumina for solid oxide fuel cell (SOFC) refractory applications. The objectives of this investigation are to study: (1) changes of aluminosilicate chemistry and morphology under SOFC conditions, (2) deposition of aluminosilicate vapors on yttria stabilized zirconia (YSZ) and nickel, and (3) effects of aluminosilicate vapors on SOFC electrochemical performance. Thermal treatment of aluminosilicate under high temperature SOFC conditions is shown to result in increased mullite concentrations at the surface due to diffusion of silicon from the bulk. Water vapor accelerates the rate of surface diffusion resulting in a more uniform distribution of silicon. The high temperature condensation of volatile gases released from aluminosilicate preferentially deposit on YSZ rather than nickel. Silicon vapor deposited on YSZ consists primarily of aluminum rich clusters enclosed in an amorphous siliceous layer. Increased concentrations of silicon are observed in enlarged grain boundaries indicating separation of YSZ grains by insulating glassy phase. The presence of aluminosilicate powder in the hot zone of a fuel line supplying humidified hydrogen to an SOFC anode impeded peak performance and accelerated degradation. Energy dispersive X-ray spectroscopy detected concentrations of silicon at the interface between the electrolyte and anode interlayer above impurity levels.

Chemical vapor deposition of mullite coatings

DOEpatents

Sarin, Vinod; Mulpuri, Rao

1998-01-01

This invention is directed to the creation of crystalline mullite coatings having uniform microstructure by chemical vapor deposition (CVD). The process comprises the steps of establishing a flow of reactants which will yield mullite in a CVD reactor, and depositing a crystalline coating from the reactant flow. The process will yield crystalline coatings which are dense and of uniform thickness.

Deposition of naphthalene and tetradecane vapors in models of the human respiratory system.

PubMed

Zhang, Zhe; Kleinstreuer, Clement

2011-01-01

Jet-propulsion fuel (particularly JP-8) is currently being used worldwide, exposing especially Air Force personnel and people living near airfields to JP-8 vapors and aerosols during aircraft fueling, maintenance operations, and/or cold starts. JP-8 is a complex mixture containing >200, mostly toxic, aliphatic and aromatic hydrocarbon compounds of which tetradecane and naphthalene were chosen as two representative chemical markers for computer simulations. Thus, transport and deposition of naphthalene and tetradecane vapors have been simulated in models of the human respiratory system. The inspiratory deposition data were analyzed in terms of regional deposition fractions (DFs) and deposition enhancement factors (DEF). The vapor depositions are affected by vapor properties (e.g. diffusivity), airway geometric features, breathing patterns, inspiratory flow rates, as well as airway-wall absorption parameter. Specifically, the respiratory uptake of vapors is greatly influenced by the degree of airway-wall absorption. For example, being an almost insoluble species in the mucus layer, the deposition of tetradecane vapor is nearly zero in the extrathoracic and tracheobronchial (TB) airways, that is, the DF is <1%. The remaining vapors may penetrate further and deposit in the alveolar airways. The DF of tetradecane vapors during inhalation in the alveolar region can range from 7% to 24%, depending on breathing waveform, inhalation rate, and thickness of the mucus layer. In contrast, naphthalene vapor almost completely deposits in the extrathoracic and TB airways and hardly moves downstream and deposits in the respiratory zone. The DFs of naphthalene vapor in the extrathoracic airways from nasal/oral to trachea under normal breathing conditions (Q = 15-60 L/min) are about 12-34%, although they are about 66-87% in the TB airways. In addition, the variation of breathing routes (say, from nasal breathing to oral breathing) may influence the vapor deposition in the

Structural Coloration of a Colloidal Amorphous Array is Intensified by Carbon Nanolayers.

PubMed

Takeoka, Yukikazu; Iwata, Masanori; Seki, Takahiro; Nueangnoraj, Khanin; Nishihara, Hirotomo; Yoshioka, Shinya

2018-04-10

In this study, we introduce the possibility of applying a colloidal amorphous array composed of fine silica particles as a structural-color material to invisible information technology. The appearance of a thick filmlike colloidal amorphous array formed from fine silica particles is considerably influenced by incoherent light scattering across the entire visible region. Therefore, regardless of the diameter of the fine silica particles, the thick colloidal amorphous array exhibits a white color to the naked eye. When carbon is uniformly deposited in the colloidal amorphous array by a pressure-pulsed chemical vapor deposition method, incoherent light scattering in the colloidal amorphous array is suppressed. As a result, coherent light scattering due to the short-range order in the colloidal amorphous array becomes conspicuous and the array exhibits a vivid structural color. As structures, such as letters and pictures, can be drawn using this technology, the colloidal amorphous array as a structural-colored material may also be applicable for invisible information technology.

Chemical vapor deposition of silicon, silicon dioxide, titanium and ferroelectric thin films

NASA Astrophysics Data System (ADS)

Chen, Feng

Various silicon-based thin films (such as epitaxial, polycrystalline and amorphous silicon thin films, silicon dioxide thin films and silicon nitride thin films), titanium thin film and various ferroelectric thin films (such as BaTiO3 and PbTiO3 thin films) play critical roles in the manufacture of microelectronics circuits. For the past few years, there have been tremendous interests to search for cheap, safe and easy-to-use methods to develop those thin films with high quality and good step coverage. Silane is a critical chemical reagent widely used to deposit silicon-based thin films. Despite its wide use, silane is a dangerous material. It is pyrophoric, extremely flammable and may explode from heat, shock and/or friction. Because of the nature of silane, serious safety issues have been raised concerning the use, transportation, and storage of compressed gas cylinders of silane. Therefore it is desired to develop safer ways to deposit silicon-based films. In chapter III, I present the results of our research in the following fields: (1) Silane generator, (2) Substitutes of silane for deposition of silicon and silicon dioxide thin films, (3) Substitutes of silane for silicon dioxide thin film deposition. In chapter IV, hydropyridine is introduced as a new ligand for use in constructing precursors for chemical vapor deposition. Detachement of hydropyridine occurs by a low-temperature reaction leaving hydrogen in place of the hydropyridine ligands. Hydropyridine ligands can be attached to a variety of elements, including main group metals, such as aluminum and antimony, transition metals, such as titanium and tantalum, semiconductors such as silicon, and non-metals such as phosphorus and arsenic. In this study, hydropyridine-containing titanium compounds were synthesized and used as chemical vapor deposition precursors for deposition of titanium containing thin films. Some other titanium compounds were also studied for comparison. In chapter V, Chemical Vapor

Simple Chemical Vapor Deposition Experiment

ERIC Educational Resources Information Center

Pedersen, Henrik

2014-01-01

Chemical vapor deposition (CVD) is a process commonly used for the synthesis of thin films for several important technological applications, for example, microelectronics, hard coatings, and smart windows. Unfortunately, the complexity and prohibitive cost of CVD equipment makes it seldom available for undergraduate chemistry students. Here, a…

Amorphous silicon as high index photonic material

NASA Astrophysics Data System (ADS)

Lipka, T.; Harke, A.; Horn, O.; Amthor, J.; Müller, J.

2009-05-01

Silicon-on-Insulator (SOI) photonics has become an attractive research topic within the area of integrated optics. This paper aims to fabricate SOI-structures for optical communication applications with lower costs compared to standard fabrication processes as well as to provide a higher flexibility with respect to waveguide and substrate material choice. Amorphous silicon is deposited on thermal oxidized silicon wafers with plasma-enhanced chemical vapor deposition (PECVD). The material is optimized in terms of optical light transmission and refractive index. Different a-Si:H waveguides with low propagation losses are presented. The waveguides were processed with CMOS-compatible fabrication technologies and standard DUV-lithography enabling high volume production. To overcome the large mode-field diameter mismatch between incoupling fiber and sub-μm waveguides three dimensional, amorphous silicon tapers were fabricated with a KOH etched shadow mask for patterning. Using ellipsometric and Raman spectroscopic measurements the material properties as refractive index, layer thickness, crystallinity and material composition were analyzed. Rapid thermal annealing (RTA) experiments of amorphous thin films and rib waveguides were performed aiming to tune the refractive index of the deposited a-Si:H waveguide core layer after deposition.

Structural transition in sputter-deposited amorphous germanium films by aging at ambient temperature

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

Okugawa, M.; Nakamura, R., E-mail: nakamura@mtr.osakafu-u.ac.jp; Numakura, H.

The structure of amorphous Ge (a-Ge) films prepared by sputter-deposition and the effects of aging at ambient temperature and pressure were studied by pair-distribution-function (PDF) analysis from electron scattering and molecular dynamics simulations. The PDFs of the as-deposited and aged samples for 3–13 months showed that the major peaks for Ge-Ge bonds decrease in intensity and broaden with aging for up to 7 months. In the PDFs of a-Ge of molecular dynamics simulation obtained by quenching liquid at different rates, the major peak intensities of a slowly cooled model are higher than those of a rapidly cooled model. Analyses onmore » short- and medium-range configurations show that the slowly cooled model includes a certain amount of medium-range ordered (MRO) clusters, while the rapidly cooled model includes liquid-like configurations rather than MRO clusters. The similarity between experimental and computational PDFs implies that as-deposited films are similar in structure to the slowly cooled model, whereas the fully aged films are similar to the rapidly cooled model. It is assumed that as they undergo room-temperature aging, the MRO clusters disintegrate and transform into liquid-like regions in the same matrix. This transition in local configurations is discussed in terms of instability and the non-equilibrium of nanoclusters produced by a vapor-deposition process.« less

Electrochemical vapor deposition of semiconductors from gas phase with a solid membrane cell.

PubMed

Cho, Sung Ki; Fan, Fu-Ren F; Bard, Allen J

2015-05-27

We demonstrate the feasibility of semiconductor deposition via the electrochemical reduction of gaseous precursors by the use of an anhydrous proton-conducting membrane, the solid acid CsHSO4, at 165 °C. This membrane electrode assembly was operated within the oxidation of hydrogen on a porous Pt anode and the deposition of Si or Ge under bias at the cathode from chloride-based gaseous precursors; SiCl4 and GeCl4 in an Ar flow with a reduction potential over -1.0 V (vs RHE).

Characterization of thin film deposits on tungsten filaments in catalytic chemical vapor deposition using 1,1-dimethylsilacyclobutane

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

Shi, Yujun, E-mail: shiy@ucalgary.ca; Tong, Ling; Mulmi, Suresh

Metal filament plays a key role in the technique of catalytic chemical vapor deposition (Cat-CVD) as it serves as a catalyst in dissociating the source gas to form reactive species. These reactive species initiate the gas-phase reaction chemistry and final thin film and nanostructure formation. At the same time, they also react with the metal itself, leading to the formation of metal alloys and other deposits. The deposits on the tungsten filaments when exposed to 1,1-dimethylsilacyclobutane (DMSCB), a single-source precursor for silicon carbide thin films, in the process of Cat-CVD were studied in this work. It has been demonstrated thatmore » a rich variety of deposits, including tungsten carbides (W{sub 2}C and WC), tungsten silicide (W{sub 5}Si{sub 3}), silicon carbide, amorphous carbon, and graphite, form on the W filament surfaces. The structural and morphological changes in the tungsten filaments depend strongly on the DMSCB pressure and filament temperature. At 1000 and 2000 °C, the formation of WC and W{sub 2}C dominates. In addition, a thin amorphous carbon layer has been found at 1500 °C with the 0.12 and 0.24 Torr of DMSCB and a lower temperature of 1200 °C with the 0.48 Torr of DMSCB. An increase in the DMSCB sample pressure gives rise to higher Si and C contents. As a result, the formation of SiC and W{sub 5}Si{sub 3} has been observed with the two high-pressure DMSCB samples (i.e., 0.24 and 0.48 Torr). The rich decomposition chemistry of DMSCB on the W surfaces is responsible for the extensive changes in the structure of the W filament, providing support for the close relationship between the gas-phase decomposition chemistry and the nature of alloy formation on the metal surface. The understanding of the structural changes obtained from this work will help guide the development of efficient methods to solve the filament aging problem in Cat-CVD and also to achieve a controllable deposition process.« less

Substrate temperature controls molecular orientation in two-component vapor-deposited glasses

DOE PAGES

Jiang, J.; Walters, D. M.; Zhou, D.; ...

2016-02-22

Vapor-deposited glasses can be anisotropic and molecular orientation is important for organic electronics applications. In organic light emitting diodes (OLEDs), for example, the orientation of dye molecules in two-component emitting layers significantly influences emission efficiency. Here we investigate how substrate temperature during vapor deposition influences the orientation of dye molecules in a model two-component system. We determine the average orientation of a linear blue light emitter 1,4-di-[4-( N,N-diphenyl)amino]styrylbenzene (DSA-Ph) in mixtures with aluminum-tris(8-hydroxyquinoline) (Alq 3) by spectroscopic ellipsometry and IR dichroism. We find that molecular orientation is controlled by the ratio of the substrate temperature during deposition and the glassmore » transition temperature of the mixture. Furthermore, these findings extend recent results for single component vapor-deposited glasses and suggest that, during vapor deposition, surface mobility allows partial equilibration towards orientations preferred at the free surface of the equilibrium liquid.« less

Chemical vapor deposition reactor. [providing uniform film thickness

NASA Technical Reports Server (NTRS)

Chern, S. S.; Maserjian, J. (Inventor)

1977-01-01

An improved chemical vapor deposition reactor is characterized by a vapor deposition chamber configured to substantially eliminate non-uniformities in films deposited on substrates by control of gas flow and removing gas phase reaction materials from the chamber. Uniformity in the thickness of films is produced by having reactive gases injected through multiple jets which are placed at uniformally distributed locations. Gas phase reaction materials are removed through an exhaust chimney which is positioned above the centrally located, heated pad or platform on which substrates are placed. A baffle is situated above the heated platform below the mouth of the chimney to prevent downdraft dispersion and scattering of gas phase reactant materials.

Chemical vapor deposition of epitaxial silicon

DOEpatents

Berkman, Samuel

1984-01-01

A single chamber continuous chemical vapor deposition (CVD) reactor is described for depositing continuously on flat substrates, for example, epitaxial layers of semiconductor materials. The single chamber reactor is formed into three separate zones by baffles or tubes carrying chemical source material and a carrier gas in one gas stream and hydrogen gas in the other stream without interaction while the wafers are heated to deposition temperature. Diffusion of the two gas streams on heated wafers effects the epitaxial deposition in the intermediate zone and the wafers are cooled in the final zone by coolant gases. A CVD reactor for batch processing is also described embodying the deposition principles of the continuous reactor.

Formation of amorphous materials

DOEpatents

Johnson, William L.; Schwarz, Ricardo B.

1986-01-01

Metastable amorphous or fine crystalline materials are formed by solid state reactions by diffusion of a metallic component into a solid compound or by diffusion of a gas into an intermetallic compound. The invention can be practiced on layers of metals deposited on an amorphous substrate or by intermixing powders with nucleating seed granules. All that is required is that the diffusion of the first component into the second component be much faster than the self-diffusion of the first component. The method is practiced at a temperature below the temperature at which the amorphous phase transforms into one or more crystalline phases and near or below the temperature at which the ratio of the rate of diffusion of the first component to the rate of self-diffusion is at least 10.sup.4. This anomalous diffusion criteria is found in many binary, tertiary and higher ordered systems of alloys and appears to be found in all alloy systems that form amorphous materials by rapid quenching. The method of the invention can totally convert much larger dimensional materials to amorphous materials in practical periods of several hours or less.

Impact of hydrogen dilution on optical properties of intrinsic hydrogenated amorphous silicon films prepared by high density plasma chemical vapor deposition for solar cell applications

NASA Astrophysics Data System (ADS)

Chen, Huai-Yi; Lee, Yao-Jen; Chang, Chien-Pin; Koo, Horng-Show; Lai, Chiung-Hui

2013-01-01

P-i-n single-junction hydrogenated amorphous silicon (a-Si:H) thin film solar cells were successfully fabricated in this study on a glass substrate by high density plasma chemical vapor deposition (HDP-CVD) at low power of 50 W, low temperature of 200°C and various hydrogen dilution ratios (R). The open circuit voltage (Voc ), short circuit current density (Jsc ), fill factor (FF) and conversion efficiency (η) of the solar cell as well as the refractive index (n) and absorption coefficient (α) of the i-layer at 600 nm wavelength rise with increasing R until an abrupt drop at high hydrogen dilution, i.e. R > 0.95. However, the optical energy bandgap (Eg ) of the i-layer decreases with the R increase. Voc and α are inversely correlated with Eg . The hydrogen content affects the i-layer and p/i interface quality of the a-Si:H thin film solar cell with an optimal value of R = 0.95, which corresponds to solar cell conversion efficiency of 3.85%. The proposed a-Si:H thin film solar cell is expected to be improved in performance.

Protective interlayer for high temperature solid electrolyte electrochemical cells

DOEpatents

Isenberg, Arnold O.; Ruka, Roswell J.

1986-01-01

A high temperature, solid electrolyte electrochemical cell is made, having a first and second electrode with solid electrolyte between them, where the electrolyte is formed by hot chemical vapor deposition, where a solid, interlayer material, which is electrically conductive, oxygen permeable, and protective of electrode material from hot metal halide vapor attack, is placed between the first electrode and the electrolyte, to protect the first electrode from the hot metal halide vapors during vapor deposition.

Protective interlayer for high temperature solid electrolyte electrochemical cells

DOEpatents

Isenberg, Arnold O.; Ruka, Roswell J.; Zymboly, Gregory E.

1985-01-01

A high temperature, solid electrolyte electrochemical cell is made, having a first and second electrode with solid electrolyte between them, where the electrolyte is formed by hot chemical vapor deposition, where a solid, interlayer material, which is electrically conductive, oxygen permeable, and protective of electrode material from hot metal halide vapor attack, is placed between the first electrode and the electrolyte, to protect the first electrode from the hot metal halide vapors during vapor deposition.

Protective interlayer for high temperature solid electrolyte electrochemical cells

DOEpatents

Isenberg, Arnold O.; Ruka, Roswell J.

1987-01-01

A high temperature, solid electrolyte electrochemical cell is made, having a first and second electrode with solid electrolyte between them, where the electrolyte is formed by hot chemical vapor deposition, where a solid, interlayer material, which is electrically conductive, oxygen permeable, and protective of electrode material from hot metal halide vapor attack, is placed between the first electrode and the electrolyte, to protect the first electrode from the hot metal halide vapors during vapor deposition.

Vacuum vapor deposition gun assembly

DOEpatents

Zeren, Joseph D.

1985-01-01

A vapor deposition gun assembly includes a hollow body having a cylindrical outer surface and an end plate for holding an adjustable heat sink, a hot hollow cathode gun, two magnets for steering the plasma from the gun into a crucible on the heat sink, and a shutter for selectively covering and uncovering the crucible.

A solid-state nuclear magnetic resonance study of post-plasma reactions in organosilicone microwave plasma-enhanced chemical vapor deposition (PECVD) coatings.

PubMed

Hall, Colin J; Ponnusamy, Thirunavukkarasu; Murphy, Peter J; Lindberg, Mats; Antzutkin, Oleg N; Griesser, Hans J

2014-06-11

Plasma-polymerized organosilicone coatings can be used to impart abrasion resistance and barrier properties to plastic substrates such as polycarbonate. Coating rates suitable for industrial-scale deposition, up to 100 nm/s, can be achieved through the use of microwave plasma-enhanced chemical vapor deposition (PECVD), with optimal process vapors such as tetramethyldisiloxane (TMDSO) and oxygen. However, it has been found that under certain deposition conditions, such coatings are subject to post-plasma changes; crazing or cracking can occur anytime from days to months after deposition. To understand the cause of the crazing and its dependence on processing plasma parameters, the effects of post-plasma reactions on the chemical bonding structure of coatings deposited with varying TMDSO-to-O2 ratios was studied with (29)Si and (13)C solid-state magic angle spinning nuclear magnetic resonance (MAS NMR) using both single-pulse and cross-polarization techniques. The coatings showed complex chemical compositions significantly altered from the parent monomer. (29)Si MAS NMR spectra revealed four main groups of resonance lines, which correspond to four siloxane moieties (i.e., mono (M), di (D), tri (T), and quaternary (Q)) and how they are bound to oxygen. Quantitative measurements showed that the ratio of TMDSO to oxygen could shift the chemical structure of the coating from 39% to 55% in Q-type bonds and from 28% to 16% for D-type bonds. Post-plasma reactions were found to produce changes in relative intensities of (29)Si resonance lines. The NMR data were complemented by Fourier transform infrared (FTIR) spectroscopy. Together, these techniques have shown that the bonding environment of Si is drastically altered by varying the TMDSO-to-O2 ratio during PECVD, and that post-plasma reactions increase the cross-link density of the silicon-oxygen network. It appears that Si-H and Si-OH chemical groups are the most susceptible to post-plasma reactions. Coatings produced at a

Stochastic approach to plasticity and yield in amorphous solids.

PubMed

Hentschel, H G E; Jaiswal, Prabhat K; Procaccia, Itamar; Sastry, Srikanth

2015-12-01

We focus on the probability distribution function (PDF) P(Δγ;γ) where Δγ are the measured strain intervals between plastic events in a athermal strained amorphous solids, and γ measures the accumulated strain. The tail of this distribution as Δγ→0 (in the thermodynamic limit) scales like Δγ(η). The exponent η is related via scaling relations to the tail of the PDF of the eigenvalues of the plastic modes of the Hessian matrix P(λ) which scales like λ(θ), η=(θ-1)/2. The numerical values of η or θ can be determined easily in the unstrained material and in the yielded state of plastic flow. Special care is called for in the determination of these exponents between these states as γ increases. Determining the γ dependence of the PDF P(Δγ;γ) can shed important light on plasticity and yield. We conclude that the PDF's of both Δγ and λ are not continuous functions of γ. In slowly quenched amorphous solids they undergo two discontinuous transitions, first at γ=0(+) and then at the yield point γ=γ(Y) to plastic flow. In quickly quenched amorphous solids the second transition is smeared out due to the nonexisting stress peak before yield. The nature of these transitions and scaling relations with the system size dependence of 〈Δγ〉 are discussed.

Comparison of InGaAs(100) Grown by Chemical Beam Epitaxy and Metal Organic Chemical Vapor Deposition

NASA Technical Reports Server (NTRS)

Williams, M. D.; Greene, A. L.; Daniels-Race, T.; Lum, R. M.

2000-01-01

Secondary ion mass spectrometry is used to study the effects of substrate temperature on the composition and growth rate of InGaAs/InP(100) multilayers grown by chemical beam epitaxy, metal-organic chemical vapor deposition and solid source molecular beam epitaxy. The growth kinetics of the material grown by the different techniques are analyzed and compared.

Interface amorphization in hexagonal boron nitride films on sapphire substrate grown by metalorganic vapor phase epitaxy

NASA Astrophysics Data System (ADS)

Yang, Xu; Nitta, Shugo; Pristovsek, Markus; Liu, Yuhuai; Nagamatsu, Kentaro; Kushimoto, Maki; Honda, Yoshio; Amano, Hiroshi

2018-05-01

Hexagonal boron nitride (h-BN) films directly grown on c-plane sapphire substrates by pulsed-mode metalorganic vapor phase epitaxy exhibit an interlayer for growth temperatures above 1200 °C. Cross-sectional transmission electron microscopy shows that this interlayer is amorphous, while the crystalline h-BN layer above has a distinct orientational relationship with the sapphire substrate. Electron energy loss spectroscopy shows the energy-loss peaks of B and N in both the amorphous interlayer and the overlying crystalline h-BN layer, while Al and O signals are also seen in the amorphous interlayer. Thus, the interlayer forms during h-BN growth through the decomposition of the sapphire at elevated temperatures.

Solar-induced chemical vapor deposition of diamond-type carbon films

DOEpatents

Pitts, J.R.; Tracy, C.E.; King, D.E.; Stanley, J.T.

1994-09-13

An improved chemical vapor deposition method for depositing transparent continuous coatings of sp[sup 3]-bonded diamond-type carbon films, comprises: (a) providing a volatile hydrocarbon gas/H[sub 2] reactant mixture in a cold wall vacuum/chemical vapor deposition chamber containing a suitable substrate for said films, at pressure of about 1 to 50 Torr; and (b) directing a concentrated solar flux of from about 40 to about 60 watts/cm[sup 2] through said reactant mixture to produce substrate temperatures of about 750 C to about 950 C to activate deposition of the film on said substrate. 11 figs.

Solar-induced chemical vapor deposition of diamond-type carbon films

DOEpatents

Pitts, J. Roland; Tracy, C. Edwin; King, David E.; Stanley, James T.

1994-01-01

An improved chemical vapor deposition method for depositing transparent continuous coatings of sp.sup.3 -bonded diamond-type carbon films, comprising: a) providing a volatile hydrocarbon gas/H.sub.2 reactant mixture in a cold wall vacuum/chemical vapor deposition chamber containing a suitable substrate for said films, at pressure of about 1 to 50 Torr; and b) directing a concentrated solar flux of from about 40 to about 60 watts/cm.sup.2 through said reactant mixture to produce substrate temperatures of about 750.degree. C. to about 950.degree. C. to activate deposition of the film on said substrate.

Low temperature deposition of polycrystalline silicon thin films on a flexible polymer substrate by hot wire chemical vapor deposition

NASA Astrophysics Data System (ADS)

Lee, Sang-hoon; Jung, Jae-soo; Lee, Sung-soo; Lee, Sung-bo; Hwang, Nong-moon

2016-11-01

For the applications such as flexible displays and solar cells, the direct deposition of crystalline silicon films on a flexible polymer substrate has been a great issue. Here, we investigated the direct deposition of polycrystalline silicon films on a polyimide film at the substrate temperature of 200 °C. The low temperature deposition of crystalline silicon on a flexible substrate has been successfully made based on two ideas. One is that the Si-Cl-H system has a retrograde solubility of silicon in the gas phase near the substrate temperature. The other is the new concept of non-classical crystallization, where films grow by the building block of nanoparticles formed in the gas phase during hot-wire chemical vapor deposition (HWCVD). The total amount of precipitation of silicon nanoparticles decreased with increasing HCl concentration. By adding HCl, the amount and the size of silicon nanoparticles were reduced remarkably, which is related with the low temperature deposition of silicon films of highly crystalline fraction with a very thin amorphous incubation layer. The dark conductivity of the intrinsic film prepared at the flow rate ratio of RHCl=[HCl]/[SiH4]=3.61 was 1.84×10-6 Scm-1 at room temperature. The Hall mobility of the n-type silicon film prepared at RHCl=3.61 was 5.72 cm2 V-1s-1. These electrical properties of silicon films are high enough and could be used in flexible electric devices.

One-step microwave plasma enhanced chemical vapor deposition (MW-PECVD) for transparent superhydrophobic surface

NASA Astrophysics Data System (ADS)

Thongrom, Sukrit; Tirawanichakul, Yutthana; Munsit, Nantakan; Deangngam, Chalongrat

2018-02-01

We demonstrate a rapid and environmental friendly fabrication technique to produce optically clear superhydrophobic surfaces using poly (dimethylsiloxane) (PDMS) as a sole coating material. The inert PDMS chain is transformed into a 3-D irregular solid network through microwave plasma enhanced chemical vapor deposition (MW-PECVD) process. Thanks to high electron density in the microwave-activated plasma, coating can be done in just a single step with rapid deposition rate, typically much shorter than 10 s. Deposited layers show excellent superhydrophobic properties with water contact angles of ∼170° and roll-off angles as small as ∼3°. The plasma-deposited films can be ultrathin with thicknesses under 400 nm, greatly diminishing the optical loss. Moreover, with appropriate coating conditions, the coating layer can even enhance the transmission over the entire visible spectrum due to a partial anti-reflection effect.

Method of depositing wide bandgap amorphous semiconductor materials

DOEpatents

Ellis, Jr., Frank B.; Delahoy, Alan E.

1987-09-29

A method of depositing wide bandgap p type amorphous semiconductor materials on a substrate without photosensitization by the decomposition of one or more higher order gaseous silanes in the presence of a p-type catalytic dopant at a temperature of about 200.degree. C. and a pressure in the range from about 1-50 Torr.

Effects of thermal annealing on the structural, mechanical, and tribological properties of hard fluorinated carbon films deposited by plasma enhanced chemical vapor deposition

NASA Astrophysics Data System (ADS)

Maia da Costa, M. E. H.; Baumvol, I. J. R.; Radke, C.; Jacobsohn, L. G.; Zamora, R. R. M.; Freire, F. L.

2004-11-01

Hard amorphous fluorinated carbon films (a-C:F) deposited by plasma enhanced chemical vapor deposition were annealed in vacuum for 30 min in the temperature range of 200-600 °C. The structural and compositional modifications were followed by several analytical techniques: Rutherford backscattering spectrometry (RBS), elastic recoil detection analysis (ERDA), x-ray photoelectron spectroscopy (XPS) and Raman spectroscopy. Nanoidentation measurements and lateral force microscopy experiments were carried out in order to provide the film hardness and the friction coefficient, respectively. The internal stress and contact angle were also measured. RBS, ERDA, and XPS results indicate that both fluorine and hydrogen losses occur for annealing temperatures higher than 300 °C. Raman spectroscopy shows a progressive graphitization upon annealing, while the surface became slightly more hydrophobic as revealed by the increase of the contact angle. Following the surface wettability reduction, a decrease of the friction coefficient was observed. These results highlight the influence of the capillary condensation on the nanoscale friction. The film hardness and the internal stress are constant up to 300 °C and decrease for higher annealing temperatures, showing a direct correlation with the atomic density of the films. Since the thickness variation is negligible, the mass loss upon thermal treatment results in amorphous structures with a lower degree of cross-linking, explaining the deterioration of the mechanical properties of the a-C:F films.

Phase Behavior of Ritonavir Amorphous Solid Dispersions during Hydration and Dissolution.

PubMed

Purohit, Hitesh S; Taylor, Lynne S

2017-12-01

The aim of this research was to study the interplay of solid and solution state phase transformations during the dissolution of ritonavir (RTV) amorphous solid dispersions (ASDs). RTV ASDs with polyvinylpyrrolidone (PVP), polyvinylpyrrolidone vinyl acetate (PVPVA) and hydroxypropyl methylcellulose acetate succinate (HPMCAS) were prepared at 10-50% drug loading by solvent evaporation. The miscibility of RTV ASDs was studied before and after exposure to 97% relative humidity (RH). Non-sink dissolution studies were performed on fresh and moisture-exposed ASDs. RTV and polymer release were monitored using ultraviolet-visible spectroscopy. Techniques including fluorescence spectroscopy, confocal imaging, scanning electron microscopy (SEM), atomic force microscopy (AFM), differential scanning calorimetry (DSC) and nanoparticle tracking analysis (NTA) were utilized to monitor solid and the solution state phase transformations. All RTV-PVP and RTV-PVPVA ASDs underwent moisture-induced amorphous-amorphous phase separation (AAPS) on high RH storage whereas RTV-HPMCAS ASDs remained miscible. Non-sink dissolution of PVP- and PVPVA-based ASDs at low drug loadings led to rapid RTV and polymer release resulting in concentrations in excess of amorphous solubility, liquid-liquid phase separation (LLPS) and amorphous nanodroplet formation. High drug loading PVP- and PVPVA-based ASDs did not exhibit LLPS upon dissolution as a consequence of extensive AAPS in the hydrated ASD matrix. All RTV-HPMCAS ASDs led to LLPS upon dissolution. RTV ASD dissolution is governed by a competition between the dissolution rate and the rate of phase separation in the hydrated ASD matrix. LLPS was observed for ASDs where the drug release was polymer controlled and only ASDs that remained miscible during the initial phase of dissolution led to LLPS. Techniques such as fluorescence spectroscopy, confocal imaging and SEM were useful in understanding the phase behavior of ASDs upon hydration and dissolution

Enthalpy and high temperature relaxation kinetics of stable vapor-deposited glasses of toluene

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

Bhattacharya, Deepanjan; Sadtchenko, Vlad, E-mail: vlad@gwu.edu

Stable non-crystalline toluene films of micrometer and nanometer thicknesses were grown by vapor deposition at distinct rates and probed by fast scanning calorimetry. Fast scanning calorimetry is shown to be extremely sensitive to the structure of the vapor-deposited phase and was used to characterize simultaneously its kinetic stability and its thermodynamic properties. According to our analysis, transformation of vapor-deposited samples of toluene during heating with rates in excess 10{sup 5} K s{sup −1} follows the zero-order kinetics. The transformation rate correlates strongly with the initial enthalpy of the sample, which increases with the deposition rate according to sub-linear law. Analysismore » of the transformation kinetics of vapor-deposited toluene films of various thicknesses reveal a sudden increase in the transformation rate for films thinner than 250 nm. The change in kinetics seems to correlate with the surface roughness scale of the substrate. The implications of these findings for the formation mechanism and structure of vapor-deposited stable glasses are discussed.« less

Nano-Crystalline Diamond Films with Pineapple-Like Morphology Grown by the DC Arcjet vapor Deposition Method

NASA Astrophysics Data System (ADS)

Li, Bin; Zhang, Qin-Jian; Shi, Yan-Chao; Li, Jia-Jun; Li, Hong; Lu, Fan-Xiu; Chen, Guang-Chao

2014-08-01

A nano-crystlline diamond film is grown by the dc arcjet chemical vapor deposition method. The film is characterized by scanning electron microscopy, high-resolution transmission electron microscopy (HRTEM), x-ray diffraction (XRD) and Raman spectra, respectively. The nanocrystalline grains are averagely with 80 nm in the size measured by XRD, and further proven by Raman and HRTEM. The observed novel morphology of the growth surface, pineapple-like morphology, is constructed by cubo-octahedral growth zones with a smooth faceted top surface and coarse side surfaces. The as-grown film possesses (100) dominant surface containing a little amorphous sp2 component, which is far different from the nano-crystalline film with the usual cauliflower-like morphology.

Amorphous and nanocrystalline luminescent Si and Ge obtained via a solid-state chemical metathesis synthesis route

NASA Astrophysics Data System (ADS)

McMillan, Paul F.; Gryko, Jan; Bull, Craig; Arledge, Richard; Kenyon, Anthony J.; Cressey, Barbara A.

2005-03-01

A new solid-state metathesis synthesis route was applied to obtain bulk samples of amorphous or microcrystalline Si and Ge. The method involves reaction of Zintl phases such as NaSi or NaGe, with ammonium or metal (e.g., CuCl, CoBr 2) halides. The driving force for the solid-state reaction is provided by the formation of alkali halides and the transition metals or metal silicides, or gaseous ammonia and hydrogen. The semiconductors were purified by washing to remove other solid products. The amorphous semiconductors were obtained in bulk form from reactions carried out at 200-300 °C. Syntheses at higher temperatures gave rise to microcrystalline semiconductors, or to micro-/nanocrystalline particles contained within the amorphous material. Similar crystalline/amorphous composites were obtained after heat treatment of bulk amorphous materials.

Aerosol-Assisted Chemical Vapor Deposited Thin Films for Space Photovoltaics

NASA Technical Reports Server (NTRS)

Hepp, Aloysius F.; McNatt, Jeremiah; Dickman, John E.; Jin, Michael H.-C.; Banger, Kulbinder K.; Kelly, Christopher V.; AquinoGonzalez, Angel R.; Rockett, Angus A.

2006-01-01

Copper indium disulfide thin films were deposited via aerosol-assisted chemical vapor deposition using single source precursors. Processing and post-processing parameters were varied in order to modify morphology, stoichiometry, crystallography, electrical properties, and optical properties in order to optimize device-quality material. Growth at atmospheric pressure in a horizontal hot-wall reactor at 395 C yielded best device films. Placing the susceptor closer to the evaporation zone and flowing a more precursor-rich carrier gas through the reactor yielded shinier, smoother, denser-looking films. Growth of (112)-oriented films yielded more Cu-rich films with fewer secondary phases than growth of (204)/(220)-oriented films. Post-deposition sulfur-vapor annealing enhanced stoichiometry and crystallinity of the films. Photoluminescence studies revealed four major emission bands (1.45, 1.43, 1.37, and 1.32 eV) and a broad band associated with deep defects. The highest device efficiency for an aerosol-assisted chemical vapor deposited cell was 1.03 percent.

Electron beam physical vapor deposition of thin ruby films for remote temperature sensing

NASA Astrophysics Data System (ADS)

Li, Wei; Coppens, Zachary J.; Greg Walker, D.; Valentine, Jason G.

2013-04-01

Thermographic phosphors (TGPs) possessing temperature-dependent photoluminescence properties have a wide range of uses in thermometry due to their remote access and large temperature sensitivity range. However, in most cases, phosphors are synthesized in powder form, which prevents their use in high resolution micro and nanoscale thermal microscopy. In the present study, we investigate the use of electron beam physical vapor deposition to fabricate thin films of chromium-doped aluminum oxide (Cr-Al2O3, ruby) thermographic phosphors. Although as-deposited films were amorphous and exhibited weak photoluminescence, the films regained the stoichiometry and α-Al2O3 crystal structure of the combustion synthesized source powder after thermal annealing. As a consequence, the annealed films exhibit both strong photoluminescence and a temperature-dependent lifetime that decreases from 2.9 ms at 298 K to 2.1 ms at 370 K. Ruby films were also deposited on multiple substrates. To ensure a continuous film with smooth surface morphology and strong photoluminescence, we use a sapphire substrate, which is thermal expansion coefficient and lattice matched to the film. These thin ruby films can potentially be used as remote temperature sensors for probing the local temperatures of micro and nanoscale structures.

Finite Element Analysis Modeling of Chemical Vapor Deposition of Silicon Carbide

DTIC Science & Technology

2014-06-19

thesis primarily focuses on mass transport by gas -phase flow and diffusion , chemical reaction in gas phase and on solid surfaces, and thin film...chemical vapor deposition (CVD). This thesis primarily focuses on mass transport by gas -phase flow and diffusion , chemical reaction in gas phase and...9 Fluid Flow…………………………………………..…………………..…………….9 Thermodynamics………………………………………..………………….….…….11 Chemical Reaction and Diffusion

Shock wave induced vaporization of porous solids

NASA Astrophysics Data System (ADS)

Shen, Andy H.; Ahrens, Thomas J.; O'Keefe, John D.

2003-05-01

Strong shock waves generated by hypervelocity impact can induce vaporization in solid materials. To pursue knowledge of the chemical species in the shock-induced vapors, one needs to design experiments that will drive the system to such thermodynamic states that sufficient vapor can be generated for investigation. It is common to use porous media to reach high entropy, vaporized states in impact experiments. We extended calculations by Ahrens [J. Appl. Phys. 43, 2443 (1972)] and Ahrens and O'Keefe [The Moon 4, 214 (1972)] to higher distentions (up to five) and improved their method with a different impedance match calculation scheme and augmented their model with recent thermodynamic and Hugoniot data of metals, minerals, and polymers. Although we reconfirmed the competing effects reported in the previous studies: (1) increase of entropy production and (2) decrease of impedance match, when impacting materials with increasing distentions, our calculations did not exhibit optimal entropy-generating distention. For different materials, very different impact velocities are needed to initiate vaporization. For aluminum at distention (m)<2.2, a minimum impact velocity of 2.7 km/s is required using tungsten projectile. For ionic solids such as NaCl at distention <2.2, 2.5 km/s is needed. For carbonate and sulfate minerals, the minimum impact velocities are much lower, ranging from less than 1 to 1.5 km/s.

Solid state amorphization of nanocrystalline nickel by cryogenic laser shock peening

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

Ye, Chang, E-mail: cye@uakron.edu; Ren, Zhencheng; Zhao, Jingyi

2015-10-07

In this study, complete solid state amorphization in nanocrystalline nickel has been achieved through cryogenic laser shock peening (CLSP). High resolution transmission electron microscopy has revealed the complete amorphous structure of the sample after CLSP processing. A molecular dynamic model has been used to investigate material behavior during the shock loading and the effects of nanoscale grain boundaries on the amorphization process. It has been found that the initial nanoscale grain boundaries increase the initial Gibbs free energy before plastic deformation and also serve as dislocation emission sources during plastic deformation to contribute to defect density increase, leading to themore » amorphization of pure nanocrystalline nickel.« less

Solid-state amorphization of rebamipide and investigation on solubility and stability of the amorphous form.

PubMed

Xiong, Xinnuo; Xu, Kailin; Li, Shanshan; Tang, Peixiao; Xiao, Ying; Li, Hui

2017-02-01

Solid-state amorphization of crystalline rebamipide (RBM) was realized by ball milling and spray drying. The amorphous content of samples milled for various time was quantified using X-ray powder diffraction. Crystalline RBM and three amorphous RBM obtained by milling and spray drying were characterized by morphological analysis, X-ray diffraction, thermal analysis and vibrational spectroscopy. The crystal structure of RBM was first determined by single-crystal X-ray diffraction. In addition, the solubility and dissolution rate of the RBM samples were investigated in different media. Results indicated that the solubility and the dissolution rates of spray-dried RBM-PVP in different media were highly improved compared with crystalline RBM. The physical stabilities of the three amorphous RBM were systematically investigated, and the stability orders under different storage temperatures and levels of relative humidity (RH) were both as follows: spray dried RBM < milled RBM < spray dried RBM-PVP. A direct glass-to-crystal transformation was induced under high RH, and the transformation rate rose with increasing RH. However, amorphous RBM could stay stable at RH levels lower than 57.6% (25 °C).

Amorphous and nanocrystalline luminescent Si and Ge obtained via a solid-state chemical metathesis synthesis route

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

McMillan, Paul F.; Gryko, Jan; Bull, Craig

A new solid-state metathesis synthesis route was applied to obtain bulk samples of amorphous or microcrystalline Si and Ge. The method involves reaction of Zintl phases such as NaSi or NaGe, with ammonium or metal (e.g., CuCl, CoBr{sub 2}) halides. The driving force for the solid-state reaction is provided by the formation of alkali halides and the transition metals or metal silicides, or gaseous ammonia and hydrogen. The semiconductors were purified by washing to remove other solid products. The amorphous semiconductors were obtained in bulk form from reactions carried out at 200-300{sup o}C. Syntheses at higher temperatures gave rise tomore » microcrystalline semiconductors, or to micro-/nanocrystalline particles contained within the amorphous material. Similar crystalline/amorphous composites were obtained after heat treatment of bulk amorphous materials.« less

Electrical Characterization of Irradiated Semiconducting Amorphous Hydrogenated Boron Carbide

NASA Astrophysics Data System (ADS)

Peterson, George Glenn

Semiconducting amorphous partially dehydrogenated boron carbide has been explored as a neutron voltaic for operation in radiation harsh environments, such as on deep space satellites/probes. A neutron voltaic device could also be used as a solid state neutron radiation detector to provide immediate alerts for radiation workers/students, as opposed to the passive dosimetry badges utilized today. Understanding how the irradiation environment effects the electrical properties of semiconducting amorphous partially dehydrogenated boron carbide is important to predicting the stability of these devices in operation. p-n heterojunction diodes were formed from the synthesis of semiconducting amorphous partially dehydrogenated boron carbide on silicon substrates through the use of plasma enhanced chemical vapor deposition (PECVD). Many forms of structural and electrical measurements and analysis have been performed on the p-n heterojunction devices as a function of both He+ ion and neutron irradiation including: transmission electron microscopy (TEM), selected area electron diffraction (SAED), current versus voltage I(V), capacitance versus voltage C(V), conductance versus frequency G(f), and charge carrier lifetime (tau). In stark contrast to nearly all other electronic devices, the electrical performance of these p-n heterojunction diodes improved with irradiation. This is most likely the result of bond defect passivation and resolution of degraded icosahedral based carborane structures (icosahedral molecules missing a B, C, or H atom(s)).

Integrated atomic layer deposition and chemical vapor reaction for the preparation of metal organic framework coatings for solid-phase microextraction Arrow.

PubMed

Lan, Hangzhen; Salmi, Leo D; Rönkkö, Tuukka; Parshintsev, Jevgeni; Jussila, Matti; Hartonen, Kari; Kemell, Marianna; Riekkola, Marja-Liisa

2018-09-18

New chemical vapor reaction (CVR) and atomic layer deposition (ALD)-conversion methods were utilized for preparation of metal organic frameworks (MOFs) coatings of solid phase microextraction (SPME) Arrow for the first time. With simple, easy and convenient one-step reaction or conversion, four MOF coatings were made by suspend ALD iron oxide (Fe 2 O 3 ) film or aluminum oxide (Al 2 O 3 ) film above terephthalic acid (H 2 BDC) or trimesic acid (H 3 BTC) vapor. UIO-66 coating was made by zirconium (Zr)-BDC film in acetic acid vapor. As the first documented instance of all-gas phase synthesis of SPME Arrow coatings, preparation parameters including CVR/conversion time and temperature, acetic acid volume, and metal oxide film/metal-ligand films thickness were investigated. The optimal coatings exhibited crystalline structures, excellent uniformity, satisfactory thickness (2-7.5 μm), and high robustness (>80 times usage). To study the practical usefulness of the coatings for the extraction, several analytes with different chemical properties were tested. The Fe-BDC coating was found to be the most selective and sensitive for the determination of benzene ring contained compounds due to its highly hydrophobic surface and unsaturated metal site. UIO-66 coating was best for small polar, aromatic, and long chain polar compounds owing to its high porosity. The usefulness of new coatings were evaluated for gas chromatography-mass spectrometer (GC-MS) determination of several analytes, present in wastewater samples at three levels of concentration, and satisfactory results were achieved. Copyright © 2018 Elsevier B.V. All rights reserved.

Friction and Wear of Ion-Beam-Deposited Diamondlike Carbon on Chemical-Vapor-Deposited, Fine-Grain Diamond

NASA Technical Reports Server (NTRS)

Miyoshi, Kazuhisa; Wu, Richard L. C.; Lanter, William C.

1996-01-01

Friction and wear behavior of ion-beam-deposited diamondlike carbon (DLC) films coated on chemical-vapor-deposited (CVD), fine-grain diamond coatings were examined in ultrahigh vacuum, dry nitrogen, and humid air environments. The DLC films were produced by the direct impact of an ion beam (composed of a 3:17 mixture of Ar and CH4) at ion energies of 1500 and 700 eV and an RF power of 99 W. Sliding friction experiments were conducted with hemispherical CVD diamond pins sliding on four different carbon-base coating systems: DLC films on CVD diamond; DLC films on silicon; as-deposited, fine-grain CVD diamond; and carbon-ion-implanted, fine-grain CVD diamond on silicon. Results indicate that in ultrahigh vacuum the ion-beam-deposited DLC films on fine-grain CVD diamond (similar to the ion-implanted CVD diamond) greatly decrease both the friction and wear of fine-grain CVD diamond films and provide solid lubrication. In dry nitrogen and in humid air, ion-beam-deposited DLC films on fine-grain CVD diamond films also had a low steady-state coefficient of friction and a low wear rate. These tribological performance benefits, coupled with a wider range of coating thicknesses, led to longer endurance life and improved wear resistance for the DLC deposited on fine-grain CVD diamond in comparison to the ion-implanted diamond films. Thus, DLC deposited on fine-grain CVD diamond films can be an effective wear-resistant, lubricating coating regardless of environment.

High-harmonic generation in amorphous solids

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

You, Yong Sing; Yin, Yanchun; Wu, Yi

High-harmonic generation in isolated atoms and molecules has been widely utilized in extreme ultraviolet photonics and attosecond pulse metrology. Recently, high-harmonic generation has been observed in solids, which could lead to important applications such as all-optical methods to image valance charge density and reconstruct electronic band structures, as well as compact extreme ultraviolet light sources. So far these studies are confined to crystalline solids; therefore, decoupling the respective roles of long-range periodicity and high density has been challenging. Here we report the observation of high-harmonic generation from amorphous fused silica. We also decouple the role of long-range periodicity by comparingmore » harmonics generated from fused silica and crystalline quartz, which contain the same atomic constituents but differ in long-range periodicity. These results advance current understanding of the strong-field processes leading to high-harmonic generation in solids with implications for the development of robust and compact extreme ultraviolet light sources.« less

High-harmonic generation in amorphous solids

DOE PAGES

You, Yong Sing; Yin, Yanchun; Wu, Yi; ...

2017-09-28

High-harmonic generation in isolated atoms and molecules has been widely utilized in extreme ultraviolet photonics and attosecond pulse metrology. Recently, high-harmonic generation has been observed in solids, which could lead to important applications such as all-optical methods to image valance charge density and reconstruct electronic band structures, as well as compact extreme ultraviolet light sources. So far these studies are confined to crystalline solids; therefore, decoupling the respective roles of long-range periodicity and high density has been challenging. Here we report the observation of high-harmonic generation from amorphous fused silica. We also decouple the role of long-range periodicity by comparingmore » harmonics generated from fused silica and crystalline quartz, which contain the same atomic constituents but differ in long-range periodicity. These results advance current understanding of the strong-field processes leading to high-harmonic generation in solids with implications for the development of robust and compact extreme ultraviolet light sources.« less

Reversibility and criticality in amorphous solids

DOE PAGES

Regev, Ido; Weber, John; Reichhardt, Charles; ...

2015-11-13

The physical processes governing the onset of yield, where a material changes its shape permanently under external deformation, are not yet understood for amorphous solids that are intrinsically disordered. Here, using molecular dynamics simulations and mean-field theory, we show that at a critical strain amplitude the sizes of clusters of atoms undergoing cooperative rearrangements of displacements (avalanches) diverges. We compare this non-equilibrium critical behaviour to the prevailing concept of a ‘front depinning’ transition that has been used to describe steady-state avalanche behaviour in different materials. We explain why a depinning-like process can result in a transition from periodic to chaoticmore » behaviour and why chaotic motion is not possible in pinned systems. As a result, these findings suggest that, at least for highly jammed amorphous systems, the irreversibility transition may be a side effect of depinning that occurs in systems where the disorder is not quenched.« less

Flash vaporization during earthquakes evidenced by gold deposits

NASA Astrophysics Data System (ADS)

Weatherley, Dion K.; Henley, Richard W.

2013-04-01

Much of the world's known gold has been derived from arrays of quartz veins. The veins formed during periods of mountain building that occurred as long as 3 billion years ago, and were deposited by very large volumes of water that flowed along deep, seismically active faults. The veins formed under fluctuating pressures during earthquakes, but the magnitude of the pressure fluctuations and their influence on mineral deposition is not known. Here we use a simple thermo-mechanical piston model to calculate the drop in fluid pressure experienced by a fluid-filled fault cavity during an earthquake. The geometry of the model is constrained using measurements of typical fault jogs, such as those preserved in the Revenge gold deposit in Western Australia, and other gold deposits around the world. We find that cavity expansion generates extreme reductions in pressure that cause the fluid that is trapped in the jog to expand to a very low-density vapour. Such flash vaporization of the fluid results in the rapid co-deposition of silica with a range of trace elements to form gold-enriched quartz veins. Flash vaporization continues as more fluid flows towards the newly expanded cavity, until the pressure in the cavity eventually recovers to ambient conditions. Multiple earthquakes progressively build economic-grade gold deposits.

A low-energy metal-ion source for primary ion deposition and accelerated ion doping during molecular-beam epitaxy

NASA Astrophysics Data System (ADS)

Hasan, M.-A.; Knall, J.; Barnett, S. A.; Rockett, A.; Sundgren, J.-E.

1987-10-01

A single-grid electron-impact ultrahigh vacuum (UHV) compatible low-energy ion gun capable of operating with a low vapor pressure solid source material such as In is presented. The gun consists of a single chamber which integrates the functions of an effusion cell, a vapor transport tube, and a glow discharge ionizer. The initial results of experiments designed to study the role of ion/surface interactions during nucleation and the early stages of crystal growth in UHV revealed that, for deposition on amorphous substrates, the use of a partially ionized In(+) beam resulted in a progressive shift towards larger island sizes, a decreased rate of secondary nucleation, and a more uniform island size distribution.

Phase transitions of amorphous solid acetone in confined geometry investigated by reflection absorption infrared spectroscopy.

PubMed

Shin, Sunghwan; Kang, Hani; Kim, Jun Soo; Kang, Heon

2014-11-26

We investigated the phase transformations of amorphous solid acetone under confined geometry by preparing acetone films trapped in amorphous solid water (ASW) or CCl4. Reflection absorption infrared spectroscopy (RAIRS) and temperature-programmed desorption (TPD) were used to monitor the phase changes of the acetone sample with increasing temperature. An acetone film trapped in ASW shows an abrupt change in the RAIRS features of the acetone vibrational bands during heating from 80 to 100 K, which indicates the transformation of amorphous solid acetone to a molecularly aligned crystalline phase. Further heating of the sample to 140 K produces an isotropic solid phase, and eventually a fluid phase near 157 K, at which the acetone sample is probably trapped in a pressurized, superheated condition inside the ASW matrix. Inside a CCl4 matrix, amorphous solid acetone crystallizes into a different, isotropic structure at ca. 90 K. We propose that the molecularly aligned crystalline phase formed in ASW is created by heterogeneous nucleation at the acetone-water interface, with resultant crystal growth, whereas the isotropic crystalline phase in CCl4 is formed by homogeneous crystal growth starting from the bulk region of the acetone sample.

Effects of phosphorus on the electrical characteristics of plasma deposited hydrogenated amorphous silicon carbide thin films

NASA Astrophysics Data System (ADS)

Alcinkaya, Burak; Sel, Kivanc

2018-01-01

The properties of phosphorus doped hydrogenated amorphous silicon carbide (a-SiCx:H) thin films, that were deposited by plasma enhanced chemical vapor deposition technique with four different carbon contents (x), were analyzed and compared with those of the intrinsic a-SiCx:H thin films. The carbon contents of the films were determined by X-ray photoelectron spectroscopy. The thickness and optical energies, such as Tauc, E04 and Urbach energies, of the thin films were determined by UV-Visible transmittance spectroscopy. The electrical properties of the films, such as conductivities and activation energies were analyzed by temperature dependent current-voltage measurements. Finally, the conduction mechanisms of the films were investigated by numerical analysis, in which the standard transport mechanism in the extended states and the nearest neighbor hopping mechanism in the band tail states were taken into consideration. It was determined that, by the effect of phosphorus doping the dominant conduction mechanism was the standard transport mechanism for all carbon contents.

Electron-rich driven electrochemical solid-state amorphization in Li-Si alloys.

PubMed

Wang, Zhiguo; Gu, Meng; Zhou, Yungang; Zu, Xiaotao; Connell, Justin G; Xiao, Jie; Perea, Daniel; Lauhon, Lincoln J; Bang, Junhyeok; Zhang, Shengbai; Wang, Chongmin; Gao, Fei

2013-09-11

The physical and chemical behaviors of materials used in energy storage devices, such as lithium-ion batteries (LIBs), are mainly controlled by an electrochemical process, which normally involves insertion/extraction of ions into/from a host lattice with a concurrent flow of electrons to compensate charge balance. The fundamental physics and chemistry governing the behavior of materials in response to the ions insertion/extraction is not known. Herein, a combination of in situ lithiation experiments and large-scale ab initio molecular dynamics simulations are performed to explore the mechanisms of the electrochemically driven solid-state amorphization in Li-Si systems. We find that local electron-rich condition governs the electrochemically driven solid-state amorphization of Li-Si alloys. This discovery provides the fundamental explanation of why lithium insertion in semiconductor and insulators leads to amorphization, whereas in metals, it leads to a crystalline alloy. The present work correlates electrochemically driven reactions with ion insertion, electron transfer, lattice stability, and phase equilibrium.

Electron-Rich Driven Electrochemical Solid-State Amorphization in Li-Si Alloys

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

Wang, Zhiguo; Gu, Meng; Zhou, Yungang

2013-08-14

The physical and chemical behaviors of materials used in energy storage devices, such as lithium-ion batteries (LIBs), are mainly controlled by an electrochemical process, which normally involves insertion/extraction of ions into/from a host lattice with a concurrent flow of electrons to compensate charge balance. The fundamental physics and chemistry governing the behavior of materials in response to the ions insertion/extraction is not known. Herein, a combination of in situ lithiation experiments and large-scale ab initio molecular dynamics simulations are performed to explore the mechanisms of the electrochemically driven solid-state amorphization in Li-Si systems. We find that local electron-rich condition governsmore » the electrochemically driven solid-state amorphization of Li-Si alloys. This discovery provides the fundamental explanation of why lithium insertion in semiconductor and insulators leads to amorphization, whereas in metals, it leads to a crystalline alloy. The present work correlates electrochemically driven reactions with ion insertion, electron transfer, lattice stability and phase equilibrium.« less

Chemical vapor deposition for automatic processing of integrated circuits

NASA Technical Reports Server (NTRS)

Kennedy, B. W.

1980-01-01

Chemical vapor deposition for automatic processing of integrated circuits including the wafer carrier and loading from a receiving air track into automatic furnaces and unloading on to a sending air track is discussed. Passivation using electron beam deposited quartz is also considered.

Plasma-deposited amorphous hydrogenated carbon films and their tribological properties

NASA Technical Reports Server (NTRS)

Miyoshi, Kazuhisa; Pouch, John J.; Alterovitz, Samuel A.

1989-01-01

Recent work on the properties of diamondlike carbon films and their dependence on preparation conditions are reviewed. The results of the study indicate that plasma deposition enables one to deposit a variety of amorphous hydrogenated carbon (a-C:H ) films exhibiting more diamondlike behavior to more graphitic behavior. The plasma-deposited a-C:H can be effectively used as hard, wear-resistant, and protective lubricating films on ceramic materials such as Si(sub 3)N(sub 4) under a variety of environmental conditions such as moist air, dry nitrogrn, and vacuum.

In vitro characterization of a novel polymeric system for preparation of amorphous solid drug dispersions.

PubMed

Mahmoudi, Zahra N; Upadhye, Sampada B; Ferrizzi, David; Rajabi-Siahboomi, Ali R

2014-07-01

Preparation of amorphous solid dispersions using polymers is a commonly used formulation strategy for enhancing the solubility of poorly water-soluble drugs. However, often a single polymer may not bring about a significant enhancement in solubility or amorphous stability of a poorly water-soluble drug. This study describes application of a unique and novel binary polymeric blend in preparation of solid dispersions. The objective of this study was to investigate amorphous solid dispersions of glipizide, a BCS class II model drug, in a binary polymeric system of polyvinyl acetate phthalate (PVAP) and hypromellose (hydroxypropyl methylcellulose, HPMC). The solid dispersions were prepared using two different solvent methods: rotary evaporation (rotavap) and fluid bed drug layering on sugar spheres. The performance and physical stability of the dispersions were evaluated with non-sink dissolution testing, powder X-ray diffraction (PXRD), and modulated differential scanning calorimetry (mDSC). PXRD analysis demonstrated an amorphous state for glipizide, and mDSC showed no evidence of phase separation. Non-sink dissolution testing in pH 7.5 phosphate buffer indicated more than twofold increase in apparent solubility of the drug with PVAP-HPMC system. The glipizide solid dispersions demonstrated a high glass transition temperature (Tg) and acceptable chemical and physical stability during the stability period irrespective of the manufacturing process. In conclusion, the polymeric blend of PVAP-HPMC offers a unique formulation approach for developing amorphous solid dispersions with the flexibility towards the use of these polymers in different ratios and combined quantities depending on drug properties.

Theory of amorphous ices.

PubMed

Limmer, David T; Chandler, David

2014-07-01

We derive a phase diagram for amorphous solids and liquid supercooled water and explain why the amorphous solids of water exist in several different forms. Application of large-deviation theory allows us to prepare such phases in computer simulations. Along with nonequilibrium transitions between the ergodic liquid and two distinct amorphous solids, we establish coexistence between these two amorphous solids. The phase diagram we predict includes a nonequilibrium triple point where two amorphous phases and the liquid coexist. Whereas the amorphous solids are long-lived and slowly aging glasses, their melting can lead quickly to the formation of crystalline ice. Further, melting of the higher density amorphous solid at low pressures takes place in steps, transitioning to the lower-density glass before accessing a nonequilibrium liquid from which ice coarsens.

Theory of amorphous ices

PubMed Central

Limmer, David T.; Chandler, David

2014-01-01

We derive a phase diagram for amorphous solids and liquid supercooled water and explain why the amorphous solids of water exist in several different forms. Application of large-deviation theory allows us to prepare such phases in computer simulations. Along with nonequilibrium transitions between the ergodic liquid and two distinct amorphous solids, we establish coexistence between these two amorphous solids. The phase diagram we predict includes a nonequilibrium triple point where two amorphous phases and the liquid coexist. Whereas the amorphous solids are long-lived and slowly aging glasses, their melting can lead quickly to the formation of crystalline ice. Further, melting of the higher density amorphous solid at low pressures takes place in steps, transitioning to the lower-density glass before accessing a nonequilibrium liquid from which ice coarsens. PMID:24858957

Nanoscale amorphization of GeTe nanowire with conductive atomic force microscope.

PubMed

Kim, JunHo

2014-10-01

We fabricated GeTe nanowires by using Au catalysis mediated vapor-liquid-solid method. The fabricated nanowires were confirmed by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. For a nanowire with - 150 nm diameter, we performed amorphization experiment with conductive atomic force microscope. We examined the structural change of the nanowire with several bias voltages from 0 V to 10 V. Above bias voltage of 6-7 V, some points of the nanowire showed transition to amorphous phase. The consumed energy for the amorphization was estimated to be 4-5 nJ, which was close to the other result of nanowire tested with a four probe device.

Research on chemical vapor deposition processes for advanced ceramic coatings

NASA Technical Reports Server (NTRS)

Rosner, Daniel E.

1993-01-01

Our interdisciplinary background and fundamentally-oriented studies of the laws governing multi-component chemical vapor deposition (VD), particle deposition (PD), and their interactions, put the Yale University HTCRE Laboratory in a unique position to significantly advance the 'state-of-the-art' of chemical vapor deposition (CVD) R&D. With NASA-Lewis RC financial support, we initiated a program in March of 1988 that has led to the advances described in this report (Section 2) in predicting chemical vapor transport in high temperature systems relevant to the fabrication of refractory ceramic coatings for turbine engine components. This Final Report covers our principal results and activities for the total NASA grant of $190,000. over the 4.67 year period: 1 March 1988-1 November 1992. Since our methods and the technical details are contained in the publications listed (9 Abstracts are given as Appendices) our emphasis here is on broad conclusions/implications and administrative data, including personnel, talks, interactions with industry, and some known applications of our work.

Photoluminescence of silicon nanowires obtained by epitaxial chemical vapor deposition

NASA Astrophysics Data System (ADS)

Demichel, O.; Oehler, F.; Calvo, V.; Noé, P.; Pauc, N.; Gentile, P.; Ferret, P.; Baron, T.; Magnea, N.

2009-05-01

We have carried out photoluminescence measurements of silicon nanowires (SiNWs) obtained by the chemical vapor deposition method with a copper-catalyzed vapor-liquid-solid mechanism. The nanowires have a typical diameter of 200 nm. Spectrum of the as-grown SiNWs exhibits radiative states below the energy bandgap and a small contribution near the silicon gap energy at 1.08 eV. A thermal oxidation allows to decrease the intensity at low energy and to enhance the intensity of the 1.08 eV contribution. The behavior of this contribution as a function of the pump power is correlated to a free carrier recombination. Furthermore, the spatial confinement of the carriers in SiNWs could explain the difference of shape and recombination energy of this contribution compared to the recombination of free exciton in the bulk silicon. The electronic system seems to be in an electron-hole plasma (ehp), as it has already been shown in SOI structures [M. Tajima, et al., J. Appl. Phys. 84 (1998) 2224]. A simulation of the radiative emission of an ehp is performed and results are discussed.

Infrared analysis of vapor phase deposited tricresylphosphate (TCP)

NASA Technical Reports Server (NTRS)

Morales, Wilfredo; Hanyaloglu, Bengi; Graham, Earl E.

1994-01-01

Infrared transmission was employed to study the formation of a lubricating film deposited on two different substrates at 700 C. The deposit was formed from tricresylphosphate vapors and collected onto a NaCl substrate and on an iron coated NaCl substrate. Analysis of the infrared data suggests that a metal phosphate is formed initially, followed by the formation of organophosphorus polymeric compounds.

Robust, functional nanocrystal solids by infilling with atomic layer deposition.

PubMed

Liu, Yao; Gibbs, Markelle; Perkins, Craig L; Tolentino, Jason; Zarghami, Mohammad H; Bustamante, Jorge; Law, Matt

2011-12-14

Thin films of colloidal semiconductor nanocrystals (NCs) are inherently metatstable materials prone to oxidative and photothermal degradation driven by their large surface-to-volume ratios and high surface energies. (1) The fabrication of practical electronic devices based on NC solids hinges on preventing oxidation, surface diffusion, ripening, sintering, and other unwanted physicochemical changes that can plague these materials. Here we use low-temperature atomic layer deposition (ALD) to infill conductive PbSe NC solids with metal oxides to produce inorganic nanocomposites in which the NCs are locked in place and protected against oxidative and photothermal damage. Infilling NC field-effect transistors and solar cells with amorphous alumina yields devices that operate with enhanced and stable performance for at least months in air. Furthermore, ALD infilling with ZnO lowers the height of the inter-NC tunnel barrier for electron transport, yielding PbSe NC films with electron mobilities of 1 cm2 V(-1) s(-1). Our ALD technique is a versatile means to fabricate robust NC solids for optoelectronic devices.

Multivariate Quantification of the Solid State Phase Composition of Co-Amorphous Naproxen-Indomethacin.

PubMed

Beyer, Andreas; Grohganz, Holger; Löbmann, Korbinian; Rades, Thomas; Leopold, Claudia S

2015-10-27

To benefit from the optimized dissolution properties of active pharmaceutical ingredients in their amorphous forms, co-amorphisation as a viable tool to stabilize these amorphous phases is of both academic and industrial interest. Reports dealing with the physical stability and recrystallization behavior of co-amorphous systems are however limited to qualitative evaluations based on the corresponding X-ray powder diffractograms. Therefore, the objective of the study was to develop a quantification model based on X-ray powder diffractometry (XRPD), followed by a multivariate partial least squares regression approach that enables the simultaneous determination of up to four solid state fractions: crystalline naproxen, γ-indomethacin, α-indomethacin as well as co-amorphous naproxen-indomethacin. For this purpose, a calibration set that covers the whole range of possible combinations of the four components was prepared and analyzed by XRPD. In order to test the model performances, leave-one-out cross validation was performed and revealed root mean square errors of validation between 3.11% and 3.45% for the crystalline molar fractions and 5.57% for the co-amorphous molar fraction. In summary, even four solid state phases, involving one co-amorphous phase, can be quantified with this XRPD data-based approach.

Raman studied of undoped amorphous carbon thin film deposited by bias assisted-CVD

NASA Astrophysics Data System (ADS)

Ishak, A.; Fadzilah, A. N.; Dayana, K.; Saurdi, I.; Malek, M. F.; Nurbaya, Z.; Shafura, A. K.; Rusop, M.

2018-05-01

The undoped amorphous carbon thin film carbon was deposited at 200°C-350°C by bias assisted-CVD using palm oil as a precursor material. The effect of different substrate deposition temperatures on structural and electrical properties of undoped doped amorphous carbon film was discussed. The structural of undoped amorphous carbon films were correlated with Raman analysis through the evolution of D and G bands, Fourier spectra, and conductivity measurement. The spectral evolution observed showed the increase of upward shift of D and G peaks as substrate deposition temperatures increased. The spectral evolution observed at different substrate deposition temperatures show progressive formation of crystallites. It was predicted that small number of hydrogen is terminated with carbon at surface of thin film as shown by FTIR spectra since palm oil has high number of hydrogen (C67H127O8). These structural changes were further correlated with conductivity and the results obtained are discussed and compared. The conductivity is found in the range of 10-8 Scm-1. The increase of conductivity is correlated by the change of structural properties as correlated with characteristic parameters of Raman spectra including the position of G peak, full width at half maximum of G peak, and ID/IG and FTIR result.

Corrosion processes of physical vapor deposition-coated metallic implants.

PubMed

Antunes, Renato Altobelli; de Oliveira, Mara Cristina Lopes

2009-01-01

Protecting metallic implants from the harsh environment of physiological fluids is essential to guaranteeing successful long-term use in a patient's body. Chemical degradation may lead to the failure of an implant device in two different ways. First, metal ions may cause inflammatory reactions in the tissues surrounding the implant and, in extreme cases, these reactions may inflict acute pain on the patient and lead to loosening of the device. Therefore, increasing wear strength is beneficial to the performance of the metallic implant. Second, localized corrosion processes contribute to the nucleation of fatigue cracks, and corrosion fatigue is the main reason for the mechanical failure of metallic implants. Common biomedical alloys such as stainless steel, cobalt-chrome alloys, and titanium alloys are prone to at least one of these problems. Vapor-deposited hard coatings act directly to improve corrosion, wear, and fatigue resistances of metallic materials. The effectiveness of the corrosion protection is strongly related to the structure of the physical vapor deposition layer. The aim of this paper is to present a comprehensive review of the correlation between the structure of physical vapor deposition layers and the corrosion properties of metallic implants.

Modeling Physical Stability of Amorphous Solids Based on Temperature and Moisture Stresses.

PubMed

Zhu, Donghua Alan; Zografi, George; Gao, Ping; Gong, Yuchuan; Zhang, Geoff G Z

2016-09-01

Isothermal microcalorimetry was utilized to monitor the crystallization process of amorphous ritonavir (RTV) and its hydroxypropylmethylcellulose acetate succinate-based amorphous solid dispersion under various stressed conditions. An empirical model was developed: ln(τ)=ln(A)+EaRT-b⋅wc, where τ is the crystallization induction period, A is a pre-exponential factor, Ea is the apparent activation energy, b is the moisture sensitivity parameter, and wc is water content. To minimize the propagation of errors associated with the estimates, a nonlinear approach was used to calculate mean estimates and confidence intervals. The physical stability of neat amorphous RTV and RTV in hydroxypropylmethylcellulose acetate succinate solid dispersions was found to be mainly governed by the nucleation kinetic process. The impact of polymers and moisture on the crystallization process can be quantitatively described by Ea and b in this Arrhenius-type model. The good agreement between the measured values under some less stressful test conditions and those predicted, reflected by the slope and R(2) of the correlation plot of these 2 sets of data on a natural logarithm scale, indicates its predictability of long-term physical stability of amorphous RTV in solid dispersions. To further improve the model, more understanding of the impact of temperature and moisture on the amorphous physical stability and fundamentals regarding nucleation and crystallization is needed. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

CuInS2 Films Deposited by Aerosol-Assisted Chemical Vapor Deposition Using Ternary Single-Source Precursors

NASA Technical Reports Server (NTRS)

Jin, Michael; Banger, Kal; Harris, Jerry; Hepp, Aloysius

2003-01-01

Polycrystalline CuInS2 films were deposited by aerosol-assisted chemical vapor deposition using both solid and liquid ternary single-source precursors (SSPs) which were prepared in-house. Films with either (112) or (204/220) preferred orientation, had a chalcopyrite structure, and (112)-oriented films contained more copper than (204/220)-oriented films. The preferred orientation of the film is likely related to the decomposition and reaction kinetics associated with the molecular structure of the precursors at the substrate. Interestingly, the (204/220)-oriented films were always In-rich and were accompanied by a secondary phase. From the results of post-growth annealing, etching experiments, and Raman spectroscopic data, the secondary phase was identified as an In-rich compound. On the contrary, (112)-oriented films were always obtained with a minimal amount of the secondary phase, and had a maximum grain size of about 0.5 micron. Electrical and optical properties of all the films grown were characterized. They all showed p-type conduction with an electrical resistivity between 0.1 and 30 Omega-cm, and an optical band gap of approximately 1.46 eV +/- 0.02, as deposited. The material properties of deposited films revealed this methodology of using SSPs for fabricating chalcopyrite-based solar cells to be highly promising.

High Temperature Multilayer Environmental Barrier Coatings Deposited Via Plasma Spray-Physical Vapor Deposition

NASA Technical Reports Server (NTRS)

Harder, Bryan James; Zhu, Dongming; Schmitt, Michael P.; Wolfe, Douglas E.

2014-01-01

Si-based ceramic matrix composites (CMCs) require environmental barrier coatings (EBCs) in combustion environments to avoid rapid material loss. Candidate EBC materials have use temperatures only marginally above current technology, but the addition of a columnar oxide topcoat can substantially increase the durability. Plasma Spray-Physical Vapor Deposition (PS-PVD) allows application of these multilayer EBCs in a single process. The PS-PVD technique is a unique method that combines conventional thermal spray and vapor phase methods, allowing for tailoring of thin, dense layers or columnar microstructures by varying deposition conditions. Multilayer coatings were deposited on CMC specimens and assessed for durability under high heat flux and load. Coated samples with surface temperatures ranging from 2400-2700F and 10 ksi loads using the high heat flux laser rigs at NASA Glenn. Coating morphology was characterized in the as-sprayed condition and after thermomechanical loading using electron microscopy and the phase structure was tracked using X-ray diffraction.

Deposition of thermal and hot-wire chemical vapor deposition copper thin films on patterned substrates.

PubMed

Papadimitropoulos, G; Davazoglou, D

2011-09-01

In this work we study the hot-wire chemical vapor deposition (HWCVD) of copper films on blanket and patterned substrates at high filament temperatures. A vertical chemical vapor deposition reactor was used in which the chemical reactions were assisted by a tungsten filament heated at 650 degrees C. Hexafluoroacetylacetonate Cu(I) trimethylvinylsilane (CupraSelect) vapors were used, directly injected into the reactor with the aid of a liquid injection system using N2 as carrier gas. Copper thin films grown also by thermal and hot-wire CVD. The substrates used were oxidized silicon wafers on which trenches with dimensions of the order of 500 nm were formed and subsequently covered with LPCVD W. HWCVD copper thin films grown at filament temperature of 650 degrees C showed higher growth rates compared to the thermally ones. They also exhibited higher resistivities than thermal and HWCVD films grown at lower filament temperatures. Thermally grown Cu films have very uniform deposition leading to full coverage of the patterned substrates while the HWCVD films exhibited a tendency to vertical growth, thereby creating gaps and incomplete step coverage.

Numerical modeling tools for chemical vapor deposition

NASA Technical Reports Server (NTRS)

Jasinski, Thomas J.; Childs, Edward P.

1992-01-01

Development of general numerical simulation tools for chemical vapor deposition (CVD) was the objective of this study. Physical models of important CVD phenomena were developed and implemented into the commercial computational fluid dynamics software FLUENT. The resulting software can address general geometries as well as the most important phenomena occurring with CVD reactors: fluid flow patterns, temperature and chemical species distribution, gas phase and surface deposition. The physical models are documented which are available and examples are provided of CVD simulation capabilities.

Plasma Spray-Physical Vapor Deposition (PS-PVD) of Ceramics for Protective Coatings

NASA Technical Reports Server (NTRS)

Harder, Bryan J.; Zhu, Dongming

2011-01-01

In order to generate advanced multilayer thermal and environmental protection systems, a new deposition process is needed to bridge the gap between conventional plasma spray, which produces relatively thick coatings on the order of 125-250 microns, and conventional vapor phase processes such as electron beam physical vapor deposition (EB-PVD) which are limited by relatively slow deposition rates, high investment costs, and coating material vapor pressure requirements. The use of Plasma Spray - Physical Vapor Deposition (PS-PVD) processing fills this gap and allows thin (< 10 microns) single layers to be deposited and multilayer coatings of less than 100 microns to be generated with the flexibility to tailor microstructures by changing processing conditions. Coatings of yttria-stabilized zirconia (YSZ) were applied to NiCrAlY bond coated superalloy substrates using the PS-PVD coater at NASA Glenn Research Center. A design-of-experiments was used to examine the effects of process variables (Ar/He plasma gas ratio, the total plasma gas flow, and the torch current) on chamber pressure and torch power. Coating thickness, phase and microstructure were evaluated for each set of deposition conditions. Low chamber pressures and high power were shown to increase coating thickness and create columnar-like structures. Likewise, high chamber pressures and low power had lower growth rates, but resulted in flatter, more homogeneous layers

Deposition-temperature dependence of structural anisotropy in amorphous Tb-Fe films

NASA Astrophysics Data System (ADS)

Harris, V. G.; Elam, W. T.; Koon, N. C.; Hellman, F.

1994-02-01

The anisotropic local structure in a series of amorphous Tb26Fe74 films deposited at different deposition temperatures and having different magnetic anisotropy energies have been investigated using polarization-dependent extended x-ray-absorption fine-structure measurements. Samples deposited at temperatures >=300 K exhibit anisotropic pair correlations where like atomic pairs are favored in plane and unlike pairs are favored out of plane. Both the anisotropic pair correlations and the perpendicular magnetic anisotropy increase with increasing deposition temperature. In contrast, a sample deposited at 77 K was found to have isotropic pair correlations, low perpendicular magnetic anisotropy, and a large (~=1%) in-plane compression.

Understanding the Vapor-Liquid-Solid and Vapor-Solid-Solid Mechanisms of Si Nanowire Growth to Synthetically Encode Precise Nanoscale Morphology

NASA Astrophysics Data System (ADS)

Pinion, Christopher William

Precise patterning of semiconductor materials utilizing top-down lithographic techniques is integral to the advanced electronics we use on a daily basis. However, continuing development of these lithographic technologies often results in the trade-off of either high cost or low throughput, and three-dimensional (3D) patterning can be difficult to achieve. Bottom-up, chemical methods to control the 3D nanoscale morphology of semiconductor nanostructures have received significant attention as a complementary technique. Semiconductor nanowires, nanoscale filaments of semiconductor material 10-500 nm in diameter and 1-50 microns in length, are an especially promising platform because the wire composition can be modulated during growth and the high aspect ratio, one-dimensional structure enables integration in a range of devices. In this thesis, we first report a bottom-up method to break the conventional "wire" symmetry and synthetically encode a high-resolution array of arbitrary shapes along the nanowire growth axis. Rapid modulation of phosphorus doping combined with selective wet-chemical etching enables morphological features as small as 10 nm to be patterned over wires more than 50 ?m in length. Next, our focus shifts to more fundamental studies of the nanowire synthetic mechanisms. We presented comprehensive experimental measurements on the growth rate of Au catalyzed Si nanowires and developed a kinetic model of vapor-liquid-solid growth. Our analysis revealed an abrupt transition from a diameter-independent growth rate that is limited by incorporation to a diameter-dependent growth rate that is limited by crystallization. While investigating the vapor-liquid-solid mechanism, we noticed instances of unique catalyst behavior. Upon further study, we showed that it is possible to instantaneously and reversibly switch the phase of the catalyst between a liquid and superheated solid state under isothermal conditions above the eutectic temperature. The solid catalyst

Vapor-deposited porous films for energy conversion

DOEpatents

Jankowski, Alan F.; Hayes, Jeffrey P.; Morse, Jeffrey D.

2005-07-05

Metallic films are grown with a "spongelike" morphology in the as-deposited condition using planar magnetron sputtering. The morphology of the deposit is characterized by metallic continuity in three dimensions with continuous and open porosity on the submicron scale. The stabilization of the spongelike morphology is found over a limited range of the sputter deposition parameters, that is, of working gas pressure and substrate temperature. This spongelike morphology is an extension of the features as generally represented in the classic zone models of growth for physical vapor deposits. Nickel coatings were deposited with working gas pressures up 4 Pa and for substrate temperatures up to 1000 K. The morphology of the deposits is examined in plan and in cross section views with scanning electron microscopy (SEM). The parametric range of gas pressure and substrate temperature (relative to absolute melt point) under which the spongelike metal deposits are produced appear universal for other metals including gold, silver, and aluminum.

Phase-field model of vapor-liquid-solid nanowire growth

NASA Astrophysics Data System (ADS)

Wang, Nan; Upmanyu, Moneesh; Karma, Alain

2018-03-01

We present a multiphase-field model to describe quantitatively nanowire growth by the vapor-liquid-solid (VLS) process. The free-energy functional of this model depends on three nonconserved order parameters that distinguish the vapor, liquid, and solid phases and describe the energetic properties of various interfaces, including arbitrary forms of anisotropic γ plots for the solid-vapor and solid-liquid interfaces. The evolution equations for those order parameters describe basic kinetic processes including the rapid (quasi-instantaneous) equilibration of the liquid catalyst to a droplet shape with constant mean curvature, the slow incorporation of growth atoms at the droplet surface, and crystallization within the droplet. The standard constraint that the sum of the phase fields equals unity and the conservation of the number of catalyst atoms, which relates the catalyst volume to the concentration of growth atoms inside the droplet, are handled via separate Lagrange multipliers. An analysis of the model is presented that rigorously maps the phase-field equations to a desired set of sharp-interface equations for the evolution of the phase boundaries under the constraint of force balance at three-phase junctions (triple points) given by the Young-Herring relation that includes torque term related to the anisotropy of the solid-liquid and solid-vapor interface excess free energies. Numerical examples of growth in two dimensions are presented for the simplest case of vanishing crystalline anisotropy and the more realistic case of a solid-liquid γ plot with cusped minima corresponding to two sets of (10 ) and (11 ) facets. The simulations reproduce many of the salient features of nanowire growth observed experimentally, including growth normal to the substrate with tapering of the side walls, transitions between different growth orientations, and crawling growth along the substrate. They also reproduce different observed relationships between the nanowire growth

Extended vapor-liquid-solid growth of silicon carbide nanowires.

PubMed

Rajesh, John Anthuvan; Pandurangan, Arumugam

2014-04-01

We developed an alloy catalytic method to explain extended vapor-liquid-solid (VLS) growth of silicon carbide nanowires (SiC NWs) by a simple thermal evaporation of silicon and activated carbon mixture using lanthanum nickel (LaNi5) alloy as catalyst in a chemical vapor deposition process. The LaNi5 alloy binary phase diagram and the phase relationships in the La-Ni-Si ternary system were play a key role to determine the growth parameters in this VLS mechanism. Different reaction temperatures (1300, 1350 and 1400 degrees C) were applied to prove the established growth process by experimentally. Scanning electron microscopy and transmission electron microscopy studies show that the crystalline quality of the SiC NWs increases with the temperature at which they have been synthesized. La-Ni alloyed catalyst particles observed on the top of the SiC NWs confirms that the growth process follows this extended VLS mechanism. The X-ray diffraction and confocal Raman spectroscopy analyses demonstrate that the crystalline structure of the SiC NWs was zinc blende 3C-SiC. Optical property of the SiC NWs was investigated by photoluminescence technique at room temperature. Such a new alloy catalytic method may be extended to synthesis other one-dimensional nanostructures.

Enabling thermal processing of ritonavir-polyvinyl alcohol amorphous solid dispersions by KinetiSol® Dispersing.

PubMed

LaFountaine, Justin S; Jermain, Scott V; Prasad, Leena Kumari; Brough, Chris; Miller, Dave A; Lubda, Dieter; McGinity, James W; Williams, Robert O

2016-04-01

Polyvinyl alcohol has received little attention as a matrix polymer in amorphous solid dispersions (ASDs) due to its thermal and rheological limitations in extrusion processing and limited organic solubility in spray drying applications. Additionally, in extrusion processing, the high temperatures required to process often exclude thermally labile APIs. The purpose of this study was to evaluate the feasibility of processing polyvinyl alcohol amorphous solid dispersions utilizing the model compound ritonavir with KinetiSol® Dispersing (KSD) technology. The effects of KSD rotor speed and ejection temperature on the physicochemical properties of the processed material were evaluated. Powder X-ray diffraction and modulated differential scanning calorimetry were used to confirm amorphous conversion. Liquid chromatography-mass spectroscopy was used to characterize and identify degradation pathways of ritonavir during KSD processing and (13)C nuclear magnetic resonance spectroscopy was used to investigate polymer stability. An optimal range of processing conditions was found that resulted in amorphous product and minimal to no drug and polymer degradation. Drug release of the ASD produced from the optimal processing conditions was evaluated using a non-sink, pH-shift dissolution test. The ability to process amorphous solid dispersions with polyvinyl alcohol as a matrix polymer will enable further investigations of the polymer's performance in amorphous systems for poorly water-soluble compounds. Copyright © 2016 Elsevier B.V. All rights reserved.

Inhibiting surface crystallization of amorphous indomethacin by nanocoating.

PubMed

Wu, Tian; Sun, Ye; Li, Ning; de Villiers, Melgardt M; Yu, Lian

2007-04-24

An amorphous solid (glass) may crystallize faster at the surface than through the bulk, making surface crystallization a mechanism of failure for amorphous pharmaceuticals and other materials. An ultrathin coating of gold or polyelectrolytes inhibited the surface crystallization of amorphous indomethacin (IMC), an anti-inflammatory drug and model organic glass. The gold coating (10 nm) was deposited by sputtering, and the polyelectrolyte coating (3-20 nm) was deposited by an electrostatic layer-by-layer assembly of cationic poly(dimethyldiallyl ammonium chloride) (PDDA) and anionic sodium poly(styrenesulfonate) (PSS) in aqueous solution. The coating also inhibited the growth of existing crystals. The inhibition was strong even with one layer of PDDA. The polyelectrolyte coating still permitted fast dissolution of amorphous IMC and improved its wetting and flow. The finding supports the view that the surface crystallization of amorphous IMC is enabled by the mobility of a thin layer of surface molecules, and this mobility can be suppressed by a coating of only a few nanometers. This technique may be used to stabilize amorphous drugs prone to surface crystallization, with the aqueous coating process especially suitable for drugs of low aqueous solubility.

Chemical vapor deposition of sialon

DOEpatents

Landingham, Richard L.; Casey, Alton W.

1982-01-01

A laminated composite and a method for forming the composite by chemical vapor deposition. The composite includes a layer of sialon and a material to which the layer is bonded. The method includes the steps of exposing a surface of the material to an ammonia containing atmosphere; heating the surface to at least about 1200.degree. C.; and impinging a gas containing in a flowing atmosphere of air N.sub.2, SiCl.sub.4, and AlCl.sub.3 on the surface.

Chemical vapor deposition of sialon

DOEpatents

Landingham, R.L.; Casey, A.W.

A laminated composite and a method for forming the composite by chemical vapor deposition are described. The composite includes a layer of sialon and a material to which the layer is bonded. The method includes the steps of exposing a surface of the material to an ammonia containing atmosphere; heating the surface to at least about 1200/sup 0/C; and impinging a gas containing N/sub 2/, SiCl/sub 4/, and AlCl/sub 3/ on the surface.

The Chemical Vapor Deposition of Thin Metal Oxide Films

NASA Astrophysics Data System (ADS)

Laurie, Angus Buchanan

1990-01-01

Chemical vapor deposition (CVD) is an important method of preparing thin films of materials. Copper (II) oxide is an important p-type semiconductor and a major component of high T_{rm c} superconducting oxides. By using a volatile copper (II) chelate precursor, copper (II) bishexafluoroacetylacetonate, it has been possible to prepare thin films of copper (II) oxide by low temperature normal pressure metalorganic chemical vapor deposition. In the metalorganic CVD (MOCVD) production of oxide thin films, oxygen gas saturated with water vapor has been used mainly to reduce residual carbon and fluorine content. This research has investigated the influence of water-saturated oxygen on the morphology of thin films of CuO produced by low temperature chemical vapor deposition onto quartz, magnesium oxide and cubic zirconia substrates. ZnO is a useful n-type semiconductor material and is commonly prepared by the MOCVD method using organometallic precursors such as dimethyl or diethylzinc. These compounds are difficult to handle under atmospheric conditions. In this research, thin polycrystalline films of zinc oxide were grown on a variety of substrates by normal pressure CVD using a zinc chelate complex with zinc(II) bishexafluoroacetylacetonate dihydrate (Zn(hfa)_2.2H _2O) as the zinc source. Zn(hfa) _2.2H_2O is not moisture - or air-sensitive and is thus more easily handled. By operating under reduced-pressure conditions (20-500 torr) it is possible to substantially reduce deposition times and improve film quality. This research has investigated the reduced-pressure CVD of thin films of CuO and ZnO. Sub-micron films of tin(IV) oxide (SnO _2) have been grown by normal pressure CVD on quartz substrates by using tetraphenyltin (TPT) as the source of tin. All CVD films were characterized by X-ray powder diffraction (XRPD), scanning electron microscopy (SEM) and electron probe microanalysis (EPMA).

Thermodynamic study of (anthracene + benzo[a]pyrene) solid mixtures

PubMed Central

Rice, James W.; Suuberg, Eric M.

2010-01-01

To characterize better the thermodynamic behavior of a binary polycyclic aromatic hydrocarbon mixture, thermochemical and vapor pressure experiments were used to examine the phase behavior of the {anthracene (1) + benzo[a]pyrene (2)} system. A solid-liquid phase diagram was mapped for the mixture. A eutectic point occurs at x1 = 0.26. The eutectic mixture is an amorphous solid that lacks organized crystal structure and melts between T = (414 and 420) K. For mixtures that contain 0.10 < x1 < 0.90, the enthalpy of fusion is dominated by that of the eutectic. Solid-vapor equilibrium studies show that mixtures of anthracene and benzo[a]pyrene at x1 < 0.10 sublime at the vapor pressure of pure benzo[a]pyrene. These results suggest that the solid-vapor equilibrium of benzo[a]pyrene is not significantly influenced by moderate levels of anthracene in the crystal structure. PMID:20814451

Interfacial interaction track of amorphous solid dispersions established by water-soluble polymer and indometacin.

PubMed

Li, Jing; Fan, Na; Wang, Xin; Li, Chang; Sun, Mengchi; Wang, Jian; Fu, Qiang; He, Zhonggui

2017-08-30

The present work studied interfacial interactions of amorphous solid dispersions matrix of indometacin (IMC) that established using PVP K30 (PVP) and PEG 6000 (PEG) by focusing on their interaction forces and wetting process. Infrared spectroscopy (IR), raman spectroscopy, X-ray photoelectron spectra and contact angle instrument were used throughout the study. Hydrogen bond energy formed between PEG and IMC were stronger than that of PVP and IMC evidenced by molecular modeling measurement. The blue shift of raman spectroscopy confirmed that hydrogen bonding forces were formed between IMC and two polymers. The contact angle study can be used as an easy method to determine the dissolution mechanism of amorphous solid dispersions through fitting the profile of contact angle of water on a series of tablets. It is believed that the track of interfacial interactions will certainly become powerful tools to for designing and evaluating amorphous solid dispersions. Copyright © 2017 Elsevier B.V. All rights reserved.

Thermal Processing of PVP- and HPMC-Based Amorphous Solid Dispersions.

PubMed

LaFountaine, Justin S; Prasad, Leena Kumari; Brough, Chris; Miller, Dave A; McGinity, James W; Williams, Robert O

2016-02-01

Thermal processing technologies continue to gain interest in pharmaceutical manufacturing. However, the types and grades of polymers that can be utilized in common thermal processing technologies, such as hot-melt extrusion (HME), are often limited by thermal or rheological factors. The objectives of the present study were to compare and contrast two thermal processing methods, HME and KinetiSol® Dispersing (KSD), and investigate the influence of polymer type, polymer molecular weight, and drug loading on the ability to produce amorphous solid dispersions (ASDs) containing the model compound griseofulvin (GRIS). Dispersions were analyzed by a variety of imaging, solid-state, thermal, and solution-state techniques. Dispersions were prepared by both HME and KSD using polyvinylpyrrolidone (PVP) K17 or hydroxypropyl methylcellulose (HPMC) E5. Dispersions were only prepared by KSD using higher molecular weight grades of HPMC and PVP, as these could not be extruded under the conditions selected. Powder X-ray diffraction (PXRD) analysis showed that dispersions prepared by HME were amorphous at 10% and 20% drug load; however, it showed significant crystallinity at 40% drug load. PXRD analysis of KSD samples showed all formulations and drug loads to be amorphous with the exception of trace crystallinity seen in PVP K17 and PVP K30 samples at 40% drug load. These results were further supported by other analytical techniques. KSD produced amorphous dispersions at higher drug loads than could be prepared by HME, as well as with higher molecular weight polymers that were not processable by HME, due to its higher rate of shear and torque output.

Vaporization of a mixed precursors in chemical vapor deposition for YBCO films

NASA Technical Reports Server (NTRS)

Zhou, Gang; Meng, Guangyao; Schneider, Roger L.; Sarma, Bimal K.; Levy, Moises

1995-01-01

Single phase YBa2Cu3O7-delta thin films with T(c) values around 90 K are readily obtained by using a single source chemical vapor deposition technique with a normal precursor mass transport. The quality of the films is controlled by adjusting the carrier gas flow rate and the precursor feed rate.

Surface Temperature Dependence of Hydrogen Ortho-Para Conversion on Amorphous Solid Water.

PubMed

Ueta, Hirokazu; Watanabe, Naoki; Hama, Tetsuya; Kouchi, Akira

2016-06-24

The surface temperature dependence of the ortho-to-para conversion of H_{2} on amorphous solid water is first reported. A combination of photostimulated desorption and resonance-enhanced multiphoton ionization techniques allowed us to sensitively probe the conversion on the surface of amorphous solid water at temperatures of 9.2-16 K. Within a narrow temperature window of 8 K, the conversion time steeply varied from ∼4.1×10^{3} to ∼6.4×10^{2}  s. The observed temperature dependence is discussed in the context of previously suggested models and the energy dissipation process. The two-phonon process most likely dominates the conversion rate at low temperatures.

Vapor deposition in basaltic stalactites, Kilauea, Hawaii

NASA Astrophysics Data System (ADS)

Baird, A. K.; Mohrig, D. C.; Welday, E. E.

Basaltic stalacties suspended from the ceiling of a large lava tube at Kilauea, Hawaii, have totally enclosed vesicles whose walls are covered with euhedral FeTi oxide and silicate crystals. The walls of the vesicles and the exterior surfaces of stalactites are Fe and Ti enriched and Si depleted compared to common basalt. Minerals in vesicles have surface ornamentations on crystal faces which include alkali-enriched, aluminosilicate glass(?) hemispheres. No sulfide-, chloride-, fluoride-, phosphate- or carbonate-bearing minerals are present. Minerals in the stalactites must have formed by deposition from an iron oxide-rich vapor phase produced by the partial melting and vaporization of wall rocks in the tube.

Neutron Scattering Analysis of Water's Glass Transition and Micropore Collapse in Amorphous Solid Water.

PubMed

Hill, Catherine R; Mitterdorfer, Christian; Youngs, Tristan G A; Bowron, Daniel T; Fraser, Helen J; Loerting, Thomas

2016-05-27

The question of the nature of water's glass transition has continued to be disputed over many years. Here we use slow heating scans (0.4  K min^{-1}) of compact amorphous solid water deposited at 77 K and an analysis of the accompanying changes in the small-angle neutron scattering signal, to study mesoscale changes in the ice network topology. From the data we infer the onset of rotational diffusion at 115 K, a sudden switchover from nondiffusive motion and enthalpy relaxation of the network at <121  K to diffusive motion across sample grains and sudden pore collapse at >121  K, in excellent agreement with the glass transition onset deduced from heat capacity and dielectric measurements. This indicates that water's glass transition is linked with long-range transport of water molecules on the time scale of minutes and, thus, clarifies its nature. Furthermore, the slow heating rates combined with the high crystallization resistance of the amorphous sample allow us to identify the glass transition end point at 136 K, which is well separated from the crystallization onset at 144 K-in contrast to all earlier experiments in the field.

Influence of isotopic disorder on solid state amorphization and polyamorphism in solid H2O -D2O solutions

NASA Astrophysics Data System (ADS)

Gromnitskaya, E. L.; Danilov, I. V.; Lyapin, A. G.; Brazhkin, V. V.

2015-10-01

We present a low-temperature and high-pressure ultrasonic study of elastic properties of isotopic H2O-D2O solid solutions, comparing their properties with those of the isotopically pure H2O and D2O ices. Measurements were carried out for solid state amorphization (SSA) from 1h to high-density amorphous (HDA) ice upon compression up to 1.8 GPa at 77 K and for the temperature-induced (77 -190 K ) u-HDA (unrelaxed HDA) → e-HDA (expanded HDA) → low-density amorphous (LDA )→1 c cascade of ice transformations near room pressure. There are many similarities in the elasticity behaviour of H2O ,D2O , and H2O-D2O solid solutions, including the softening of the shear elastic modulus as a precursor of SSA and the HDA →LDA transition. We have found significant isotopic effects during H/D substitution, including elastic softening of H2O -D2O solid solutions with respect to the isotopically pure ices in the case of the bulk moduli of ices 1c and 1h and for both bulk and shear elastic moduli of HDA ice at high pressures (>1 GPa ) . This softening is related to the configurational isotopic disorder in the solid solutions. At low pressures, the isotope concentration dependence of the elastic moduli of u-HDA ice changes remarkably and becomes monotonic with pronounced change of the bulk modulus (≈20 %) .

Liquid-vapor equilibrium and interfacial properties of square wells in two dimensions

NASA Astrophysics Data System (ADS)

Armas-Pérez, Julio C.; Quintana-H, Jacqueline; Chapela, Gustavo A.

2013-01-01

Liquid-vapor coexistence and interfacial properties of square wells in two dimensions are calculated. Orthobaric densities, vapor pressures, surface tensions, and interfacial thicknesses are reported. Results are presented for a series of potential widths λ* = 1.4, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, and 5, where λ* is given in units of the hard core diameter σ. Critical and triple points are explored. No critical point was found for λ* < 1.4. Corresponding states principle analysis is performed for the whole series. For λ* = 1.4 and 1.5 evidence is presented that at an intermediate temperature between the critical and the triple point temperatures the liquid branch becomes an amorphous solid. This point is recognized in Armas-Pérez et al. [unpublished] as a hexatic phase transition. It is located at reduced temperatures T* = 0.47 and 0.35 for λ* = 1.4 and 1.5, respectively. Properties such as the surface tension, vapor pressure, and interfacial thickness do not present any discontinuity at these points. This amorphous solid branch does not follow the corresponding state principle, which is only applied to liquids and gases.

Flexible all solid-state supercapacitors based on chemical vapor deposition derived graphene fibers.

PubMed

Li, Xinming; Zhao, Tianshuo; Chen, Qiao; Li, Peixu; Wang, Kunlin; Zhong, Minlin; Wei, Jinquan; Wu, Dehai; Wei, Bingqing; Zhu, Hongwei

2013-11-07

Flexible all-solid-state supercapacitors based on graphene fibers are demonstrated in this study. Surface-deposited oxide nanoparticles are used as pseudo-capacitor electrodes to achieve high capacitance. This supercapacitor electrode has an areal capacitance of 42 mF cm(-2), which is comparable to the capacitance for fiber-based supercapacitors reported to date. During the bending and cycling of the fiber-based supercapacitor, the stability could be maintained without sacrificing the electrochemical performance, which provides a novel and simple way to develop flexible, lightweight and efficient graphene-based devices.

Improved Vemurafenib Dissolution and Pharmacokinetics as an Amorphous Solid Dispersion Produced by KinetiSol® Processing.

PubMed

Ellenberger, Daniel J; Miller, Dave A; Kucera, Sandra U; Williams, Robert O

2018-03-14

Vemurafenib is a poorly soluble, low permeability drug that has a demonstrated need for a solubility-enhanced formulation. However, conventional approaches for amorphous solid dispersion production are challenging due to the physiochemical properties of the compound. A suitable and novel method for creating an amorphous solid dispersion, known as solvent-controlled coprecipitation, was developed to make a material known as microprecipitated bulk powder (MBP). However, this approach has limitations in its processing and formulation space. In this study, it was hypothesized that vemurafenib can be processed by KinetiSol into the same amorphous formulation as MBP. The KinetiSol process utilizes high shear to rapidly process amorphous solid dispersions containing vemurafenib. Analysis of the material demonstrated that KinetiSol produced amorphous, single-phase material with acceptable chemical purity and stability. Values obtained were congruent to analysis conducted on the comparator material. However, the materials differed in particle morphology as the KinetiSol material was dense, smooth, and uniform while the MBP comparator was porous in structure and exhibited high surface area. The particles produced by KinetiSol had improved in-vitro dissolution and pharmacokinetic performance for vemurafenib compared to MBP due to slower drug nucleation and recrystallization which resulted in superior supersaturation maintenance during drug release. In the in-vivo rat pharmacokinetic study, both amorphous solid dispersions produced by KinetiSol exhibited mean AUC values at least two-fold that of MBP when dosed as a suspension. It was concluded that the KinetiSol process produced superior dosage forms containing vemurafenib with the potential for substantial reduction in patient pill burden.

Physical vapor deposition as a route to glasses with liquid crystalline order

NASA Astrophysics Data System (ADS)

Gomez, Jaritza

Physical vapor deposition (PVD) is an effective route to prepare glasses with a unique combination of properties. Substrate temperatures near the glass transition (Tg) and slow deposition rates can access enhanced mobility at the surface of the glass allowing molecules at the surface additional time to sample different molecular configurations. The temperature of the substrate can be used to control molecular mobility during deposition and properties in the resulting glasses such as higher density, kinetic stability and preferential molecular orientation. PVD was used to prepare glasses of itraconazole, a smectic A liquid crystal. We characterized molecular orientation using infrared and ellipsometry. Molecular orientation can be controlled by choice of Tsubstrate in a range of temperatures near Tg. Glasses deposited at Tsubstrate = Tg show nearly vertical molecular orientation relative to the substrate; at lower Tsubstrate, molecules are nearly parallel to the substrate. The molecular orientation depends on the temperature of the substrate during preparation and not on the molecular orientation of the underlying layer. This allows preparing samples of layers with differing orientations. We find these glasses are homogeneous solids without evidence of domain boundaries and are molecularly flat. We interpret the combination of properties obtained for vapor-deposited glasses of itraconazole to result from a process where molecular orientation is determined by the structure and dynamics at the free surface of the glass during deposition. We report the thermal and structural properties of glasses prepared using PVD of a rod-like molecule, posaconazole, which does not show equilibrium liquid crystal phases. These glasses show substantial molecular orientation that can be controlled by choice of Tsubstrate during deposition. Ellipsometry and IR indicate that glasses prepared at Tg - 3 K are highly ordered. At these Tsubstrate, molecules show preferential vertical

Atomic transport during solid-phase epitaxial recrystallization of amorphous germanium

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

Radek, M.; Bracht, H., E-mail: bracht@uni-muenster.de; Johnson, B. C.

2015-08-24

The atomic mixing of matrix atoms during solid-phase epitaxy (SPE) is studied by means of isotopically enriched germanium (Ge) multilayer structures that were amorphized by Ge ion implantation up to a depth of 1.5 μm. Recrystallization of the amorphous structure is performed at temperatures between 350 °C and 450 °C. Secondary-ion-mass-spectrometry is used to determine the concentration-depth profiles of the Ge isotope before and after SPE. An upper limit of 0.5 nm is deduced for the displacement length of the Ge matrix atoms by the SPE process. This small displacement length is consistent with theoretical models and atomistic simulations of SPE, indicating that themore » SPE mechanism consists of bond-switching with nearest-neighbours across the amorphous-crystalline (a/c) interface.« less

Control of composition and crystallinity in hydroxyapatite films deposited by electron cyclotron resonance plasma sputtering

NASA Astrophysics Data System (ADS)

Akazawa, Housei; Ueno, Yuko

2014-01-01

Hydroxyapatite (HAp) films were deposited by electron cyclotron resonance plasma sputtering under a simultaneous flow of H2O vapor gas. Crystallization during sputter-deposition at elevated temperatures and solid-phase crystallization of amorphous films were compared in terms of film properties. When HAp films were deposited with Ar sputtering gas at temperatures above 460 °C, CaO byproducts precipitated with HAp crystallites. Using Xe instead of Ar resolved the compositional problem, yielding a single HAp phase. Preferentially c-axis-oriented HAp films were obtained at substrate temperatures between 460 and 500 °C and H2O pressures higher than 1×10-2 Pa. The absorption signal of the asymmetric stretching mode of the PO43- unit (ν3) in the Fourier-transform infrared absorption (FT-IR) spectra was the narrowest for films as-crystallized during deposition with Xe, but widest for solid-phase crystallized films. While the symmetric stretching mode of PO43- (ν1) is theoretically IR-inactive, this signal emerged in the FT-IR spectra of solid-phase crystallized films, but was absent for as-crystallized films, indicating superior crystallinity for the latter. The Raman scattering signal corresponding to ν1 PO43- sensitively reflected this crystallinity. The surface hardness of as-crystallized films evaluated by a pencil hardness test was higher than that of solid-phase crystallized films.

Barrier coated drug layered particles for enhanced performance of amorphous solid dispersion dosage form.

PubMed

Puri, Vibha; Dantuluri, Ajay K; Bansal, Arvind K

2012-01-01

Amorphous solid dispersions (ASDs) may entail tailor-made dosage form design to exploit their solubility advantage. Surface phenomena dominated the performance of amorphous celecoxib solid dispersion (ACSD) comprising of amorphous celecoxib (A-CLB), polyvinylpyrrolidone, and meglumine (7:2:1, w/w). ACSD cohesive interfacial interactions hindered its capsule dosage form dissolution (Puri V, Dhantuluri AK, Bansal AK 2011. J Pharm Sci 100:2460-2468). Furthermore, ACSD underwent significant devitrification under environmental stress. In the present study, enthalpy relaxation studies revealed its free surface to contribute to molecular mobility. Based on all these observations, barrier coated amorphous CLB solid dispersion layered particles (ADLP) were developed by Wurster process, using microcrystalline cellulose as substrate and polyvinyl alcohol (PVA), inulin, and polyvinyl acetate phthalate (PVAP) as coating excipients. Capsule formulations of barrier coated-ADLP could achieve rapid dispersibility and high drug release. Evaluation under varying temperature and RH conditions suggested the crystallization inhibitory efficiency in order of inulin < PVA ≈ PVAP; however, under only temperature treatment, crystallization inhibition increased with increase in T(g) of the coating material. Simulated studies using DSC evidenced drug-polymer mixing at the interface as a potential mechanism for surface stabilization. In conclusion, surface modification yielded a fast dispersing robust high drug load ASD based dosage form. Copyright © 2011 Wiley-Liss, Inc.

Chemical vapor deposition of group IIIB metals

DOEpatents

Erbil, Ahmet

1989-01-01

Coatings of Group IIIB metals and compounds thereof are formed by chemical vapor deposition, in which a heat decomposable organometallic compound of the formula (I) ##STR1## where M is a Group IIIB metal, such as lanthanum or yttrium and R is a lower alkyl or alkenyl radical containing from 2 to about 6 carbon atoms, with a heated substrate which is above the decomposition temperature of the organometallic compound. The pure metal is obtained when the compound of the formula I is the sole heat decomposable compound present and deposition is carried out under nonoxidizing conditions. Intermetallic compounds such as lanthanum telluride can be deposited from a lanthanum compound of formula I and a heat decomposable tellurium compound under nonoxidizing conditions.

Chemical vapor deposition of group IIIB metals

DOEpatents

Erbil, A.

1989-11-21

Coatings of Group IIIB metals and compounds thereof are formed by chemical vapor deposition, in which a heat decomposable organometallic compound of the formula given in the patent where M is a Group IIIB metal, such as lanthanum or yttrium and R is a lower alkyl or alkenyl radical containing from 2 to about 6 carbon atoms, with a heated substrate which is above the decomposition temperature of the organometallic compound. The pure metal is obtained when the compound of the formula 1 is the sole heat decomposable compound present and deposition is carried out under nonoxidizing conditions. Intermetallic compounds such as lanthanum telluride can be deposited from a lanthanum compound of formula 1 and a heat decomposable tellurium compound under nonoxidizing conditions.

Preparation of membranes using solvent-less vapor deposition followed by in-situ polymerization

DOEpatents

O'Brien, Kevin C [San Ramon, CA; Letts, Stephan A [San Ramon, CA; Spadaccini, Christopher M [Oakland, CA; Morse, Jeffrey C [Pleasant Hill, CA; Buckley, Steven R [Modesto, CA; Fischer, Larry E [Los Gatos, CA; Wilson, Keith B [San Ramon, CA

2012-01-24

A system of fabricating a composite membrane from a membrane substrate using solvent-less vapor deposition followed by in-situ polymerization. A first monomer and a second monomer are directed into a mixing chamber in a deposition chamber. The first monomer and the second monomer are mixed in the mixing chamber providing a mixed first monomer and second monomer. The mixed first monomer and second monomer are solvent-less vapor deposited onto the membrane substrate in the deposition chamber. The membrane substrate and the mixed first monomer and second monomer are heated to produce in-situ polymerization and provide the composite membrane.

Preparation of membranes using solvent-less vapor deposition followed by in-situ polymerization

DOEpatents

O'Brien, Kevin C [San Ramon, CA; Letts, Stephan A [San Ramon, CA; Spadaccini, Christopher M [Oakland, CA; Morse, Jeffrey C [Pleasant Hill, CA; Buckley, Steven R [Modesto, CA; Fischer, Larry E [Los Gatos, CA; Wilson, Keith B [San Ramon, CA

2010-07-13

A system of fabricating a composite membrane from a membrane substrate using solvent-less vapor deposition followed by in-situ polymerization. A first monomer and a second monomer are directed into a mixing chamber in a deposition chamber. The first monomer and the second monomer are mixed in the mixing chamber providing a mixed first monomer and second monomer. The mixed first monomer and second monomer are solvent-less vapor deposited onto the membrane substrate in the deposition chamber. The membrane substrate and the mixed first monomer and second monomer are heated to produce in-situ polymerization and provide the composite membrane.

Thermodynamics of water-solid interactions in crystalline and amorphous pharmaceutical materials.

PubMed

Sacchetti, Mark

2014-09-01

Pharmaceutical materials, crystalline and amorphous, sorb water from the atmosphere, which affects critical factors in the development of drugs, such as the selection of drug substance crystal form, compatibility with excipients, dosage form selection, packaging, and product shelf-life. It is common practice to quantify the amount of water that a material sorbs at a given relative humidity (RH), but the results alone provide minimal to no physicochemical insight into water-solid interactions, without which pharmaceutical scientists cannot develop an understanding of their materials, so as to anticipate and circumvent potential problems. This research was conducted to advance the science of pharmaceutical materials by examining the thermodynamics of solids with sorbed water. The compounds studied include nonhygroscopic drugs, a channel hydrate drug, a stoichiometric hydrate excipient, and an amorphous excipient. The water sorption isotherms were measured over a range of temperature to extract the partial molar enthalpy and entropy of sorbed water as well as the same quantities for some of the solids. It was found that water-solid interactions spanned a range of energy and entropy as a function of RH, which was unique to the solid, and which could be valuable in identifying batch-to-batch differences and effects of processing in material performance. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association.

Process for the preparation of fiber-reinforced ceramic composites by chemical vapor deposition

DOEpatents

Lackey, Jr., Walter J.; Caputo, Anthony J.

1986-01-01

A chemical vapor deposition (CVD) process for preparing fiber-reinforced ceramic composites. A specially designed apparatus provides a steep thermal gradient across the thickness of a fibrous preform. A flow of gaseous ceramic matrix material is directed into the fibrous preform at the cold surface. The deposition of the matrix occurs progressively from the hot surface of the fibrous preform toward the cold surface. Such deposition prevents the surface of the fibrous preform from becoming plugged. As a result thereof, the flow of reactant matrix gases into the uninfiltrated (undeposited) portion of the fibrous preform occurs throughout the deposition process. The progressive and continuous deposition of ceramic matrix within the fibrous preform provides for a significant reduction in process time over known chemical vapor deposition processes.

Imparting passivity to vapor deposited magnesium alloys

NASA Astrophysics Data System (ADS)

Wolfe, Ryan C.

Magnesium has the lowest density of all structural metals. Utilization of low density materials is advantageous from a design standpoint, because lower weight translates into improved performance of engineered products (i.e., notebook computers are more portable, vehicles achieve better gas mileage, and aircraft can carry more payload). Despite their low density and high strength to weight ratio, however, the widespread implementation of magnesium alloys is currently hindered by their relatively poor corrosion resistance. The objective of this research dissertation is to develop a scientific basis for the creation of a corrosion resistant magnesium alloy. The corrosion resistance of magnesium alloys is affected by several interrelated factors. Among these are alloying, microstructure, impurities, galvanic corrosion effects, and service conditions, among others. Alloying and modification of the microstructure are primary approaches to controlling corrosion. Furthermore, nonequilibrium alloying of magnesium via physical vapor deposition allows for the formation of single-phase magnesium alloys with supersaturated concentrations of passivity-enhancing elements. The microstructure and surface morphology is also modifiable during physical vapor deposition through the variation of evaporation power, pressure, temperature, ion bombardment, and the source-to-substrate distance. Aluminum, titanium, yttrium, and zirconium were initially chosen as candidates likely to impart passivity on vapor deposited magnesium alloys. Prior to this research, alloys of this type have never before been produced, much less studied. All of these metals were observed to afford some degree of corrosion resistance to magnesium. Due to the especially promising results from nonequilibrium alloying of magnesium with yttrium and titanium, the ternary magnesium-yttrium-titanium system was investigated in depth. While all of the alloys are lustrous, surface morphology is observed under the scanning

Biomimetic Dissolution: A Tool to Predict Amorphous Solid Dispersion Performance.

PubMed

Puppolo, Michael M; Hughey, Justin R; Dillon, Traciann; Storey, David; Jansen-Varnum, Susan

2017-11-01

The presented study describes the development of a membrane permeation non-sink dissolution method that can provide analysis of complete drug speciation and emulate the in vivo performance of poorly water-soluble Biopharmaceutical Classification System class II compounds. The designed membrane permeation methodology permits evaluation of free/dissolved/unbound drug from amorphous solid dispersion formulations with the use of a two-cell apparatus, biorelevant dissolution media, and a biomimetic polymer membrane. It offers insight into oral drug dissolution, permeation, and absorption. Amorphous solid dispersions of felodipine were prepared by hot melt extrusion and spray drying techniques and evaluated for in vitro performance. Prior to ranking performance of extruded and spray-dried felodipine solid dispersions, optimization of the dissolution methodology was performed for parameters such as agitation rate, membrane type, and membrane pore size. The particle size and zeta potential were analyzed during dissolution experiments to understand drug/polymer speciation and supersaturation sustainment of felodipine solid dispersions. Bland-Altman analysis was performed to measure the agreement or equivalence between dissolution profiles acquired using polymer membranes and porcine intestines and to establish the biomimetic nature of the treated polymer membranes. The utility of the membrane permeation dissolution methodology is seen during the evaluation of felodipine solid dispersions produced by spray drying and hot melt extrusion. The membrane permeation dissolution methodology can suggest formulation performance and be employed as a screening tool for selection of candidates to move forward to pharmacokinetic studies. Furthermore, the presented model is a cost-effective technique.

Combinatorial Characterization of TiO2 Chemical Vapor Deposition Utilizing Titanium Isopropoxide.

PubMed

Reinke, Michael; Ponomarev, Evgeniy; Kuzminykh, Yury; Hoffmann, Patrik

2015-07-13

The combinatorial characterization of the growth kinetics in chemical vapor deposition processes is challenging because precise information about the local precursor flow is usually difficult to access. In consequence, combinatorial chemical vapor deposition techniques are utilized more to study functional properties of thin films as a function of chemical composition, growth rate or crystallinity than to study the growth process itself. We present an experimental procedure which allows the combinatorial study of precursor surface kinetics during the film growth using high vacuum chemical vapor deposition. As consequence of the high vacuum environment, the precursor transport takes place in the molecular flow regime, which allows predicting and modifying precursor impinging rates on the substrate with comparatively little experimental effort. In this contribution, we study the surface kinetics of titanium dioxide formation using titanium tetraisopropoxide as precursor molecule over a large parameter range. We discuss precursor flux and temperature dependent morphology, crystallinity, growth rates, and precursor deposition efficiency. We conclude that the surface reaction of the adsorbed precursor molecules comprises a higher order reaction component with respect to precursor surface coverage.

Modifying hydrogen-bonded structures by physical vapor deposition: 4-methyl-3-heptanol

NASA Astrophysics Data System (ADS)

Young-Gonzales, A. R.; Guiseppi-Elie, A.; Ediger, M. D.; Richert, R.

2017-11-01

We prepared films of 4-methyl-3-heptanol by vapor depositing onto substrates held at temperatures between Tdep = 0.6Tg and Tg, where Tg is the glass transition temperature. Using deposition rates between 0.9 and 6.0 nm/s, we prepared films about 5 μm thick and measured the dielectric properties via an interdigitated electrode cell onto which films were deposited. Samples prepared at Tdep = Tg display the dielectric behavior of the ordinary supercooled liquid. Films deposited at lower deposition temperatures show a high dielectric loss upon heating toward Tg, which decreases by a factor of about 12 by annealing at Tg = 162 K. This change is consistent with either a drop of the Kirkwood correlation factor, gk, by a factor of about 10, or an increase in the dielectric relaxation times, both being indicative of changes toward ring-like hydrogen-bonded structure characteristic of the ordinary liquid. We rationalize the high dielectric relaxation amplitude in the vapor deposited glass by suggesting that depositions at low temperature provide insufficient time for molecules to form ring-like supramolecular structures for which dipole moments cancel. Surprisingly, above Tg of the ordinary liquid, these vapor deposited films fail to completely recover the dielectric properties of the liquid obtained by supercooling. Instead, the dielectric relaxation remains slower and its amplitude much higher than that of the equilibrium liquid state, indicative of a structure that differs from the equilibrium liquid up to at least Tg + 40 K.

Reaction mechanism of electrochemical-vapor deposition of yttria-stabilized zirconia film

NASA Astrophysics Data System (ADS)

Sasaki, Hirokazu; Yakawa, Chiori; Otoshi, Shoji; Suzuki, Minoru; Ippommatsu, Masamichi

1993-10-01

The reaction mechanism for electrochemical-vapor deposition of yttria-stabilized zirconia was studied. Yttria-stabilized zirconia films were deposited on porous La(Sr)MnOx using the electrochemical-vapor-deposition process. The distribution of yttria concentration through the film was investigated by means of secondary-ion-mass spectroscopy and x-ray microanalysis and found to be nearly constant. The deposition rate was approximately proportional to the minus two-thirds power of the film thickness, the one-third power of the partial pressure of ZrCl4/YCl3 mixed gas, and the two-thirds power of the product of the reaction temperature and the electronic conductivity of yttria-stabilized zirconia film. These experimental results were explained by a model for electron transport through the YSZ film and reaction between the surface oxygen and the metal chloride on the chloride side of the film, both of which affect the deposition rate. If the film thickness is very small, the deposition rate is thought to be controlled by the surface reaction step. On the other hand, if large, the electron transport step is rate controlling.

Low temperature junction growth using hot-wire chemical vapor deposition

DOEpatents

Wang, Qi; Page, Matthew; Iwaniczko, Eugene; Wang, Tihu; Yan, Yanfa

2014-02-04

A system and a process for forming a semi-conductor device, and solar cells (10) formed thereby. The process includes preparing a substrate (12) for deposition of a junction layer (14); forming the junction layer (14) on the substrate (12) using hot wire chemical vapor deposition; and, finishing the semi-conductor device.

Chemical Vapor Deposition of Multispectral Domes

DTIC Science & Technology

1975-04-01

optical testing, was also cut out as indicated in Figure 10. The image spoiling measureinents were performed at the Air Force Avionics Laboratory on...AD-A014 362 CHEMICAL VAPOR DEPOSITION OF MULTISPECTRAL DOMES B. A. diBenedetto, et al Raytheon Company Prepared for: Air Force Materials Laboratory...Approved for public release; distribution unlimited. ) F) .• •~~EP 7 ’+ i.i AIR FORCE MATERIALS LABORATORY AIR FORCE SYSTEMS COMMAND WRIGHT-PATrERSON AIR

Low temperature photochemical vapor deposition of alloy and mixed metal oxide films

DOEpatents

Liu, David K.

1992-01-01

Method and apparatus for formation of an alloy thin film, or a mixed metal oxide thin film, on a substrate at relatively low temperatures. Precursor vapor(s) containing the desired thin film constituents is positioned adjacent to the substrate and irradiated by light having wavelengths in a selected wavelength range, to dissociate the gas(es) and provide atoms or molecules containing only the desired constituents. These gases then deposit at relatively low temperatures as a thin film on the substrate. The precursor vapor(s) is formed by vaporization of one or more precursor materials, where the vaporization temperature(s) is selected to control the ratio of concentration of metals present in the precursor vapor(s) and/or the total precursor vapor pressure.

Low temperature photochemical vapor deposition of alloy and mixed metal oxide films

DOEpatents

Liu, D.K.

1992-12-15

Method and apparatus are described for formation of an alloy thin film, or a mixed metal oxide thin film, on a substrate at relatively low temperatures. Precursor vapor(s) containing the desired thin film constituents is positioned adjacent to the substrate and irradiated by light having wavelengths in a selected wavelength range, to dissociate the gas(es) and provide atoms or molecules containing only the desired constituents. These gases then deposit at relatively low temperatures as a thin film on the substrate. The precursor vapor(s) is formed by vaporization of one or more precursor materials, where the vaporization temperature(s) is selected to control the ratio of concentration of metals present in the precursor vapor(s) and/or the total precursor vapor pressure. 7 figs.

Structural and growth aspects of electron beam physical vapor deposited NiO-CeO{sub 2} nanocomposite films

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

Kuanr, Sushil Kumar; K, Suresh Babu, E-mail: sureshbabu.nst@pondiuni.edu.in

2016-03-15

Deposition of composite materials as thin film by electron beam physical vapor deposition technique (EB-PVD) still remains as a challenge. Here, the authors report the deposition of NiO-CeO{sub 2} (30/70 wt. %) composites on quartz substrate by EB-PVD. Two NiO-CeO{sub 2} nanocomposite targets—one as green compact and the other after sintering at 1250 °C—were used for the deposition. Though the targets varied with respect to physical properties such as crystallite size (11–45 nm) and relative density (44% and 96%), the resultant thin films exhibited a mean crystallite size in the range of 20–25 nm underlining the role of physical nature of deposition. In spitemore » of the crystalline nature of the targets and similar elemental concentration, a transformation from amorphous to crystalline structure was observed in thin films on using sintered target. Postannealing of the as deposited film at 800 °C resulted in a polycrystalline structure consisting of CeO{sub 2} and NiO. Deposition using pure CeO{sub 2} or NiO as target resulted in the preferential orientation toward (111) and (200) planes, respectively, showing the influence of adatoms on the evaporation and growth process of NiO-CeO{sub 2} composite. The results demonstrate the influence of electron beam gun power on the adatom energy for the growth process of composite oxide thin films.« less

Directed Vapor Deposition: Low Vacuum Materials Processing Technology

DTIC Science & Technology

2000-01-01

constituent A Crucible with constituent B Electron beam AB Substrate Deposit Flux of A Flux of B Composition "Skull" melt Electron beam Coolant Copper ... crucible Evaporation target Evaporant material Vapor flux Fibrous Coating Surface a) b) sharp (0.5 mm) beam focussing. When used with multisource

Chemical Vapor Deposition of Aluminum Oxide Thin Films

ERIC Educational Resources Information Center

Vohs, Jason K.; Bentz, Amy; Eleamos, Krystal; Poole, John; Fahlman, Bradley D.

2010-01-01

Chemical vapor deposition (CVD) is a process routinely used to produce thin films of materials via decomposition of volatile precursor molecules. Unfortunately, the equipment required for a conventional CVD experiment is not practical or affordable for many undergraduate chemistry laboratories, especially at smaller institutions. In an effort to…

Low-temperature growth of highly crystalline β-Ga2O3 nanowires by solid-source chemical vapor deposition

PubMed Central

2014-01-01

Growing Ga2O3 dielectric materials at a moderately low temperature is important for the further development of high-mobility III-V semiconductor-based nanoelectronics. Here, β-Ga2O3 nanowires are successfully synthesized at a relatively low temperature of 610°C by solid-source chemical vapor deposition employing GaAs powders as the source material, which is in a distinct contrast to the typical synthesis temperature of above 1,000°C as reported by other methods. In this work, the prepared β-Ga2O3 nanowires are mainly composed of Ga and O elements with an atomic ratio of approximately 2:3. Importantly, they are highly crystalline in the monoclinic structure with varied growth orientations in low-index planes. The bandgap of the β-Ga2O3 nanowires is determined to be 251 nm (approximately 4.94 eV), in good accordance with the literature. Also, electrical characterization reveals that the individual nanowire has a resistivity of up to 8.5 × 107 Ω cm, when fabricated in the configuration of parallel arrays, further indicating the promise of growing these highly insulating Ga2O3 materials in this III-V nanowire-compatible growth condition. PACS 77.55.D; 61.46.Km; 78.40.Fy PMID:25114641

Low-temperature growth of highly crystalline β-Ga2O3 nanowires by solid-source chemical vapor deposition.

PubMed

Han, Ning; Wang, Fengyun; Yang, Zaixing; Yip, SenPo; Dong, Guofa; Lin, Hao; Fang, Ming; Hung, TakFu; Ho, Johnny C

2014-01-01

Growing Ga2O3 dielectric materials at a moderately low temperature is important for the further development of high-mobility III-V semiconductor-based nanoelectronics. Here, β-Ga2O3 nanowires are successfully synthesized at a relatively low temperature of 610°C by solid-source chemical vapor deposition employing GaAs powders as the source material, which is in a distinct contrast to the typical synthesis temperature of above 1,000°C as reported by other methods. In this work, the prepared β-Ga2O3 nanowires are mainly composed of Ga and O elements with an atomic ratio of approximately 2:3. Importantly, they are highly crystalline in the monoclinic structure with varied growth orientations in low-index planes. The bandgap of the β-Ga2O3 nanowires is determined to be 251 nm (approximately 4.94 eV), in good accordance with the literature. Also, electrical characterization reveals that the individual nanowire has a resistivity of up to 8.5 × 10(7) Ω cm, when fabricated in the configuration of parallel arrays, further indicating the promise of growing these highly insulating Ga2O3 materials in this III-V nanowire-compatible growth condition. 77.55.D; 61.46.Km; 78.40.Fy.

Development of a Computational Chemical Vapor Deposition Model: Applications to Indium Nitride and Dicyanovinylaniline

NASA Technical Reports Server (NTRS)

Cardelino, Carlos

1999-01-01

A computational chemical vapor deposition (CVD) model is presented, that couples chemical reaction mechanisms with fluid dynamic simulations for vapor deposition experiments. The chemical properties of the systems under investigation are evaluated using quantum, molecular and statistical mechanics models. The fluid dynamic computations are performed using the CFD-ACE program, which can simulate multispecies transport, heat and mass transfer, gas phase chemistry, chemistry of adsorbed species, pulsed reactant flow and variable gravity conditions. Two experimental setups are being studied, in order to fabricate films of: (a) indium nitride (InN) from the gas or surface phase reaction of trimethylindium and ammonia; and (b) 4-(1,1)dicyanovinyl-dimethylaminoaniline (DCVA) by vapor deposition. Modeling of these setups requires knowledge of three groups of properties: thermodynamic properties (heat capacity), transport properties (diffusion, viscosity, and thermal conductivity), and kinetic properties (rate constants for all possible elementary chemical reactions). These properties are evaluated using computational methods whenever experimental data is not available for the species or for the elementary reactions. The chemical vapor deposition model is applied to InN and DCVA. Several possible InN mechanisms are proposed and analyzed. The CVD model simulations of InN show that the deposition rate of InN is more efficient when pulsing chemistry is used under conditions of high pressure and microgravity. An analysis of the chemical properties of DCVA show that DCVA dimers may form under certain conditions of physical vapor transport. CVD simulations of the DCVA system suggest that deposition of the DCVA dimer may play a small role in the film and crystal growth processes.

Methods of amorphization and investigation of the amorphous state.

PubMed

Einfal, Tomaž; Planinšek, Odon; Hrovat, Klemen

2013-09-01

The amorphous form of pharmaceutical materials represents the most energetic solid state of a material. It provides advantages in terms of dissolution rate and bioavailability. This review presents the methods of solid- -state amorphization described in literature (supercooling of liquids, milling, lyophilization, spray drying, dehydration of crystalline hydrates), with the emphasis on milling. Furthermore, we describe how amorphous state of pharmaceuticals differ depending on the method of preparation and how these differences can be screened by a variety of spectroscopic (X-ray powder diffraction, solid state nuclear magnetic resonance, atomic pairwise distribution, infrared spectroscopy, terahertz spectroscopy) and calorimetry methods.

Hydrodynamic and Chemical Modeling of a Chemical Vapor Deposition Reactor for Zirconia Deposition

NASA Astrophysics Data System (ADS)

Belmonte, T.; Gavillet, J.; Czerwiec, T.; Ablitzer, D.; Michel, H.

1997-09-01

Zirconia is deposited on cylindrical substrates by flowing post-discharge enhanced chemical vapor deposition. In this paper, a two dimensional hydrodynamic and chemical modeling of the reactor is described for given plasma characteristics. It helps in determining rate constants of the synthesis reaction of zirconia in gas phase and on the substrate which is ZrCl4 hydrolysis. Calculated deposition rate profiles are obtained by modeling under various conditions and fits with a satisfying accuracy the experimental results. The role of transport processes and the mixing conditions of excited gases with remaining ones are studied. Gas phase reaction influence on the growth rate is also discussed.

Direct synthesis of large area graphene on insulating substrate by gallium vapor-assisted chemical vapor deposition

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

Murakami, Katsuhisa, E-mail: k.murakami@bk.tsukuba.ac.jp; Hiyama, Takaki; Kuwajima, Tomoya

2015-03-02

A single layer of graphene with dimensions of 20 mm × 20 mm was grown directly on an insulating substrate by chemical vapor deposition using Ga vapor catalysts. The graphene layer showed highly homogeneous crystal quality over a large area on the insulating substrate. The crystal quality of the graphene was measured by Raman spectroscopy and was found to improve with increasing Ga vapor density on the reaction area. High-resolution transmission electron microscopy observations showed that the synthesized graphene had a perfect atomic-scale crystal structure within its grains, which ranged in size from 50 nm to 200 nm.

Amorphous surface layer versus transient amorphous precursor phase in bone - A case study investigated by solid-state NMR spectroscopy.

PubMed

Von Euw, Stanislas; Ajili, Widad; Chan-Chang, Tsou-Hsi-Camille; Delices, Annette; Laurent, Guillaume; Babonneau, Florence; Nassif, Nadine; Azaïs, Thierry

2017-09-01

The presence of an amorphous surface layer that coats a crystalline core has been proposed for many biominerals, including bone mineral. In parallel, transient amorphous precursor phases have been proposed in various biomineralization processes, including bone biomineralization. Here we propose a methodology to investigate the origin of these amorphous environments taking the bone tissue as a key example. This study relies on the investigation of a bone tissue sample and its comparison with synthetic calcium phosphate samples, including a stoichiometric apatite, an amorphous calcium phosphate sample, and two different biomimetic apatites. To reveal if the amorphous environments in bone originate from an amorphous surface layer or a transient amorphous precursor phase, a combined solid-state nuclear magnetic resonance (NMR) experiment has been used. The latter consists of a double cross polarization 1 H→ 31 P→ 1 H pulse sequence followed by a 1 H magnetization exchange pulse sequence. The presence of an amorphous surface layer has been investigated through the study of the biomimetic apatites; while the presence of a transient amorphous precursor phase in the form of amorphous calcium phosphate particles has been mimicked with the help of a physical mixture of stoichiometric apatite and amorphous calcium phosphate. The NMR results show that the amorphous and the crystalline environments detected in our bone tissue sample belong to the same particle. The presence of an amorphous surface layer that coats the apatitic core of bone apatite particles has been unambiguously confirmed, and it is certain that this amorphous surface layer has strong implication on bone tissue biogenesis and regeneration. Questions still persist on the structural organization of bone and biomimetic apatites. The existing model proposes a core/shell structure, with an amorphous surface layer coating a crystalline bulk. The accuracy of this model is still debated because amorphous calcium

Particle formation in SiOx film deposition by low frequency plasma enhanced chemical vapor deposition

NASA Astrophysics Data System (ADS)

Yamaguchi, Tomoyo; Sakamoto, Naoshi; Shimozuma, Mitsuo; Yoshino, Masaki; Tagashira, Hiroaki

1998-01-01

Dust particle formation dynamics in the process of SiOx film deposition from a SiH4 and N2O gas mixture by a low frequency plasma enhanced chemical vapor deposition have been investigated using scanning electron microscopy and laser light scattering. The deposited films are confirmed to be SiOx from the measurements of Auger electron spectroscopy, x-ray photoelectron spectroscopy, and Fourier transform infrared spectroscopy. It is observed by scanning electron microscopy that particles are deposited on Si substrate at the plasma power frequency f=5 kHz and above both with and without substrate heating (400 °C), while no particle is deposited below f=1 kHz. Moreover, the laser light scattering indicates that particles are generated at the plasma power frequency of f=3 kHz and above in the gas phase, and that they are not generated in the gas phase at below f=3 kHz. Properties (the refractive index, resistivity, and Vickers hardness) of the films with particles are inferior to those of the films without particles. This article has revealed experimentally the effect of plasma power frequency on SiOx particle formation and makes a contribution to the explication of the particle formation mechanism. We suggest that high-quality film deposition with the low frequency plasma enhanced chemical vapor deposition method is attained at f=1 kHz or less without substrate heating.

Graphitized hollow carbon spheres and yolk-structured carbon spheres fabricated by metal-catalyst-free chemical vapor deposition

DOE PAGES

Li, Xufan; Chi, Miaofang; Mahurin, Shannon Mark; ...

2016-01-18

Hard-sphere-templating method has been widely used to synthesize hollow carbon spheres (HCSs), in which the spheres were firstly coated with a carbon precursor, followed by carbonization and core removal. The obtained HCSs are generally amorphous or weakly graphitized (with the help of graphitization catalysts). In this work, we report on the fabrication of graphitized HCSs and yolk–shell Au@HCS nanostructures using a modified templating method, in which smooth, uniform graphene layers were grown on SiO 2 spheres or Au@SiO 2 nanoparticles via metal-catalyst-free chemical vapor deposition (CVD) of methane. Furthermore, our work not only provides a new method to fabricate high-quality,more » graphitized HCSs but also demonstrates a reliable approach to grow quality graphene on oxide surfaces using CVD without the presence of metal catalysts.« less

Spontaneous crystalline-to-amorphous phase transformation of organic or medicinal compounds in the presence of porous media, part 2: amorphization capacity and mechanisms of interaction.

PubMed

Qian, Ken K; Suib, Steven L; Bogner, Robin H

2011-11-01

Amorphization of crystalline compounds using mesoporous media is a promising technique to improve the solubility and dissolution rate of poorly soluble compounds. The objective of this paper is to determine the capacity of amorphization and understand the mechanisms of phase transformation. Commercial grades of mesoporous silicon dioxide (SiO(2)) samples (5- to 30-nm mean pore diameters) with either constant surface area or constant pore volume were used. The amorphization capacity of naphthalene was not proportional to either the surface area or the pore volume measured using adsorption chambers. Instead, the amorphization capacity correlated with surface curvature, that is, the smaller the pore diameter and the higher the surface curvature, the greater the amorphization capacity. The change in surface chemistry due to a highly curved surface may be responsible for the enhanced amorphization capacity as well. The amorphization of crystalline compounds was facilitated through capillary condensation, with the decrease in pore volume as the direct experimental evidence. The amorphization capacity was also enhanced by the dipole-dipole or dipole-induced dipole interaction, promoted by the hydroxyl groups on the surface of SiO(2). The enthalpy of vapor-solid condensation of crystalline compounds was a useful indicator to predict the rank order of amorphization capacity. Copyright © 2011 Wiley-Liss, Inc.

Chemical vapor deposition of fluorine-doped zinc oxide

DOEpatents

Gordon, Roy G.; Kramer, Keith; Liang, Haifan

2000-06-06

Fims of fluorine-doped zinc oxide are deposited from vaporized precursor compounds comprising a chelate of a dialkylzinc, such as an amine chelate, an oxygen source, and a fluorine source. The coatings are highly electrically conductive, transparent to visible light, reflective to infrared radiation, absorbing to ultraviolet light, and free of carbon impurity.

Confined high-pressure chemical deposition of hydrogenated amorphous silicon.

PubMed

Baril, Neil F; He, Rongrui; Day, Todd D; Sparks, Justin R; Keshavarzi, Banafsheh; Krishnamurthi, Mahesh; Borhan, Ali; Gopalan, Venkatraman; Peacock, Anna C; Healy, Noel; Sazio, Pier J A; Badding, John V

2012-01-11

Hydrogenated amorphous silicon (a-Si:H) is one of the most technologically important semiconductors. The challenge in producing it from SiH(4) precursor is to overcome a significant kinetic barrier to decomposition at a low enough temperature to allow for hydrogen incorporation into a deposited film. The use of high precursor concentrations is one possible means to increase reaction rates at low enough temperatures, but in conventional reactors such an approach produces large numbers of homogeneously nucleated particles in the gas phase, rather than the desired heterogeneous deposition on a surface. We report that deposition in confined micro-/nanoreactors overcomes this difficulty, allowing for the use of silane concentrations many orders of magnitude higher than conventionally employed while still realizing well-developed films. a-Si:H micro-/nanowires can be deposited in this way in extreme aspect ratio, small-diameter optical fiber capillary templates. The semiconductor materials deposited have ~0.5 atom% hydrogen with passivated dangling bonds and good electronic properties. They should be suitable for a wide range of photonic and electronic applications such as nonlinear optical fibers and solar cells. © 2011 American Chemical Society

Electron beam physical vapor deposition of YSZ electrolyte coatings for SOFCs

NASA Astrophysics Data System (ADS)

He, Xiaodong; Meng, Bin; Sun, Yue; Liu, Bochao; Li, Mingwei

2008-09-01

YSZ electrolyte coatings were prepared by electron beam physical vapor deposition (EB-PVD) at a high deposition rate of up to 1 μm/min. The YSZ coating consisted of a single cubic phase and no phase transformation occurred after annealing treatment at 1000 °C. A typical columnar structure was observed in this coating by SEM and feather-like characteristics appeared in every columnar grain. In columnar grain boundaries there were many micron-sized gaps and pores. In TEM image, many white lines were found, originating from the alignment of nanopores existing within feather-like columnar grains. The element distribution along the cross-section of the coating was homogeneous except Zr with a slight gradient. The coating exhibited a characteristic anisotropic behavior in electrical conductivity. In the direction perpendicular to coating surface the electrical conductivity was remarkably higher than that in the direction parallel to coating surface. This mainly attributed to the typical columnar structure for EB-PVD coating and the existence of many grain boundaries along the direction parallel to coating surface. For as-deposited coating, the gas permeability coefficient of 9.78 × 10 -5 cm 4 N -1 s -1 was obtained and this value was close to the critical value of YSZ electrolyte layer required for solid oxide fuel cell (SOFC) operation.

Atomic Layer Deposition of the Solid Electrolyte LiPON

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

Kozen, Alexander C.; Pearse, Alexander J.; Lin, Chuan -Fu

We demonstrate an atomic layer deposition (ALD) process for the solid electrolyte lithium phosphorousoxynitride (LiPON) using lithium tert-butoxide (LiO tBu), H 2O, trimethylphosphate (TMP), and plasma N 2 ( PN 2) as precursors. We use in-situ spectroscopic ellipsometry to determine growth rates for process optimization to design a rational, quaternary precursor ALD process where only certain substrate–precursor chemical reactions are favorable. We demonstrate via in-situ XPS tunable nitrogen incorporation into the films by variation of the PN 2 dose and find that ALD films over approximately 4.5% nitrogen are amorphous, whereas LiPON ALD films with less than 4.5% nitrogen aremore » polycrystalline. Lastly, we characterize the ionic conductivity of the ALD films as a function of nitrogen content and demonstrate their functionality on a model battery electrode—a Si anode on a Cu current collector.« less

Atomic Layer Deposition of the Solid Electrolyte LiPON

DOE PAGES

Kozen, Alexander C.; Pearse, Alexander J.; Lin, Chuan -Fu; ...

2015-07-09

We demonstrate an atomic layer deposition (ALD) process for the solid electrolyte lithium phosphorousoxynitride (LiPON) using lithium tert-butoxide (LiO tBu), H 2O, trimethylphosphate (TMP), and plasma N 2 ( PN 2) as precursors. We use in-situ spectroscopic ellipsometry to determine growth rates for process optimization to design a rational, quaternary precursor ALD process where only certain substrate–precursor chemical reactions are favorable. We demonstrate via in-situ XPS tunable nitrogen incorporation into the films by variation of the PN 2 dose and find that ALD films over approximately 4.5% nitrogen are amorphous, whereas LiPON ALD films with less than 4.5% nitrogen aremore » polycrystalline. Lastly, we characterize the ionic conductivity of the ALD films as a function of nitrogen content and demonstrate their functionality on a model battery electrode—a Si anode on a Cu current collector.« less

Communication: Distinguishing between bulk and interface-enhanced crystallization in nanoscale films of amorphous solid water.

PubMed

Yuan, Chunqing; Smith, R Scott; Kay, Bruce D

2017-01-21

The crystallization of amorphous solid water (ASW) nanoscale films was investigated using reflection absorption infrared spectroscopy. Two ASW film configurations were studied. In one case the ASW film was deposited on top of and capped with a decane layer ("sandwich" configuration). In the other case, the ASW film was deposited on top of a decane layer and not capped ("no cap" configuration). Crystallization of ASW films in the "sandwich" configuration is about eight times slower than in the "no cap." Selective placement of an isotopic layer (5% D 2 O in H 2 O) at various positions in an ASW (H 2 O) film was used to determine the crystallization mechanism. In the "sandwich" configuration, the crystallization kinetics were independent of the isotopic layer placement whereas in the "no cap" configuration the closer the isotopic layer was to the vacuum interface, the earlier the isotopic layer crystallized. These results are consistent with a mechanism whereby the decane overlayer suppresses surface nucleation and provide evidence that the observed ASW crystallization in "sandwich" films is the result of uniform bulk nucleation.

Surface Morphology of Vapor-Deposited Chitosan: Evidence of Solid-State Dewetting during the Formation of Biopolymer Films.

PubMed

Retamal, Maria Jose; Corrales, Tomas P; Cisternas, Marcelo A; Moraga, Nicolas H; Diaz, Diego I; Catalan, Rodrigo E; Seifert, Birger; Huber, Patrick; Volkmann, Ulrich G

2016-03-14

Chitosan is a useful and versatile biopolymer with several industrial and biological applications. Whereas its physical and physicochemical bulk properties have been explored quite intensively in the past, there is a lack of studies regarding the morphology and growth mechanisms of thin films of this biopolymer. Of particular interest for applications in bionanotechnology are ultrathin films with thicknesses under 500 Å. Here, we present a study of thin chitosan films prepared in a dry process using physical vapor deposition and in situ ellipsometric monitoring. The prepared films were analyzed with atomic force microscopy in order to correlate surface morphology with evaporation parameters. We find that the surface morphology of our final thin films depends on both the optical thickness, i.e., measured with ellipsometry, and the deposition rate. Our work shows that ultrathin biopolymer films can undergo dewetting during film formation, even in the absence of solvents and thermal annealing.

Lattice Matched Iii-V IV Semiconductor Heterostructures: Metalorganic Chemical Vapor Deposition and Remote Plasma Enhanced Chemical Vapor Deposition.

NASA Astrophysics Data System (ADS)

Choi, Sungwoo

1992-01-01

This thesis describes the growth and characterization of wide gap III-V compound semiconductors such as aluminum gallium arsenide (Al_{rm x} Ga_{rm 1-x}As), gallium nitride (GaN), and gallium phosphide (GaP), deposited by the metalorganic chemical vapor deposition (MOCVD) and remote plasma enhanced chemical vapor deposition (Remote PECVD). In the first part of the thesis, the optimization of GaAs and Al_{rm x}Ga _{rm 1-x}As hetero -epitaxial layers on Ge substrates is described in the context of the application in the construction of cascade solar cells. The emphasis on this study is on the trade-offs in the choice of the temperature related to increasing interdiffusion/autodoping and increasing perfection of the epilayer with increasing temperature. The structural, chemical, optical, and electrical properties of the heterostructures are characterized by x-ray rocking curve measurement, scanning electron microscopy (SEM), electron beam induced current (EBIC), cross-sectional transmission electron microscopy (X-TEM), Raman spectroscopy, secondary ion mass spectrometry (SIMS), and steady-state and time-resolved photoluminescence (PL). Based on the results of this work the optimum growth temperature is 720^circC. The second part of the thesis describes the growth of GaN and GaP layers on silicon and sapphire substrates and the homoepitaxy of GaP by remote PECVD. I have designed and built an ultra high vacuum (UHV) deposition system which includes: the gas supply system, the pumping system, the deposition chamber, the load-lock chamber, and the waste disposal system. The work on the deposition of GaN on Si and sapphire focuses onto the understanding of the growth kinetics. In addition, Auger electron spectroscopy (AES) for surface analysis, x-ray diffraction methods and microscopic analyses using SEM and TEM for structural characterization, infrared (IR) and ultraviolet (UV) absorption measurements for optical characterization, and electrical characterization results

Enhanced performance of a structured cyclo olefin copolymer-based amorphous silicon solar cell

NASA Astrophysics Data System (ADS)

Zhan, Xinghua; Chen, Fei; Gao, Mengyu; Tie, Shengnian; Gao, Wei

2017-07-01

The submicron array was fabricated onto a cyclo olefin copolymer (COC) film by a hot embossing method. An amorphous silicon p-i-n junction and transparent conductive layers were then deposited onto it through a plasma enhanced chemical vapor deposition (PECVD) and magnetron sputtering. The efficiency of the fabricated COC-based solar cell was measured and the result demonstrated 18.6% increase of the solar cell efficiency when compared to the sample without array structure. The imprinted polymer solar cells with submicron array indeed increase their efficiency.

Vapor-solid-solid grown Ge nanowires at integrated circuit compatible temperature by molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Zhu, Zhongyunshen; Song, Yuxin; Zhang, Zhenpu; Sun, Hao; Han, Yi; Li, Yaoyao; Zhang, Liyao; Xue, Zhongying; Di, Zengfeng; Wang, Shumin

2017-09-01

We demonstrate Au-assisted vapor-solid-solid (VSS) growth of Ge nanowires (NWs) by molecular beam epitaxy at the substrate temperature of ˜180 °C, which is compatible with the temperature window for Si-based integrated circuit. Low temperature grown Ge NWs hold a smaller size, similar uniformity, and better fit with Au tips in diameter, in contrast to Ge NWs grown at around or above the eutectic temperature of Au-Ge alloy in the vapor-liquid-solid (VLS) growth. Six ⟨110⟩ growth orientations were observed on Ge (110) by the VSS growth at ˜180 °C, differing from only one vertical growth direction of Ge NWs by the VLS growth at a high temperature. The evolution of NWs dimension and morphology from the VLS growth to the VSS growth is qualitatively explained by analyzing the mechanism of the two growth modes.

Model for the Vaporization of Mixed Organometallic Compounds in the Metalorganic Chemical Vapor Deposition of High Temperature Superconducting Films

NASA Technical Reports Server (NTRS)

Meng, Guangyao; Zhou, Gang; Schneider, Roger L.; Sarma, Bimal K.; Levy, Moises

1993-01-01

A model of the vaporization and mass transport of mixed organometallics from a single source for thin film metalorganic chemical vapor deposition is presented. A stoichiometric gas phase can be obtained from a mixture of the organometallics in the desired mole ratios, in spite of differences in the volatilities of the individual compounds. Proper film composition and growth rates are obtained by controlling the velocity of a carriage containing the organometallics through the heating zone of a vaporizer.

Preventing kinetic roughening in physical vapor-phase-deposited films.

PubMed

Vasco, E; Polop, C; Sacedón, J L

2008-01-11

The growth kinetics of the mostly used physical vapor-phase deposition techniques -molecular beam epitaxy, sputtering, flash evaporation, and pulsed laser deposition-is investigated by rate equations with the aim of testing their suitability for the preparation of ultraflat ultrathin films. The techniques are studied in regard to the roughness and morphology during early stages of growth. We demonstrate that pulsed laser deposition is the best technique for preparing the flattest films due to two key features [use of (i) a supersaturated pulsed flux of (ii) hyperthermal species] that promote a kinetically limited Ostwald ripening mechanism.

Vapor deposition on doublet airfoil substrates: Control of coating thickness and microstructure

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

Rodgers, Theron M.; Zhao, Hengbei; Wadley, Haydn N. G., E-mail: haydn@virginia.edu

Gas jet assisted vapor deposition processes for depositing coatings are conducted at higher pressures than conventional physical vapor deposition methods, and have shown promise for coating complex shaped substrates including those with non-line-of-sight (NLS) regions on their surface. These regions typically receive vapor atoms at a lower rate and with a wider incident angular distribution than substrate regions in line-of-sight (LS) of the vapor source. To investigate the coating of such substrates, the thickness and microstructure variation along the inner (curved) surfaces of a model doublet airfoil containing both LS and NLS regions has been investigated. Results from atomistic simulationsmore » and experiments confirm that the coating's thickness is thinner in flux-shadowed regions than in other regions for all the coating processes investigated. They also indicated that the coatings columnar microstructure and pore volume fraction vary with surface location through the LS to NLS transition zone. A substrate rotation strategy for optimizing the thickness over the entire doublet airfoil surface was investigated, and led to the identification of a process that resulted in only small variation of coating thickness, columnar growth angle, and pore volume fraction on all doublet airfoil surfaces.« less

A study of pyrolysis of oil shale of the Leningrad deposit by solid heat carrier

NASA Astrophysics Data System (ADS)

Gerasimov, G. Ya; Khaskhachikh, V. V.; Potapov, O. P.

2017-11-01

The investigation of the oil shale pyrolysis with a solid heat carrier was carried out using the experimental retorting system that simulates the Galoter industrial process. This system allows verifying both fractional composition of the oil shale and solid heat carrier, and their ratio and temperature. The oil shale of the Leningradsky deposit was used in the work, and quartz sand was used as the solid heat carrier. It is shown that the yield of the shale oil under the pyrolysis with solid heat carrier exceeds by more than 20% the results received in the standard Fisher retort. Using ash as the solid heat carrier results in a decrease in the yield of oil and gas with simultaneous increase in the amount of the solid residue. This is due to the chemical interaction of the acid components of the vapor-gas mixture with the oxides of alkaline-earth metals that are part of the ash.

Plasma Spray-PVD: A New Thermal Spray Process to Deposit Out of the Vapor Phase

NASA Astrophysics Data System (ADS)

von Niessen, Konstantin; Gindrat, Malko

2011-06-01

Plasma spray-physical vapor deposition (PS-PVD) is a low pressure plasma spray technology recently developed by Sulzer Metco AG (Switzerland). Even though it is a thermal spray process, it can deposit coatings out of the vapor phase. The basis of PS-PVD is the low pressure plasma spraying (LPPS) technology that has been well established in industry for several years. In comparison to conventional vacuum plasma spraying (VPS) or low pressure plasma spraying (LPPS), the new proposed process uses a high energy plasma gun operated at a reduced work pressure of 0.1 kPa (1 mbar). Owing to the high energy plasma and further reduced work pressure, PS-PVD is able to deposit a coating not only by melting the feed stock material which builds up a layer from liquid splats but also by vaporizing the injected material. Therefore, the PS-PVD process fills the gap between the conventional physical vapor deposition (PVD) technologies and standard thermal spray processes. The possibility to vaporize feedstock material and to produce layers out of the vapor phase results in new and unique coating microstructures. The properties of such coatings are superior to those of thermal spray and electron beam-physical vapor deposition (EB-PVD) coatings. In contrast to EB-PVD, PS-PVD incorporates the vaporized coating material into a supersonic plasma plume. Owing to the forced gas stream of the plasma jet, complex shaped parts such as multi-airfoil turbine vanes can be coated with columnar thermal barrier coatings using PS-PVD. Even shadowed areas and areas which are not in the line of sight of the coating source can be coated homogeneously. This article reports on the progress made by Sulzer Metco in developing a thermal spray process to produce coatings out of the vapor phase. Columnar thermal barrier coatings made of Yttria-stabilized Zircona (YSZ) are optimized to serve in a turbine engine. This process includes not only preferable coating properties such as strain tolerance and erosion

Low-Cost III-V Photovoltaic Materials by Chloride Vapor Transport Deposition Using Safe Solid Precursors

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

Boettcher, Shannon; Aloni, Shaul; Weiss, Robert

Si-based photovoltaic devices dominate the market. As photovoltaic (PV) manufacturing costs have plummeted, technologies which increase efficiency have become critical. Si cell efficiencies are nearing theoretical limits and Si-based PV modules are unlikely to reach the 25-30% efficiency range. The use of III-V semiconductors is an obvious technical solution to improve efficiency, especially if they can be integrated directly with existing Si technology as tandems. High coefficients of light absorption along with tunable bandgaps and lattice constants have resulted in record conversion efficiencies for both one-sun and concentrator PV applications. GaAs, for example, has been used to manufacture single-junction photovoltaicsmore » with world-record efficiencies of 28.8% at one sun.2 However, costs for III-Vs must be dramatically reduced to produce cost-effective, high-efficiency PV solutions. III-V costs are controlled by two factors: semiconductor growth and the substrate. III-V growth is dominated today by metal-organic vapor phase epitaxy (MOVPE) with a lesser role played by molecular beam epitaxy (MBE). MOVPE costs are high due to the expense and low utilization (~30%) of precursors, modest growth rates (~100 nm min-1), equipment complexity, and safety infrastructure needed to handle toxic, pyrophoric gases.3 MBE costs are high due to slow growth rates and limitations of scalability. Details comparing plausible low-cost III-V growth methods are available in a review article published as a result of this project. The primary goal of this project was to demonstrate that close-spaced vapor transport (CSVT) using chloride (from HCl) as a transport agent can be used for the rapid growth of device-ready III-V layers from safe, solid-source precursors. In pursuit of this goal, we designed, built, and installed a new Cl-CSVT reactor based on insights from our previous H2O-CSVT growth system and in collaboration with equipment professionals at Malachite Technologies

Room temperature deposition of silicon nanodot clusters by plasma-enhanced chemical vapor deposition.

PubMed

Kim, Jae-Kwan; Kim, Jun Young; Yoon, Jae-Sik; Lee, Ji-Myon

2013-10-01

The formation of nanometer-scale (ns)-Si dots and clusters on p-GaN layers has been studied by controlling the early stage of growth during plasma-enhanced chemical vapor deposition (PECVD) at room temperature. We found that ns-Si dots and clusters formed on the p-GaN surface, indicating that growth was the Volmer-Weber mode. The deposition parameters such as radio frequency (RF) power and processing time mainly influenced the size of the ns-Si dots (40 nm-160 nm) and the density of the ns-Si dot clusters.

Boron nitride nanowires synthesis via a simple chemical vapor deposition at 1200 °C

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

Ahmad, Pervaiz; Khandaker, Mayeen Uddin; Amin, Yusoff Mohd

2015-04-24

A very simple chemical vapor deposition technique is used to synthesize high quality boron nitride nanowires at 1200 °C within a short growth duration of 30 min. FESEM micrograph shows that the as-synthesized boron nitride nanowires have a clear wire like morphology with diameter in the range of ∼20 to 150 nm. HR-TEM confirmed the wire-like structure of boron nitride nanowires, whereas XPS and Raman spectroscopy are used to find out the elemental composition and phase of the synthesized material. The synthesized boron nitride nanowires have potential applications as a sensing element in solid state neutron detector, neutron capture therapy and microelectronicmore » devices with uniform electronic properties.« less

Experimental verification of vapor deposition rate theory in high velocity burner rigs

NASA Technical Reports Server (NTRS)

Gokoglu, Suleyman A.; Santoro, Gilbert J.

1985-01-01

The main objective has been the experimental verification of the corrosive vapor deposition theory in high-temperature, high-velocity environments. Towards this end a Mach 0.3 burner-rig appartus was built to measure deposition rates from salt-seeded (mostly Na salts) combustion gases on the internally cooled cylindrical collector. Deposition experiments are underway.

Coaxial carbon plasma gun deposition of amorphous carbon films

NASA Technical Reports Server (NTRS)

Sater, D. M.; Gulino, D. A.; Rutledge, S. K.

1984-01-01

A unique plasma gun employing coaxial carbon electrodes was used in an attempt to deposit thin films of amorphous diamond-like carbon. A number of different structural, compositional, and electrical characterization techniques were used to characterize these films. These included scanning electron microscopy, scanning transmission electron microscopy, X ray diffraction and absorption, spectrographic analysis, energy dispersive spectroscopy, and selected area electron diffraction. Optical absorption and electrical resistivity measurements were also performed. The films were determined to be primarily amorphous, with poor adhesion to fused silica substrates. Many inclusions of particulates were found to be present as well. Analysis of these particulates revealed the presence of trace impurities, such as Fe and Cu, which were also found in the graphite electrode material. The electrodes were the source of these impurities. No evidence of diamond-like crystallite structure was found in any of the film samples. Details of the apparatus, experimental procedure, and film characteristics are presented.

Method of controllong the deposition of hydrogenated amorphous silicon and apparatus therefor

DOEpatents

Hanak, Joseph J.

1985-06-25

An improved method and apparatus for the controlled deposition of a layer of hydrogenated amorphous silicon on a substrate. Means is provided for the illumination of the coated surface of the substrate and measurement of the resulting photovoltage at the outermost layer of the coating. Means is further provided for admixing amounts of p type and n type dopants to the reactant gas in response to the measured photovoltage to achieve a desired level and type of doping of the deposited layer.

Chemical vapor deposition of W-Si-N and W-B-N

DOEpatents

Fleming, James G.; Roherty-Osmun, Elizabeth Lynn; Smith, Paul M.; Custer, Jonathan S.; Jones, Ronald V.; Nicolet, Marc-A.; Madar, Roland; Bernard, Claude

1999-01-01

A method of depositing a ternary, refractory based thin film on a substrate by chemical vapor deposition employing precursor sources of tungsten comprising WF.sub.6, either silicon or boron, and nitrogen. The result is a W--Si--N or W--B--N thin film useful for diffusion barrier and micromachining applications.

Effect of deposition pressure on the morphology and structural properties of carbon nanotubes synthesized by hot-filament chemical vapor deposition.

PubMed

Arendse, C J; Malgas, G F; Scriba, M R; Cummings, F R; Knoesen, D

2007-10-01

Hot-filament chemical vapor deposition has developed into an attractive method for the synthesis of various carbon nanostructures, including carbon nanotubes. This is primarily due to its versatility, low cost, repeatability, up-scalability, and ease of production. The resulting nano-material synthesized by this technique is dependent on the deposition conditions which can be easily controlled. In this paper we report on the effect of the deposition pressure on the structural properties and morphology of carbon nanotubes synthesized by hot-filament chemical vapor deposition, using Raman spectroscopy and high-resolution scanning electron microscopy, respectively. A 10 nm-thick Ni layer, deposited on a SiO2/Si substrate, was used as catalyst for carbon nanotube growth. Multi-walled carbon nanotubes with diameters ranging from 20-100 nm were synthesized at 500 degrees C with high structural perfection at deposition pressures between 150 and 200 Torr. Raman spectroscopy measurements confirm that the carbon nanotube deposit is homogeneous across the entire substrate area.

Photo-oxidation of polymer-like amorphous hydrogenated carbon under visible light illumination

DOE PAGES

Baxamusa, Salmaan; Laurence, Ted; Worthington, Matthew; ...

2015-11-10

Amorphous hydrogenated carbon (a-C:H), a polymer-like network typically synthesized by plasma chemical vapor deposition, has long been understood to exhibit optical absorption of visible light (λ > 400 nm). In this report we explain that this absorption is accompanied by rapid photo-oxidation (within minutes) that behaves in most respects like classic polymer photo-oxidation with the exception that it occurs under visible light illumination rather than ultraviolet illumination.

Physical stabilization of low-molecular-weight amorphous drugs in the solid state: a material science approach.

PubMed

Qi, Sheng; McAuley, William J; Yang, Ziyi; Tipduangta, Pratchaya

2014-07-01

Use of the amorphous state is considered to be one of the most effective approaches for improving the dissolution and subsequent oral bioavailability of poorly water-soluble drugs. However as the amorphous state has much higher physical instability in comparison with its crystalline counterpart, stabilization of amorphous drugs in a solid-dosage form presents a major challenge to formulators. The currently used approaches for stabilizing amorphous drug are discussed in this article with respect to their preparation, mechanism of stabilization and limitations. In order to realize the potential of amorphous formulations, significant efforts are required to enable the prediction of formulation performance. This will facilitate the development of computational tools that can inform a rapid and rational formulation development process for amorphous drugs.

On coarse projective integration for atomic deposition in amorphous systems

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

Chuang, Claire Y., E-mail: yungc@seas.upenn.edu, E-mail: meister@unm.edu, E-mail: zepedaruiz1@llnl.gov; Sinno, Talid, E-mail: talid@seas.upenn.edu; Han, Sang M., E-mail: yungc@seas.upenn.edu, E-mail: meister@unm.edu, E-mail: zepedaruiz1@llnl.gov

2015-10-07

Direct molecular dynamics simulation of atomic deposition under realistic conditions is notoriously challenging because of the wide range of time scales that must be captured. Numerous simulation approaches have been proposed to address the problem, often requiring a compromise between model fidelity, algorithmic complexity, and computational efficiency. Coarse projective integration, an example application of the “equation-free” framework, offers an attractive balance between these constraints. Here, periodically applied, short atomistic simulations are employed to compute time derivatives of slowly evolving coarse variables that are then used to numerically integrate differential equations over relatively large time intervals. A key obstacle to themore » application of this technique in realistic settings is the “lifting” operation in which a valid atomistic configuration is recreated from knowledge of the coarse variables. Using Ge deposition on amorphous SiO{sub 2} substrates as an example application, we present a scheme for lifting realistic atomistic configurations comprised of collections of Ge islands on amorphous SiO{sub 2} using only a few measures of the island size distribution. The approach is shown to provide accurate initial configurations to restart molecular dynamics simulations at arbitrary points in time, enabling the application of coarse projective integration for this morphologically complex system.« less

On Coarse Projective Integration for Atomic Deposition in Amorphous Systems

DOE PAGES

Chuang, Claire Y.; Han, Sang M.; Zepeda-Ruiz, Luis A.; ...

2015-10-02

Direct molecular dynamics simulation of atomic deposition under realistic conditions is notoriously challenging because of the wide range of timescales that must be captured. Numerous simulation approaches have been proposed to address the problem, often requiring a compromise between model fidelity, algorithmic complexity and computational efficiency. Coarse projective integration, an example application of the ‘equation-free’ framework, offers an attractive balance between these constraints. Here, periodically applied, short atomistic simulations are employed to compute gradients of slowly-evolving coarse variables that are then used to numerically integrate differential equations over relatively large time intervals. A key obstacle to the application of thismore » technique in realistic settings is the ‘lifting’ operation in which a valid atomistic configuration is recreated from knowledge of the coarse variables. Using Ge deposition on amorphous SiO 2 substrates as an example application, we present a scheme for lifting realistic atomistic configurations comprised of collections of Ge islands on amorphous SiO 2 using only a few measures of the island size distribution. In conclusion, the approach is shown to provide accurate initial configurations to restart molecular dynamics simulations at arbitrary points in time, enabling the application of coarse projective integration for this morphologically complex system.« less

Influence of vapor deposition on structural and charge transport properties of ethylbenzene films

DOE PAGES

Antony, Lucas W.; Jackson, Nicholas E.; Lyubimov, Ivan; ...

2017-04-14

Organic glass films formed by physical vapor deposition exhibit enhanced stability relative to those formed by conventional liquid cooling and aging techniques. Recently, experimental and computational evidence has emerged indicating that the average molecular orientation can be tuned by controlling the substrate temperature at which these “stable glasses” are grown. In this work, we present a comprehensive all-atom simulation study of ethylbenzene, a canonical stable-glass former, using a computational film formation procedure that closely mimics the vapor deposition process. Atomistic studies of experimentally formed vapor-deposited glasses have not been performed before, and this study therefore begins by verifying that themore » model and method utilized here reproduces key structural features observed experimentally. Having established agreement between several simulated and experimental macroscopic observables, simulations are used to examine the substrate temperature dependence of molecular orientation. The results indicate that ethylbenzene glasses are anisotropic, depending upon substrate temperature, and that this dependence can be understood from the orientation present at the surface of the equilibrium liquid. By treating ethylbenzene as a simple model for molecular semiconducting materials, a quantum-chemical analysis is then used to show that the vapor-deposited glasses exhibit decreased energetic disorder and increased magnitude of the mean-squared transfer integral relative to isotropic, liquid-cooled films, an effect that is attributed to the anisotropic ordering of the molecular film. Finally, these results suggest a novel structure–function simulation strategy capable of tuning the electronic properties of organic semiconducting glasses prior to experimental deposition, which could have considerable potential for organic electronic materials design.« less

Influence of vapor deposition on structural and charge transport properties of ethylbenzene films

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

Antony, Lucas W.; Jackson, Nicholas E.; Lyubimov, Ivan

Organic glass films formed by physical vapor deposition exhibit enhanced stability relative to those formed by conventional liquid cooling and aging techniques. Recently, experimental and computational evidence has emerged indicating that the average molecular orientation can be tuned by controlling the substrate temperature at which these “stable glasses” are grown. In this work, we present a comprehensive all-atom simulation study of ethylbenzene, a canonical stable-glass former, using a computational film formation procedure that closely mimics the vapor deposition process. Atomistic studies of experimentally formed vapor-deposited glasses have not been performed before, and this study therefore begins by verifying that themore » model and method utilized here reproduces key structural features observed experimentally. Having established agreement between several simulated and experimental macroscopic observables, simulations are used to examine the substrate temperature dependence of molecular orientation. The results indicate that ethylbenzene glasses are anisotropic, depending upon substrate temperature, and that this dependence can be understood from the orientation present at the surface of the equilibrium liquid. By treating ethylbenzene as a simple model for molecular semiconducting materials, a quantum-chemical analysis is then used to show that the vapor-deposited glasses exhibit decreased energetic disorder and increased magnitude of the mean-squared transfer integral relative to isotropic, liquid-cooled films, an effect that is attributed to the anisotropic ordering of the molecular film. Finally, these results suggest a novel structure–function simulation strategy capable of tuning the electronic properties of organic semiconducting glasses prior to experimental deposition, which could have considerable potential for organic electronic materials design.« less

Influence of Vapor Deposition on Structural and Charge Transport Properties of Ethylbenzene Films

PubMed Central

2017-01-01

Organic glass films formed by physical vapor deposition exhibit enhanced stability relative to those formed by conventional liquid cooling and aging techniques. Recently, experimental and computational evidence has emerged indicating that the average molecular orientation can be tuned by controlling the substrate temperature at which these “stable glasses” are grown. In this work, we present a comprehensive all-atom simulation study of ethylbenzene, a canonical stable-glass former, using a computational film formation procedure that closely mimics the vapor deposition process. Atomistic studies of experimentally formed vapor-deposited glasses have not been performed before, and this study therefore begins by verifying that the model and method utilized here reproduces key structural features observed experimentally. Having established agreement between several simulated and experimental macroscopic observables, simulations are used to examine the substrate temperature dependence of molecular orientation. The results indicate that ethylbenzene glasses are anisotropic, depending upon substrate temperature, and that this dependence can be understood from the orientation present at the surface of the equilibrium liquid. By treating ethylbenzene as a simple model for molecular semiconducting materials, a quantum-chemical analysis is then used to show that the vapor-deposited glasses exhibit decreased energetic disorder and increased magnitude of the mean-squared transfer integral relative to isotropic, liquid-cooled films, an effect that is attributed to the anisotropic ordering of the molecular film. These results suggest a novel structure–function simulation strategy capable of tuning the electronic properties of organic semiconducting glasses prior to experimental deposition, which could have considerable potential for organic electronic materials design. PMID:28573203

Chemical vapor deposition growth

NASA Technical Reports Server (NTRS)

Ruth, R. P.; Manasevit, H. M.; Kenty, J. L.; Moudy, L. A.; Simpson, W. I.; Yang, J. J.

1976-01-01

The chemical vapor deposition (CVD) method for the growth of Si sheet on inexpensive substrate materials is investigated. The objective is to develop CVD techniques for producing large areas of Si sheet on inexpensive substrate materials, with sheet properties suitable for fabricating solar cells meeting the technical goals of the Low Cost Silicon Solar Array Project. Specific areas covered include: (1) modification and test of existing CVD reactor system; (2) identification and/or development of suitable inexpensive substrate materials; (3) experimental investigation of CVD process parameters using various candidate substrate materials; (4) preparation of Si sheet samples for various special studies, including solar cell fabrication; (5) evaluation of the properties of the Si sheet material produced by the CVD process; and (6) fabrication and evaluation of experimental solar cell structures, using standard and near-standard processing techniques.

Synthesis of boron nitride nanostructures from catalyst of iron compounds via thermal chemical vapor deposition technique

NASA Astrophysics Data System (ADS)

da Silva, Wellington M.; Ribeiro, Hélio; Ferreira, Tiago H.; Ladeira, Luiz O.; Sousa, Edésia M. B.

2017-05-01

For the first time, patterned growth of boron nitride nanostructures (BNNs) is achieved by thermal chemical vapor deposition (TCVD) technique at 1150 °C using a mixture of FeS/Fe2O3 catalyst supported in alumina nanostructured, boron amorphous and ammonia (NH3) as reagent gas. This innovative catalyst was synthesized in our laboratory and systematically characterized. The materials were characterized by X-ray diffraction (XRD), Raman spectroscopy, Fourier-transform infrared spectroscopy (FTIR), Thermogravimetric analysis (TGA), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The X-ray diffraction profile of the synthesized catalyst indicates the coexistence of three different crystal structures showing the presence of a cubic structure of iron oxide and iron sulfide besides the gamma alumina (γ) phase. The results show that boron nitride bamboo-like nanotubes (BNNTs) and hexagonal boron nitride (h-BN) nanosheets were successfully synthesized. Furthermore, the important contribution of this work is the manufacture of BNNs from FeS/Fe2O3 mixture.

Chemical vapor deposition of high T(sub c) superconducting films in a microgravity environment

NASA Technical Reports Server (NTRS)

Levy, Moises; Sarma, Bimal K.

1994-01-01

Since the discovery of the YBaCuO bulk materials in 1987, Metalorganic Chemical Vapor Deposition (MOCVD) has been proposed for preparing HTSC high T(sub c) films. This technique is now capable of producing high-T(sub c) superconducting thin films comparable in quality to those prepared by any other methods. The MOCVD technique has demonstrated its superior advantage in making large area high quality HTSC thin films and will play a major role in the advance of device applications of HTSC thin films. The organometallic precursors used in the MOCVD preparation of HTSC oxide thin films are most frequently metal beta-diketonates. High T(sub c) superconductors are multi-component oxides which require more than one component source, with each source, containing one kind of precursor. Because the volatility and stability of the precursors are strongly dependent on temperature, system pressure, and carrier gas flow rate, it has been difficult to control the gas phase composition, and hence film stoichiometry. In order circumvent these problems we have built and tested a single source MOCVD reactor in which a specially designed vaporizer was employed. This vaporizer can be used to volatilize a stoichiometric mixture of diketonates of yttrium, barium and copper to produce a mixed vapor in a 1:2:3 ratio respectively of the organometellics. This is accomplished even though the three compounds have significantly different volatilities. We have developed a model which provides insight into the process of vaporizing mixed precursors to produce high quality thin films of Y1Ba2Cu3O7. It shows that under steady state conditions the mixed organometallic vapor must have a stoichiometric ratio of the individual organometallics identical to that in the solid mixture.

Chemical vapor deposition of W-Si-N and W-B-N

DOEpatents

Fleming, J.G.; Roherty-Osmun, E.L.; Smith, P.M.; Custer, J.S.; Jones, R.V.; Nicolet, M.; Madar, R.; Bernard, C.

1999-06-29

A method of depositing a ternary, refractory based thin film on a substrate by chemical vapor deposition employing precursor sources of tungsten comprising WF[sub 6], either silicon or boron, and nitrogen. The result is a W-Si-N or W-B-N thin film useful for diffusion barrier and micromachining applications. 10 figs.

Improving the chemical stability of amorphous solid dispersion with cocrystal technique by hot melt extrusion.

PubMed

Liu, Xu; Lu, Ming; Guo, Zhefei; Huang, Lin; Feng, Xin; Wu, Chuanbin

2012-03-01

To explore in-situ forming cocrystal as a single-step, efficient method to significantly depress the processing temperature and thus minimize the thermal degradation of heat-sensitive drug in preparation of solid dispersions by melting method (MM) and hot melt extrusion (HME). Carbamazepine (CBZ)-nicotinamide (NIC) cocrystal solid dispersions were prepared with polymer carriers PVP/VA, SOLUPLUS and HPMC by MM and/or HME. The formation of cocrystal was investigated by differential scanning calorimetry and hot stage polarized optical microscopy. State of CBZ in solid dispersion was characterized by X-ray powder diffraction and optical microscopy. Interactions between CBZ, NIC and polymers were investigated by FTIR. Dissolution behaviors of solid dispersions were compared with that of pure CBZ. CBZ-NIC cocrystal with melting point of 160°C was formed in polymer carriers during heating process, and the preparation temperature of amorphous CBZ solid dispersion was therefore depressed to 160°C. The dissolution rate of CBZ-NIC cocrystal solid dispersion was significantly increased. By in-situ forming cocrystal, chemically stable amorphous solid dispersions were prepared by MM and HME at a depressed processing temperature. This method provides an attractive opportunity for HME of heat-sensitive drugs.

Physicochemical characterization of atorvastatin calcium/ezetimibe amorphous nano-solid dispersions prepared by electrospraying method.

PubMed

Jahangiri, Azin; Barzegar-Jalali, Mohammad; Javadzadeh, Yousef; Hamishehkar, Hamed; Adibkia, Khosro

2017-09-01

In the present study, electrospraying was applied as a novel method for the fabrication of amorphous nano-solid dispersions (N-SDs) of atorvastatin calcium (ATV), ezetimibe (EZT), and ATV/EZT combination as poorly water-soluble drugs. N-SDs were prepared using polyvinylpyrrolidone K30 as an amorphous carrier in 1:1 and 1:5 drug to polymer ratios and the total solid (including drug and polymer) concentrations of 10 and 20% (w/v). The prepared formulations were further investigated for their morphological, physicochemical, and dissolution properties. Scanning electron microscopy studies indicated that the morphology and diameter of the electrosprayed samples (ESs) were influenced by the solution concentration and drug:polymer ratio, so that an increase in the solution concentration resulted in fiber formation while an increase in the polymer ratio led to enhancement of the particle diameter. Differential scanning calorimetry and X-ray powder diffraction studies together with in vitro dissolution test revealed that the ESs were present in an amorphous form with improved dissolution properties. Infrared spectroscopic studies showed hydrogen-bonding interaction between the drug and polymer in ESs. Since the electrospraying method benefits from the both amorphization and nanosizing effect, this novel approach seems to be an efficient method for the fabrication of N-SDs of poorly water-soluble drugs.

Room temperature chemical vapor deposition of c-axis ZnO

NASA Astrophysics Data System (ADS)

Barnes, Teresa M.; Leaf, Jacquelyn; Fry, Cassandra; Wolden, Colin A.

2005-02-01

Highly (0 0 2) oriented ZnO films have been deposited at temperatures between 25 and 230 °C by high-vacuum plasma-assisted chemical vapor deposition (HVP-CVD) on glass and silicon substrates. The HVP-CVD process was found to be weakly activated with an apparent activation energy of ∼0.1 eV, allowing room temperature synthesis. Films deposited on both substrates displayed a preferential c-axis texture over the entire temperature range. Films grown on glass demonstrated high optical transparency throughout the visible and near infrared.

Method of chemical vapor deposition of boron nitride using polymeric cyanoborane

DOEpatents

Maya, Leon

1994-01-01

Polymeric cyanoborane is volatilized, decomposed by thermal or microwave plasma energy, and deposited on a substrate as an amorphous film containing boron, nitrogen and carbon. Residual carbon present in the film is removed by ammonia treatment at an increased temperature, producing an adherent, essentially stoichiometric boron nitride film.

Broadband and wide-angle distributed Bragg reflectors based on amorphous germanium films by glancing angle deposition.

PubMed

Leem, Jung Woo; Yu, Jae Su

2012-08-27

We fabricated the distributed Bragg reflectors (DBRs) with amorphous germanium (a-Ge) films consisted of the same materials at a center wavelength (λc) of 1.33 μm by the glancing angle deposition. Their optical reflectance properties were investigated in the infrared wavelength region of 1-1.9 μm at incident light angles (θ inc) of 8-70°, together with the theoretical analysis using a rigorous coupled-wave analysis simulation. The two alternating a-Ge films at the incident vapor flux angles of 0 and 75° were formed as the high and low refractive index materials, respectively. The a-Ge DBR with only 5 periods exhibited a normalized stop bandwidth (∆λ/λ c) of ~24.1%, maintaining high reflectance (R) values of > 99%. Even at a high θ inc of 70°, the ∆λ/λ c was ~21.9%, maintaining R values of > 85%. The a-Ge DBR with good uniformity was obtained over the area of a 2 inch Si wafer. The calculated reflectance results showed a similar tendency to the measured data.

Hierarchical structures of amorphous solids characterized by persistent homology

PubMed Central

Hiraoka, Yasuaki; Nakamura, Takenobu; Hirata, Akihiko; Escolar, Emerson G.; Matsue, Kaname; Nishiura, Yasumasa

2016-01-01

This article proposes a topological method that extracts hierarchical structures of various amorphous solids. The method is based on the persistence diagram (PD), a mathematical tool for capturing shapes of multiscale data. The input to the PDs is given by an atomic configuration and the output is expressed as 2D histograms. Then, specific distributions such as curves and islands in the PDs identify meaningful shape characteristics of the atomic configuration. Although the method can be applied to a wide variety of disordered systems, it is applied here to silica glass, the Lennard-Jones system, and Cu-Zr metallic glass as standard examples of continuous random network and random packing structures. In silica glass, the method classified the atomic rings as short-range and medium-range orders and unveiled hierarchical ring structures among them. These detailed geometric characterizations clarified a real space origin of the first sharp diffraction peak and also indicated that PDs contain information on elastic response. Even in the Lennard-Jones system and Cu-Zr metallic glass, the hierarchical structures in the atomic configurations were derived in a similar way using PDs, although the glass structures and properties substantially differ from silica glass. These results suggest that the PDs provide a unified method that extracts greater depth of geometric information in amorphous solids than conventional methods. PMID:27298351

Chemical vapor deposition of yttria-stabilized zirconia as a thermal barrier coating for gas turbine engines

NASA Astrophysics Data System (ADS)

Varanasi, Venu Gopal

The gas turbine engine uses an yttria-stabilized zirconia (YSZ) coating to provide thermal insulation for its turbine blades. This YSZ coating must be tetragonal in crystal structure, columnar in microstructure, and be 100--250 mum thick to provide for adequate protection for the turbine blades in the severe engine environment. Currently, YSZ coatings are fabricated by electron-beam physical vapor deposition (EB-PVD), but this fabrication method is cost intensive. Chemical vapor deposition (CVD) is a more commercially viable processing method and a possible alternative to EB-PVD. The deposition of tetragonal YSZ from gaseous metal and oxidation sources were studied. A chemical equilibrium analysis modeled the feasibility of depositing tetragonal YSZ for both chloride CVD (Zr-Y-C-O-Cl-H-Inert system) and metal-organic CVD (MOCVD) (Zr-Y-C-O-H system). Pure thermochemical properties and the assessed YSZ phase diagram were used in this analysis. Using the molar input of metals ((nY + nZr) and ( nY/(nY + nZr ) = 0.08)) as bases, equilibrium calculations showed that tetragonal YSZ formation was feasible. Tetragonal YSZ formation was feasible with high oxygen content (nO/(nY + nZr) > 8) and high temperature (T > 100°C) in the case of chloride CVD (Zr-Y-C-O-Cl-H-Inert). Tetragonal YSZ formation was feasible with high oxygen content (nO/( nY + nZr) > 5) and high temperature (T > 950°C) in the case of MOCVD (Zr-Y-C-O-H). Although solid carbon formation did not appear in chloride CVD, additional oxygen (nO/( nY + nZr) > 32) and low hydrogen content relative to carbon (nH/nC < 2) were required to avoid solid carbon formation in MOCVD. Coatings were deposited using a set of base conditions derived from the chemical equilibrium analysis. In chloride CVD, YCl3 was not included because of its low vapor pressure, thus, ZrCl4 was oxidized with the H2-CO2 gas mixture. Monoclinic ZrO2 coatings were deposited at the thermochemically optimized conditions (n O/(nY + nZr) > 8, T > 1004�

High growth rate homoepitaxial diamond film deposition at high temperatures by microwave plasma-assisted chemical vapor deposition

NASA Technical Reports Server (NTRS)

Vohra, Yogesh K. (Inventor); McCauley, Thomas S. (Inventor)

1997-01-01

The deposition of high quality diamond films at high linear growth rates and substrate temperatures for microwave-plasma chemical vapor deposition is disclosed. The linear growth rate achieved for this process is generally greater than 50 .mu.m/hr for high quality films, as compared to rates of less than 5 .mu.m/hr generally reported for MPCVD processes.

Method of chemical vapor deposition of boron nitride using polymeric cyanoborane

DOEpatents

Maya, L.

1994-06-14

Polymeric cyanoborane is volatilized, decomposed by thermal or microwave plasma energy, and deposited on a substrate as an amorphous film containing boron, nitrogen and carbon. Residual carbon present in the film is removed by ammonia treatment at an increased temperature, producing an adherent, essentially stoichiometric boron nitride film. 11 figs.

Analysis of the pyrolysis products of dimethyldichlorosilane in the chemical vapor deposition of silicon carbide in argon

NASA Technical Reports Server (NTRS)

Cagliostro, Domenick E.; Riccitiello, Salvatore R.; Carswell, Marty G.

1990-01-01

A study of the products and reactions occurring during the chemical vapor deposition of silicon carbide from dimethyldichlorosilane in argon is presented. Reaction conditions were as follows: 700 to 1100 C, a contact time of about 1 min, and a pressure of 1 atm. At these conditions, the gases that formed were mainly methane, hydrogen, silicon tetrachloride, trichlorosilane, and methyltrichlorosilane. The silicon carbide solid that formed showed the presence of hydrogen and chloride as impurities, which might degrade the silicon carbide properties. These impurities were eliminated slowly, even at 1100 C, forming hydrogen, trichlorosilane, and silicon tetrachloride.

Towards a uniform and large-scale deposition of MoS2 nanosheets via sulfurization of ultra-thin Mo-based solid films.

PubMed

Vangelista, Silvia; Cinquanta, Eugenio; Martella, Christian; Alia, Mario; Longo, Massimo; Lamperti, Alessio; Mantovan, Roberto; Basset, Francesco Basso; Pezzoli, Fabio; Molle, Alessandro

2016-04-29

Large-scale integration of MoS2 in electronic devices requires the development of reliable and cost-effective deposition processes, leading to uniform MoS2 layers on a wafer scale. Here we report on the detailed study of the heterogeneous vapor-solid reaction between a pre-deposited molybdenum solid film and sulfur vapor, thus resulting in a controlled growth of MoS2 films onto SiO2/Si substrates with a tunable thickness and cm(2)-scale uniformity. Based on Raman spectroscopy and photoluminescence, we show that the degree of crystallinity in the MoS2 layers is dictated by the deposition temperature and thickness. In particular, the MoS2 structural disorder observed at low temperature (<750 °C) and low thickness (two layers) evolves to a more ordered crystalline structure at high temperature (1000 °C) and high thickness (four layers). From an atomic force microscopy investigation prior to and after sulfurization, this parametrical dependence is associated with the inherent granularity of the MoS2 nanosheet that is inherited by the pristine morphology of the pre-deposited Mo film. This work paves the way to a closer control of the synthesis of wafer-scale and atomically thin MoS2, potentially extendable to other transition metal dichalcogenides and hence targeting massive and high-volume production for electronic device manufacturing.

New Density Functional Approach for Solid-Liquid-Vapor Transitions in Pure Materials

NASA Astrophysics Data System (ADS)

Kocher, Gabriel; Provatas, Nikolas

2015-04-01

A new phase field crystal (PFC) type theory is presented, which accounts for the full spectrum of solid-liquid-vapor phase transitions within the framework of a single density order parameter. Its equilibrium properties show the most quantitative features to date in PFC modeling of pure substances, and full consistency with thermodynamics in pressure-volume-temperature space is demonstrated. A method to control either the volume or the pressure of the system is also introduced. Nonequilibrium simulations show that 2- and 3-phase growth of solid, vapor, and liquid can be achieved, while our formalism also allows for a full range of pressure-induced transformations. This model opens up a new window for the study of pressure driven interactions of condensed phases with vapor, an experimentally relevant paradigm previously missing from phase field crystal theories.

Continuous growth of single-wall carbon nanotubes using chemical vapor deposition

DOEpatents

Grigorian, Leonid [Raymond, OH; Hornyak, Louis [Evergreen, CO; Dillon, Anne C [Boulder, CO; Heben, Michael J [Denver, CO

2008-10-07

The invention relates to a chemical vapor deposition process for the continuous growth of a carbon single-wall nanotube where a carbon-containing gas composition is contacted with a porous membrane and decomposed in the presence of a catalyst to grow single-wall carbon nanotube material. A pressure differential exists across the porous membrane such that the pressure on one side of the membrane is less than that on the other side of the membrane. The single-wall carbon nanotube growth may occur predominately on the low-pressure side of the membrane or, in a different embodiment of the invention, may occur predominately in between the catalyst and the membrane. The invention also relates to an apparatus used with the carbon vapor deposition process.

Development of Nb{sub 3}Sn Cavity Vapor Diffusion Deposition System

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

Eremeev, Grigory V.; Macha, Kurt M.; Clemens, William A.

2014-02-01

Nb{sub 3}Sn is a BCS superconductors with the superconducting critical temperature higher than that of niobium, so theoretically it surpasses the limitations of niobium in RF fields. The feasibility of technology has been demonstrated at 1.5 GHz with Nb{sub 3}Sn vapor deposition technique at Wuppertal University. The benefit at these frequencies is more pronounced at 4.2 K, where Nb{sub 3}Sn coated cavities show RF resistances an order of magnitude lower than that of niobium. At Jefferson Lab we started the development of Nb{sub 3}Sn vapor diffusion deposition system within an R\\&D development program towards compact light sources. Here we presentmore » the current progress of the system development.« less

Continuous growth of single-wall carbon nanotubes using chemical vapor deposition

DOEpatents

Grigorian, Leonid; Hornyak, Louis; Dillon, Anne C; Heben, Michael J

2014-09-23

The invention relates to a chemical vapor deposition process for the continuous growth of a carbon single-wall nanotube where a carbon-containing gas composition is contacted with a porous membrane and decomposed in the presence of a catalyst to grow single-wall carbon nanotube material. A pressure differential exists across the porous membrane such that the pressure on one side of the membrane is less than that on the other side of the membrane. The single-wall carbon nanotube growth may occur predominately on the low-pressure side of the membrane or, in a different embodiment of the invention, may occur predominately in between the catalyst and the membrane. The invention also relates to an apparatus used with the carbon vapor deposition process.

Impact of surfactants on the crystallization of aqueous suspensions of celecoxib amorphous solid dispersion spray dried particles.

PubMed

Chen, Jie; Ormes, James D; Higgins, John D; Taylor, Lynne S

2015-02-02

Amorphous solid dispersions are frequently prepared by spray drying. It is important that the resultant spray dried particles do not crystallize during formulation, storage, and upon administration. The goal of the current study was to evaluate the impact of surfactants on the crystallization of celecoxib amorphous solid dispersions (ASD), suspended in aqueous media. Solid dispersions of celecoxib with hydroxypropylmethylcellulose acetate succinate were manufactured by spray drying, and aqueous suspensions were prepared by adding the particles to acidified media containing various surfactants. Nucleation induction times were evaluated for celecoxib in the presence and absence of surfactants. The impact of the surfactants on drug and polymer leaching from the solid dispersion particles was also evaluated. Sodium dodecyl sulfate and Polysorbate 80 were found to promote crystallization from the ASD suspensions, while other surfactants including sodium taurocholate and Triton X100 were found to inhibit crystallization. The promotion or inhibition of crystallization was found to be related to the impact of the surfactant on the nucleation behavior of celecoxib, as well as the tendency to promote leaching of the drug from the ASD particle into the suspending medium. It was concluded that surfactant choice is critical to avoid failure of amorphous solid dispersions through crystallization of the drug.

Formation of soft magnetic high entropy amorphous alloys composites containing in situ solid solution phase

NASA Astrophysics Data System (ADS)

Wei, Ran; Sun, Huan; Chen, Chen; Tao, Juan; Li, Fushan

2018-03-01

Fe-Co-Ni-Si-B high entropy amorphous alloys composites (HEAACs), which containing high entropy solid solution phase in amorphous matrix, show good soft magnetic properties and bending ductility even in optimal annealed state, were successfully developed by melt spinning method. The crystallization phase of the HEAACs is solid solution phase with body centered cubic (BCC) structure instead of brittle intermetallic phase. In addition, the BCC phase can transformed into face centered cubic (FCC) phase with temperature rise. Accordingly, Fe-Co-Ni-Si-B high entropy alloys (HEAs) with FCC structure and a small amount of BCC phase was prepared by copper mold casting method. The HEAs exhibit high yield strength (about 1200 MPa) and good plastic strain (about 18%). Meanwhile, soft magnetic characteristics of the HEAs are largely reserved from HEAACs. This work provides a new strategy to overcome the annealing induced brittleness of amorphous alloys and design new advanced materials with excellent comprehensive properties.

High-Density Amorphous Ice, the Frost on Interstellar Grains

NASA Technical Reports Server (NTRS)

Jenniskens, P.; Blake, D. F.; Wilson, M. A.; Pohorille, A.

1995-01-01

Most water ice in the universe is in a form which does not occur naturally on Earth and of which only minimal amounts have been made in the laboratory. We have encountered this 'high-density amorphous ice' in electron diffraction experiments of low-temperature (T less than 30 K) vapor-deposited water and have subsequently modeled its structure using molecular dynamics simulations. The characteristic feature of high-density amorphous ice is the presence of 'interstitial' oxygen pair distances between 3 and 4 A. However, we find that the structure is best described as a collapsed lattice of the more familiar low-density amorphous form. These distortions are frozen in at temperatures below 38 K because, we propose, it requires the breaking of one hydrogen bond, on average, per molecule to relieve the strain and to restructure the lattice to that of low-density amorphous ice. Several features of astrophysical ice analogs studied in laboratory experiments are readily explained by the structural transition from high-density amorphous ice into low-density amorphous ice. Changes in the shape of the 3.07 gm water band, trapping efficiency of CO, CO loss, changes in the CO band structure, and the recombination of radicals induced by low-temperature UV photolysis all covary with structural changes that occur in the ice during this amorphous to amorphous transition. While the 3.07 micrometers ice band in various astronomical environments can be modeled with spectra of simple mixtures of amorphous and crystalline forms, the contribution of the high-density amorphous form nearly always dominates.

Differential AC chip calorimeter for in situ investigation of vapor deposited thin films

NASA Astrophysics Data System (ADS)

Ahrenberg, Mathias; Schick, Christoph; Huth, Heiko; Schoifet, Evgeni; Ediger, Mark; Whitaker, Katie

2012-02-01

Physical vapor deposition (PVD) can be used to produce thin films with particular material properties like extraordinarily stable glasses of organic molecules. We describe an AC chip calorimeter for in-situ heat capacity measurements of as-deposited nanometer thin films of organic glass formers. The calorimetric system is based on a differential AC chip calorimeter which is placed in the vacuum chamber for physical vapor deposition. The sample is directly deposited onto one calorimetric chip sensor while the other sensor is protected against deposition. The device and the temperature calibration procedure are described. The latter makes use of the phase transitions of cyclopentane and the frequency dependence of the dynamic glass transition of toluene and ethylbenzene. Sample thickness determination is based on a finite element modeling (FEM) of the sensor sample arrangement. A layer of toluene was added to the sample sensor and its thickness was varied in an iterative way until the model fits the experimental data.

Effects of Deposition Parameters on Thin Film Properties of Silicon-Based Electronic Materials Deposited by Remote Plasma-Enhanced Chemical-Vapor Deposition

NASA Astrophysics Data System (ADS)

Theil, Jeremy Alfred

The motivation of this thesis is to discuss the major issues of remote plasma enhanced chemical vapor deposition (remote PECVD) that affect the properties Si-based thin films. In order to define the issues required for process optimization, the behavior of remote PECVD process must be understood. The remote PECVD process is defined as having four segments: (1) plasma generation, (2) excited species extraction, (3) excited species/downstream gas mixing, and (4) surface reaction. The double Langmuir probe technique is employed to examine plasma parameters under 13.56 MHz and 2.54 GHz excitation. Optical emission spectroscopy is used to determine changes in the excited states of radiating species in the plasma afterglow. Mass spectrometry is used to determine the excitation and consumption of process gases within the reactor during film growth. Various analytical techniques such as infrared absorption spectroscopy, (ir), high resolution transmission electron microscopy, (HRTEM), and reflected high energy electron diffraction, (RHEED), are used to ascertain film properties. The results of the Langmuir probe show that plasma coupling is frequency dependent and that the capacitive coupling mode is characterized by orders of magnitude higher electron densities in the reactor than inductive coupling. These differences can be manifested in the degree to which a hydrogenated amorphous silicon, a-Si:H, component co-deposition reaction affects film stoichiometry. Mass spectrometry shows that there is an additional excitation source in the downstream glow. In addition the growth of microcrystalline silicon, muc-Si, is correlated with the decrease in the production of disilane and heavier Si-containing species. Chloronium, H_2 Cl^{+}, a super acid ion is identified for the first time in a CVD reactor. It forms from plasma fragmentation of SiH_2 Cl_2, and H_2 . Addition of impurity gases was shown not to affect the electron temperature of the plasma. By products of deposition

Raman spectra boron doped amorphous carbon thin film deposited by bias assisted-CVD

NASA Astrophysics Data System (ADS)

Ishak, A.; Fadzilah, A. N.; Dayana, K.; Saurdi, I.; Malek, M. F.; Nurbaya, Z.; Shafura, A. K.; Rusop, M.

2018-05-01

Boron doped amorphous carbon thin film carbon was deposited at 200°C-350°C by bias assisted-CVD using palm oil as a precursor material. The structural boron doped amorphous carbon films were discussed by Raman analysis through the evolution of D and G bands. The spectral evolution observed showed the increase of upward shift of D and G peaks as substrate deposition temperatures increased. These structural changes were further correlated with optical gap and the results obtained are discussed and compared. The estimated optical band gap is found to be 1.9 to 2.05 eV and conductivity is to be in the range of 10-5 Scm-1 to 10-4 Scm-1. The decrease of optical band gap is associated to conductivity increased which change the characteristic parameters of Raman spectra including the position of G peak, full width at half maximum of G peak, and ID/IG.

Structural and electrical characterization of microcrystalline silicon films prepared by a layer-by-layer technique with a plasma-enhanced chemical-vapor deposition system

NASA Astrophysics Data System (ADS)

Hong, J. P.; Kim, C. O.; Nahm, T. U.; Kim, C. M.

2000-02-01

Microcrystalline silicon films have been prepared on indium-coated glass utilizing a layer-by-layer technique with a plasma-enhanced chemical-vapor deposition system. The microcrystalline films were fabricated by varying the number of cycles from 10 to 60 under a fixed H2 time (t2) of 120 s, where the corresponding deposition time (t1) of amorphous silicon thin film was 60 s. Structural properties, such as the crystalline volume fraction (Xc) and grain sizes were analyzed by using Raman spectroscopy and a scanning electron microscopy. The carrier transport was characterized by the temperature dependence of dark conductivity, giving rise to the calculation of activation energy (Ea). Optical energy gaps (Eg) were also investigated using an ultraviolet spectrophotometer. In addition, the process under different hydrogen plasma time (t2) at a fixed number of 20 cycles was extensively carried out to study the dominant role of hydrogen atoms in layer-by-layer deposition. Finally, the correlation between structural and electrical properties has been discussed on the basis of experimental results.

Deuterium permeation of amorphous alumina coating on 316L prepared by MOCVD

NASA Astrophysics Data System (ADS)

Li, Shuai; He, Di; Liu, Xiaopeng; Wang, Shumao; Jiang, Lijun

2012-01-01

The deuterium permeation behavior of the alumina coating on 316L stainless steel prepared by metal organic chemical vapor deposition (MOCVD) was investigated. The alumina coating was also characterized by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and scanning electron microscope (SEM). It was found that the as-prepared coating consisted of amorphous alumina. This alumina coating had a dense, crack-free and homogeneous morphology. Although the alumina coating was amorphous, effective suppression of deuterium permeation was demonstrated. The deuterium permeability of the alumina coating was 51-60 times less than that of the 316L stainless steel and 153-335 times less than that of the referred low activation martensitic steels at 860-960 K.

Magnetism of Amorphous and Nano-Crystallized Dc-Sputter-Deposited MgO Thin Films

PubMed Central

Mahadeva, Sreekanth K.; Fan, Jincheng; Biswas, Anis; Sreelatha, K.S.; Belova, Lyubov; Rao, K.V.

2013-01-01

We report a systematic study of room-temperature ferromagnetism (RTFM) in pristine MgO thin films in their amorphous and nano-crystalline states. The as deposited dc-sputtered films of pristine MgO on Si substrates using a metallic Mg target in an O2 containing working gas atmosphere of (N2 + O2) are found to be X-ray amorphous. All these films obtained with oxygen partial pressure (PO2) ~10% to 80% while maintaining the same total pressure of the working gas are found to be ferromagnetic at room temperature. The room temperature saturation magnetization (MS) value of 2.68 emu/cm3 obtained for the MgO film deposited in PO2 of 10% increases to 9.62 emu/cm3 for film deposited at PO2 of 40%. However, the MS values decrease steadily for further increase of oxygen partial pressure during deposition. On thermal annealing at temperatures in the range 600 to 800 °C, the films become nanocrystalline and as the crystallite size grows with longer annealing times and higher temperature, MS decreases. Our study clearly points out that it is possible to tailor the magnetic properties of thin films of MgO. The room temperature ferromagnetism in MgO films is attributed to the presence of Mg cation vacancies. PMID:28348346

Ultrathin NiGe films prepared via catalytic solid-vapor reaction of Ni with GeH(4).

PubMed

Peter, Antony P; Opsomer, Karl; Adelmann, Christoph; Schaekers, Marc; Meersschaut, Johan; Richard, Olivier; Vaesen, Inge; Moussa, Alain; Franquet, Alexis; Zsolt, Tokei; Van Elshocht, Sven

2013-10-09

A low-temperature (225-300 °C) solid-vapor reaction process is reported for the synthesis of ultrathin NiGe films (∼6-23 nm) on 300 mm Si wafers covered with thermal oxide. The films were prepared via catalytic chemical vapor reaction of germane (GeH4) gas with physical vapor deposited (PVD) Ni films of different thickness (2-10 nm). The process optimization by investigating GeH4 partial pressure, reaction temperature, and time shows that low resistive, stoichiometric, and phase pure NiGe films can be formed within a broad window. NiGe films crystallized in an orthorhombic structure and were found to exhibit a smooth morphology with homogeneous composition as evidenced by glancing angle X-ray diffraction (GIXRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), and Rutherford back-scattering (RBS) analysis. Transmission electron microscopy (TEM) analysis shows that the NiGe layers exhibit a good adhesion without voids and a sharp interface on the thermal oxide. The NiGe films were found to be morphologically and structurally stable up to 500 °C and exhibit a resistivity value of 29 μΩ cm for 10 nm NiGe films.

Metal Organic Chemical Vapor Deposition of Oxide Films for Advanced Applications

DTIC Science & Technology

2000-06-01

coatings , photovoltaics, touch sensitive controls, electromagnetic shielding (as found on microwave ovens and stealth fighters), static dissipaters, and so...depositing high quality films. The methods are physical vapor deposition ( PVD ), spin/mist deposition, (CVD), and alternating layer (AL) CVD. PVD ...PZT & SBT, YBa2Cu3O, CeO, InO, TCOs, Varistors Ta2O5 , ZrO, MnO, HfO, CeO, MnO, MgO SAW/microwave Silicon/: Si, SiGe, SiGeC, �. Opto-electronics

Oxidation of Chemically-Vapor-Deposited Silicon Carbide in Carbon Dioxide

NASA Technical Reports Server (NTRS)

Opila, Elizabeth J.; Nguyen, QuynhGiao N.

1998-01-01

Chemically-vapor-deposited silicon carbide (CVD SiC) was oxidized in carbon dioxide (CO2) at temperatures of 1200-1400 C for times between 96 and 500 h at several gas flow rates. Oxidation weight gains were monitored by thermogravimetric analysis (TGA) and were found to be very small and independent of temperature. Possible rate limiting kinetic mechanisms are discussed. Passive oxidation of SiC by CO2 is negligible compared to the rates measured for other oxidants that are also found in combustion environments, oxygen and water vapor.

Bimetallic-catalyst-mediated syntheses of nanomaterials (nanowires, nanotubes, nanofibers, nanodots, etc) by the VQS (vapor-quasiliquid-solid, vapor- quasisolid-solid) growth mechanism

NASA Astrophysics Data System (ADS)

Mohammad, S. N.

2016-12-01

The enhanced synergistic, catalytic effect of bimetallic nanoparticles (BNPs), as compared to monometallic nanoparticles (NPs), on the nanomaterials (nanowires, nanotubes, nanodots, nanofibers, etc) synthesed by chemical vapor deposition has been investigated. A theoretical model for this catalytic effect and hence for nanomaterial growth, has been developed. The key element of the model is the diffusion of the nanomaterial source species through the nanopores of quasiliquid (quasisolid) BNP, rather than through the liquid or solid BNP, for nanomaterial growth. The role of growth parameters such as temperature, pressure and of the BNP material characteristics such as element mole fraction of BNP, has been studied. The cause of enhanced catalytic activity of BNPs as compared to NPs as a function of temperature has been explored. The dependence of growth rate on the nanomaterial diameter has also been examined. The calculated results have been extensively compared with available experiments. Experimental supports for the growth mechanism have been presented as well. Close correspondence between the calculated and experimental results attests to the validity of the proposed model. The wide applicability of the proposed model to nanowires, nanotubes, nanofibers, nanodots, etc suggests that it is general and has broad appeal.

Criticality in the Approach to Failure in Amorphous Solids

NASA Astrophysics Data System (ADS)

Lin, Jie; Gueudré, Thomas; Rosso, Alberto; Wyart, Matthieu

2015-10-01

Failure of amorphous solids is fundamental to various phenomena, including landslides and earthquakes. Recent experiments indicate that highly plastic regions form elongated structures that are especially apparent near the maximal shear stress Σmax where failure occurs. This observation suggested that Σmax acts as a critical point where the length scale of those structures diverges, possibly causing macroscopic transient shear bands. Here, we argue instead that the entire solid phase (Σ <Σmax) is critical, that plasticity always involves system-spanning events, and that their magnitude diverges at Σmax independently of the presence of shear bands. We relate the statistics and fractal properties of these rearrangements to an exponent θ that captures the stability of the material, which is observed to vary continuously with stress, and we confirm our predictions in elastoplastic models.

Density change and viscous flow during structural relaxation of plasma-enhanced chemical-vapor-deposited silicon oxide films

NASA Astrophysics Data System (ADS)

Cao, Zhiqiang; Zhang, Xin

2004-10-01

The structural relaxation of plasma-enhanced chemical-vapor-deposited (PECVD) silane-based silicon oxide films during thermal cycling and annealing has been studied using wafer curvature measurements. These measurements, which determine stress in the amorphous silicon oxide films, are sensitive to both plastic deformation and density changes. A quantitative case study of such changes has been done based upon the experimental results. A microstructure-based mechanism elucidates seams as a source of density change and voids as a source of plastic deformation, accompanied by a viscous flow. This theory was then used to explain a series of experimental results that are related to thermal cycling as well as annealing of PECVD silicon oxide films including stress hysteresis generation and reduction and coefficient of thermal-expansion changes. In particular, the thickness effect was examined; PECVD silicon oxide films with a thickness varying from 1to40μm were studied, as certain demanding applications in microelectromechanical systems require such thick films serving as heat/electrical insulation layers.

Ion beam deposition of amorphous carbon films with diamond like properties

NASA Technical Reports Server (NTRS)

Angus, John C.; Mirtich, Michael J.; Wintucky, Edwin G.

1982-01-01

Carbon films were deposited on silicon, quartz, and potassium bromide substrates from an ion beam. Growth rates were approximately 0.3 micron/hour. The films were featureless and amorphous and contained only carbon and hydrogen in significant amounts. The density and carbon/hydrogen ratio indicate the film is a hydrogen deficient polymer. One possible structure, consistent with the data, is a random network of methylene linkages and tetrahedrally coordinated carbon atoms.

Atomic layer deposition of ultrathin blocking layer for low-temperature solid oxide fuel cell on nanoporous substrate

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

Yu, Wonjong; Cho, Gu Young; Noh, Seungtak

2015-01-15

An ultrathin yttria-stabilized zirconia (YSZ) blocking layer deposited by atomic layer deposition (ALD) was utilized for improving the performance and reliability of low-temperature solid oxide fuel cells (SOFCs) supported by an anodic aluminum oxide substrate. Physical vapor-deposited YSZ and gadolinia-doped ceria (GDC) electrolyte layers were deposited by a sputtering method. The ultrathin ALD YSZ blocking layer was inserted between the YSZ and GDC sputtered layers. To investigate the effects of an inserted ultrathin ALD blocking layer, SOFCs with and without an ultrathin ALD blocking layer were electrochemically characterized. The open circuit voltage (1.14 V) of the ALD blocking-layered SOFC was visiblymore » higher than that (1.05 V) of the other cell. Furthermore, the ALD blocking layer augmented the power density and improved the reproducibility.« less

Water–solid interactions in amorphous maltodextrin-crystalline sucrose binary mixtures

PubMed Central

Ghorab, Mohamed K.; Toth, Scott J.; Simpson, Garth J.; Mauer, Lisa J.; Taylor, Lynne S.

2016-01-01

Amorphous and crystalline solids are commonly found together in a variety of pharmaceutical and food products. In this study, the influence of co-formulation of amorphous maltodextrins (MDs) and crystalline sucrose (S) on moisture sorption, deliquescence, and glass transition (Tg) properties of powder blends was investigated. Individual components and binary mixtures of four different molecular weight MDs with sucrose in 1:1 w/w ratios were exposed to various relative humidity (RH) environments and their equilibrium and dynamic moisture contents were monitored. The deliquescence point (RH0) and dissolution behavior of sucrose alone and in blends was also monitored by polarized light microscopy and second harmonic generation imaging. In S:MD blends, the deliquescence RH of sucrose was lower than the RH0 of sucrose alone, and synergistic moisture sorption also occurred at RHs lower than the RH0. Intimate contact of sucrose crystals with the amorphous MDs resulted in complete dissolution of sucrose at RH < RH0. When blends were stored at conditions exceeding the Tg of the individual MDs (25 °C and 60%, 49% and 34%RH for MD21, MD29 and MD40, respectively), the Tg of the blends was lower than that of individual MDs. Thus, co-formulation of amorphous MDs with crystalline sucrose sensitizes the blend to moisture, potentially leading to deleterious changes in the formulation if storage conditions are not adequately controlled. PMID:23477494

Growth of diamond by RF plasma-assisted chemical vapor deposition

NASA Technical Reports Server (NTRS)

Meyer, Duane E.; Ianno, Natale J.; Woollam, John A.; Swartzlander, A. B.; Nelson, A. J.

1988-01-01

A system has been designed and constructed to produce diamond particles by inductively coupled radio-frequency, plasma-assisted chemical vapor deposition. This is a low-pressure, low-temperature process used in an attempt to deposit diamond on substrates of glass, quartz, silicon, nickel, and boron nitride. Several deposition parameters have been varied including substrate temperature, gas concentration, gas pressure, total gas flow rate, RF input power, and deposition time. Analytical methods employed to determine composition and structure of the deposits include scanning electron microscopy, absorption spectroscopy, scanning Auger microprobe spectroscopy, and Raman spectroscopy. Analysis indicates that particles having a thin graphite surface, as well as diamond particles with no surface coatings, have been deposited. Deposits on quartz have exhibited optical bandgaps as high as 4.5 eV. Scanning electron microscopy analysis shows that particles are deposited on a pedestal which Auger spectroscopy indicates to be graphite. This is a phenomenon that has not been previously reported in the literature.

Chemical vapor deposition growth

NASA Technical Reports Server (NTRS)

Ruth, R. P.; Manasevit, H. M.; Campbell, A. G.; Johnson, R. E.; Kenty, J. L.; Moudy, L. A.; Shaw, G. L.; Simpson, W. I.; Yang, J. J.

1978-01-01

The objective was to investigate and develop chemical vapor deposition (CVD) techniques for the growth of large areas of Si sheet on inexpensive substrate materials, with resulting sheet properties suitable for fabricating solar cells that would meet the technical goals of the Low Cost Silicon Solar Array Project. The program involved six main technical tasks: (1) modification and test of an existing vertical-chamber CVD reactor system; (2) identification and/or development of suitable inexpensive substrate materials; (3) experimental investigation of CVD process parameters using various candidate substrate materials; (4) preparation of Si sheet samples for various special studies, including solar cell fabrication; (5) evaluation of the properties of the Si sheet material produced by the CVD process; and (6) fabrication and evaluation of experimental solar cell structures, using impurity diffusion and other standard and near-standard processing techniques supplemented late in the program by the in situ CVD growth of n(+)/p/p(+) sheet structures subsequently processed into experimental cells.

Texture related unusual phenomena in electrodeposition and vapor deposition

NASA Astrophysics Data System (ADS)

Lee, D. N.; Han, H. N.

2015-04-01

The tensile strength of electrodeposits generally decreases with increasing bath temperature because the grain size increases and the dislocation density decreases with increasing bath temperature. Therefore, discontinuities observed in the tensile strength vs. bath temperature curves in electrodeposition of copper are unusual. The tensile strength of electrodeposits generally increases with increasing cathode current density because the rate of nucleation in electrodeposits increases with increasing current density, which in turn gives rise to a decrease in the grain size and in turn an increase in the strength. Therefore, a decrease in the tensile strength of copper electrodeposits at a high current density is unusual. The grain size of vapor deposits is expected to decrease with decreasing substrate temperature. However, rf sputtered Co-Cr deposits showed that deposits formed on water-cooled polyimide substrates had a larger grain size than deposits formed on polyimide substrates at 200 °C. These unusual phenomena can be explained by the preferred growth model for deposition texture evolution.

The silane depletion fraction as an indicator for the amorphous/crystalline silicon interface passivation quality

NASA Astrophysics Data System (ADS)

Descoeudres, A.; Barraud, L.; Bartlome, R.; Choong, G.; De Wolf, Stefaan; Zicarelli, F.; Ballif, C.

2010-11-01

In silicon heterojunction solar cells, thin amorphous silicon layers passivate the crystalline silicon wafer surfaces. By using in situ diagnostics during plasma-enhanced chemical vapor deposition (PECVD), the authors report how the passivation quality of such layers directly relate to the plasma conditions. Good interface passivation is obtained from highly depleted silane plasmas. Based upon this finding, layers deposited in a large-area very high frequency (40.68 MHz) PECVD reactor were optimized for heterojunction solar cells, yielding aperture efficiencies up to 20.3% on 4 cm2 cells.

CMAS Interactions with Advanced Environmental Barrier Coatings Deposited via Plasma Spray- Physical Vapor Deposition

NASA Technical Reports Server (NTRS)

Harder, B. J.; Wiesner, V. L.; Zhu, D.; Johnson, N. S.

2017-01-01

Materials for advanced turbine engines are expected to have temperature capabilities in the range of 1370-1500C. At these temperatures the ingestion of sand and dust particulate can result in the formation of corrosive glass deposits referred to as CMAS. The presence of this glass can both thermomechanically and thermochemically significantly degrade protective coatings on metallic and ceramic components. Plasma Spray- Physical Vapor Deposition (PS-PVD) was used to deposit advanced environmental barrier coating (EBC) systems for investigation on their interaction with CMAS compositions. Coatings were exposed to CMAS and furnace tested in air from 1 to 50 hours at temperatures ranging from 1200-1500C. Coating composition and crystal structure were tracked with X-ray diffraction and microstructure with electron microscopy.

Chemical vapor deposition modeling: An assessment of current status

NASA Technical Reports Server (NTRS)

Gokoglu, Suleyman A.

1991-01-01

The shortcomings of earlier approaches that assumed thermochemical equilibrium and used chemical vapor deposition (CVD) phase diagrams are pointed out. Significant advancements in predictive capabilities due to recent computational developments, especially those for deposition rates controlled by gas phase mass transport, are demonstrated. The importance of using the proper boundary conditions is stressed, and the availability and reliability of gas phase and surface chemical kinetic information are emphasized as the most limiting factors. Future directions for CVD are proposed on the basis of current needs for efficient and effective progress in CVD process design and optimization.

The photoexcitation of crystalline ice and amorphous solid water: A molecular dynamics study of outcomes at 11 K and 125 K

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

Crouse, J.; Loock, H.-P., E-mail: hploock@chem.queensu.ca; Cann, N. M., E-mail: ncann@chem.queensu.ca

2015-07-21

Photoexcitation of crystalline ice Ih and amorphous solid water at 7-9 eV is examined using molecular dynamics simulations and a fully flexible water model. The probabilities of photofragment desorption, trapping, and recombination are examined for crystalline ice at 11 K and at 125 K and for amorphous solid water at 11 K. For 11 K crystalline ice, a fully rigid water model is also employed for comparison. The kinetic energy of desorbed H atoms and the distance travelled by trapped fragments are correlated to the location and the local environment of the photoexcited water molecule. In all cases, H atommore » desorption is found to be the most likely outcome in the top bilayer while trapping of all photofragments is most probable deeper in the solid where the likelihood for recombination of the fragments into H{sub 2}O molecules also rises. Trajectory analysis indicates that the local hydrogen bonding network in amorphous solid water is more easily distorted by a photodissociation event compared to crystalline ice. Also, simulations indicate that desorption of OH radicals and H{sub 2}O molecules are more probable in amorphous solid water. The kinetic energy distributions for desorbed H atoms show a peak at high energy in crystalline ice, arising from photoexcited water molecules in the top monolayer. This peak is less pronounced in amorphous solid water. H atoms that are trapped may be displaced by up to ∼10 water cages, but migrate on average 3 water cages. Trapped OH fragments tend to stay near the original solvent cage.« less

The photoexcitation of crystalline ice and amorphous solid water: A molecular dynamics study of outcomes at 11 K and 125 K.

PubMed

Crouse, J; Loock, H-P; Cann, N M

2015-07-21

Photoexcitation of crystalline ice Ih and amorphous solid water at 7-9 eV is examined using molecular dynamics simulations and a fully flexible water model. The probabilities of photofragment desorption, trapping, and recombination are examined for crystalline ice at 11 K and at 125 K and for amorphous solid water at 11 K. For 11 K crystalline ice, a fully rigid water model is also employed for comparison. The kinetic energy of desorbed H atoms and the distance travelled by trapped fragments are correlated to the location and the local environment of the photoexcited water molecule. In all cases, H atom desorption is found to be the most likely outcome in the top bilayer while trapping of all photofragments is most probable deeper in the solid where the likelihood for recombination of the fragments into H2O molecules also rises. Trajectory analysis indicates that the local hydrogen bonding network in amorphous solid water is more easily distorted by a photodissociation event compared to crystalline ice. Also, simulations indicate that desorption of OH radicals and H2O molecules are more probable in amorphous solid water. The kinetic energy distributions for desorbed H atoms show a peak at high energy in crystalline ice, arising from photoexcited water molecules in the top monolayer. This peak is less pronounced in amorphous solid water. H atoms that are trapped may be displaced by up to ∼10 water cages, but migrate on average 3 water cages. Trapped OH fragments tend to stay near the original solvent cage.

Electrical Characterization of Amorphous Silicon MIS-Based Structures for HIT Solar Cell Applications

NASA Astrophysics Data System (ADS)

García, Héctor; Castán, Helena; Dueñas, Salvador; Bailón, Luis; García-Hernansanz, Rodrigo; Olea, Javier; del Prado, Álvaro; Mártil, Ignacio

2016-07-01

A complete electrical characterization of hydrogenated amorphous silicon layers (a-Si:H) deposited on crystalline silicon (c-Si) substrates by electron cyclotron resonance chemical vapor deposition (ECR-CVD) was carried out. These structures are of interest for photovoltaic applications. Different growth temperatures between 30 and 200 °C were used. A rapid thermal annealing in forming gas atmosphere at 200 °C during 10 min was applied after the metallization process. The evolution of interfacial state density with the deposition temperature indicates a better interface passivation at higher growth temperatures. However, in these cases, an important contribution of slow states is detected as well. Thus, using intermediate growth temperatures (100-150 °C) might be the best choice.

Atomic Layer Deposited Thin Films for Dielectrics, Semiconductor Passivation, and Solid Oxide Fuel Cells

NASA Astrophysics Data System (ADS)

Xu, Runshen

Atomic layer deposition (ALD) utilizes sequential precursor gas pulses to deposit one monolayer or sub-monolayer of material per cycle based on its self-limiting surface reaction, which offers advantages, such as precise thickness control, thickness uniformity, and conformality. ALD is a powerful means of fabricating nanoscale features in future nanoelectronics, such as contemporary sub-45 nm metal-oxide-semiconductor field effect transistors, photovoltaic cells, near- and far-infrared detectors, and intermediate temperature solid oxide fuel cells. High dielectric constant, kappa, materials have been recognized to be promising candidates to replace traditional SiO2 and SiON, because they enable good scalability of sub-45 nm MOSFET (metal-oxide-semiconductor field-effect transistor) without inducing additional power consumption and heat dissipation. In addition to high dielectric constant, high-kappa materials must meet a number of other requirements, such as low leakage current, high mobility, good thermal and structure stability with Si to withstand high-temperature source-drain activation annealing. In this thesis, atomic layer deposited Er2O3 doped TiO2 is studied and proposed as a thermally stable amorphous high-kappa dielectric on Si substrate. The stabilization of TiO2 in its amorphous state is found to achieve a high permittivity of 36, a hysteresis voltage of less than 10 mV, and a low leakage current density of 10-8 A/cm-2 at -1 MV/cm. In III-V semiconductors, issues including unsatisfied dangling bonds and native oxides often result in inferior surface quality that yields non-negligible leakage currents and degrades the long-term performance of devices. The traditional means for passivating the surface of III-V semiconductors are based on the use of sulfide solutions; however, that only offers good protection against oxidation for a short-term (i.e., one day). In this work, in order to improve the chemical passivation efficacy of III-V semiconductors

Spherical silicon photonic microcavities: From amorphous to polycrystalline

NASA Astrophysics Data System (ADS)

Fenollosa, R.; Garín, M.; Meseguer, F.

2016-06-01

Shaping silicon as a spherical object is not an obvious task, especially when the object size is in the micrometer range. This has the important consequence of transforming bare silicon material in a microcavity, so it is able to confine light efficiently. Here, we have explored the inside volume of such microcavities, both in their amorphous and in their polycrystalline versions. The synthesis method, which is based on chemical vapor deposition, causes amorphous microspheres to have a high content of hydrogen that produces an onionlike distributed porous core when the microspheres are crystallized by a fast annealing regime. This substantially influences the resonant modes. However, a slow crystallization regime does not yield pores, and produces higher-quality-factor resonances that could be fitted to the Mie theory. This allows the establishment of a procedure for obtaining size calibration standards with relative errors of the order of 0.1%.

Black GE based on crystalline/amorphous core/shell nanoneedle arrays

DOEpatents

Javey, Ali; Chueh, Yu-Lun; Fan, Zhiyong

2014-03-04

Direct growth of black Ge on low-temperature substrates, including plastics and rubber is reported. The material is based on highly dense, crystalline/amorphous core/shell Ge nanoneedle arrays with ultrasharp tips (.about.4 nm) enabled by the Ni catalyzed vapor-solid-solid growth process. Ge nanoneedle arrays exhibit remarkable optical properties. Specifically, minimal optical reflectance (<1%) is observed, even for high angles of incidence (.about.75.degree.) and for relatively short nanoneedle lengths (.about.1 .mu.m). Furthermore, the material exhibits high optical absorption efficiency with an effective band gap of .about.1 eV. The reported black Ge can have important practical implications for efficient photovoltaic and photodetector applications on nonconventional substrates.

Hydration products in sulfoaluminate cements: Evaluation of amorphous phases by XRD/solid-state NMR

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

Gastaldi, D., E-mail: dgastaldi@buzziunicem.it; Paul, G., E-mail: geo.paul@uniupo.it; Marchese, L.

The hydration of four sulfoaluminate cements have been studied: three sulfoaluminate systems, having different content of sulfate and silicate, and one blend Portland-CSA-calcium sulfate binder. Hydration was followed up to 90 days by means of a combination of X-ray diffraction and solid state MAS-NMR; Differential scanning calorimetry and Scanning electron microscopy were also performed in order to help the interpretation of experimental data. High amount of amorphous phases were found in all the four systems: in low-sulfate cements, amorphous part is mainly ascribed to monosulfate and aluminium hydroxide, while strätlingite is observed if belite is present in the cement; inmore » the blend system, C-S-H contributes to the amorphous phase beyond monosulfate.« less

Amorphous solid dispersions of piroxicam and Soluplus(®): Qualitative and quantitative analysis of piroxicam recrystallization during storage.

PubMed

Lust, Andres; Strachan, Clare J; Veski, Peep; Aaltonen, Jaakko; Heinämäki, Jyrki; Yliruusi, Jouko; Kogermann, Karin

2015-01-01

The conversion of active pharmaceutical ingredient (API) from amorphous to crystalline form is the primary stability issue in formulating amorphous solid dispersions (SDs). The aim of the present study was to carry out qualitative and quantitative analysis of the physical solid-state stability of the SDs of poorly water-soluble piroxicam (PRX) and polyvinyl caprolactam-polyvinyl acetate-polyethylene-glycol graft copolymer (Soluplus(®)). The SDs were prepared by a solvent evaporation method and stored for six months at 0% RH/6 °C, 0% RH/25 °C, 40% RH/25 °C and 75% RH/25 °C. Fourier transform infrared spectroscopy equipped with attenuated total reflection accessory (ATR-FTIR) and Raman spectroscopy were used for characterizing the physical solid-state changes and drug-polymer interactions. The principal component analysis (PCA) and multivariate curve resolution alternating least squares (MCR-ALS) were used for the qualitative and quantitative analysis of Raman spectra collected during storage. When stored at 0% RH/6 °C and at 0% RH/25 °C, PRX in SDs remained in an amorphous form since no recrystallization was observed by ATR-FTIR and Raman spectroscopy. Raman spectroscopy coupled with PCA and MCR-ALS and ATR-FTIR spectroscopy enabled to detect the recrystallization of amorphous PRX in the samples stored at higher humidity. Copyright © 2015 Elsevier B.V. All rights reserved.

The Use af Ion Vapor Deposited Aluminum (IVD) for the Space Shuttle Solid Rocket Booster (SRB)

NASA Technical Reports Server (NTRS)

Novak, Howard L.

2002-01-01

The USA LLC Materials & Processes (M&P) Engineering Department had recommended the application and evaluation of Ion Vapor Deposition (IVD) aluminum to SRB Hardware for corrosion protection and elimination of hazardous materials and processes such as cadmium plating. IVD is an environmentally friendly process that has no volatile organic compounds (VOCs), or hazardous waste residues. It lends itself to use with hardware exposed to corrosive seacoast environments as found at Kennedy Space Center (KSC), and Cape Canaveral Air Force Station (CCAFS), Florida. Lifting apparatus initially coated with cadmium plating for corrosion protection; was stripped and successfully re-coated with IVD aluminum after the cadmium plating no longer protected the GSE from corrosion, Since then, and after completion of a significant test program, the first flight application of the IVD Aluminum process on the Drogue Parachute Ratchet Assembly is scheduled for 2002.

Electrical property of macroscopic graphene composite fibers prepared by chemical vapor deposition

NASA Astrophysics Data System (ADS)

Sun, Haibin; Fu, Can; Gao, Yanli; Guo, Pengfei; Wang, Chunlei; Yang, Wenchao; Wang, Qishang; Zhang, Chongwu; Wang, Junya; Xu, Junqi

2018-07-01

Graphene fibers are promising candidates in portable and wearable electronics due to their tiny volume, flexibility and wearability. Here, we successfully synthesized macroscopic graphene composite fibers via a two-step process, i.e. first electrospinning and then chemical vapor deposition (CVD). Briefly, the well-dispersed PAN nanofibers were sprayed onto the copper surface in an electrified thin liquid jet by electrospinning. Subsequently, CVD growth process induced the formation of graphene films using a PAN-solid source of carbon and a copper catalyst. Finally, crumpled and macroscopic graphene composite fibers were obtained from carbon nanofiber/graphene composite webs by self-assembly process in the deionized water. Temperature-dependent conduct behavior reveals that electron transport of the graphene composite fibers belongs to hopping mechanism and the typical electrical conductivity reaches 4.59 × 103 S m‑1. These results demonstrated that the graphene composite fibers are promising for the next-generation flexible and wearable electronics.

Electrical property of macroscopic graphene composite fibers prepared by chemical vapor deposition.

PubMed

Sun, Haibin; Fu, Can; Gao, Yanli; Guo, Pengfei; Wang, Chunlei; Yang, Wenchao; Wang, Qishang; Zhang, Chongwu; Wang, Junya; Xu, Junqi

2018-07-27

Graphene fibers are promising candidates in portable and wearable electronics due to their tiny volume, flexibility and wearability. Here, we successfully synthesized macroscopic graphene composite fibers via a two-step process, i.e. first electrospinning and then chemical vapor deposition (CVD). Briefly, the well-dispersed PAN nanofibers were sprayed onto the copper surface in an electrified thin liquid jet by electrospinning. Subsequently, CVD growth process induced the formation of graphene films using a PAN-solid source of carbon and a copper catalyst. Finally, crumpled and macroscopic graphene composite fibers were obtained from carbon nanofiber/graphene composite webs by self-assembly process in the deionized water. Temperature-dependent conduct behavior reveals that electron transport of the graphene composite fibers belongs to hopping mechanism and the typical electrical conductivity reaches 4.59 × 10 3 S m -1 . These results demonstrated that the graphene composite fibers are promising for the next-generation flexible and wearable electronics.

Vapors and Droplets Mixture Deposition of Metallic Coatings by Very Low Pressure Plasma Spraying

NASA Astrophysics Data System (ADS)

Vautherin, B.; Planche, M.-P.; Bolot, R.; Quet, A.; Bianchi, L.; Montavon, G.

2014-04-01

In recent years, the very low pressure plasma-spraying (VLPPS) process has been intensely developed and implemented to manufacture thin, dense and finely structured ceramic coatings for various applications, such as Y2O3 for diffusion barriers, among other examples. This paper aims at presenting developments carried out on metallic coatings. Aluminum was chosen as a demonstrative material due to its "moderate" vaporization enthalpy (i.e., 38.23 KJ cm-3) compared to the one of copper (i.e., 55.33 KJ cm-3), cobalt (i.e., 75.03 KJ cm-3), or even tantalum (i.e., 87.18 KJ cm-3). The objective of this work is primarily to better understand the behavior of a solid precursor injected into the plasma jet leading to the formation of vapors and to better control the factors affecting the coating structure. Nearly dense aluminum coatings were successfully deposited by VLPPS at 100 Pa with an intermediate power plasma torch (i.e., Sulzer Metco F4 type gun with maximum power of 45 kW). Optical emission spectroscopy (OES) was implemented to study and analyze the vapor behavior into the plasma jet. Simplified CFD modeling allowed better understanding of some of the thermo-physical mechanisms. The effect of powder-size distribution, substrate temperature and spray distance were studied. The phase composition and microstructural features of the coatings were characterized by XRD and SEM. Moreover, Vickers microhardness measurements were implemented.

Enhanced photoluminescence from ring resonators in hydrogenated amorphous silicon thin films at telecommunications wavelengths.

PubMed

Patton, Ryan J; Wood, Michael G; Reano, Ronald M

2017-11-01

We report enhanced photoluminescence in the telecommunications wavelength range in ring resonators patterned in hydrogenated amorphous silicon thin films deposited via low-temperature plasma enhanced chemical vapor deposition. The thin films exhibit broadband photoluminescence that is enhanced by up to 5 dB by the resonant modes of the ring resonators due to the Purcell effect. Ellipsometry measurements of the thin films show a refractive index comparable to crystalline silicon and an extinction coefficient on the order of 0.001 from 1300 nm to 1600 nm wavelengths. The results are promising for chip-scale integrated optical light sources.

Differential alternating current chip calorimeter for in situ investigation of vapor-deposited thin films

NASA Astrophysics Data System (ADS)

Ahrenberg, M.; Shoifet, E.; Whitaker, K. R.; Huth, H.; Ediger, M. D.; Schick, C.

2012-03-01

Physical vapor deposition can be used to produce thin films with interesting material properties including extraordinarily stable organic glasses. We describe an ac chip calorimeter for in situ heat capacity measurements of as-deposited nanometer thin films of organic glass formers. The calorimetric system is based on a differential ac chip calorimeter which is placed in the vacuum chamber for physical vapor deposition. The sample is directly deposited onto one calorimetric chip sensor while the other sensor is protected against deposition. The device and the temperature calibration procedure are described. The latter makes use of the phase transitions of cyclopentane and the frequency dependence of the dynamic glass transition of toluene and ethylbenzene. Sample thickness determination is based on a finite element modeling of the sensor sample arrangement. In the modeling, a layer of toluene was added to the sample sensor and its thickness was varied in an iterative way until the model fit the experimental data.

Synthesis and characterization of beta-Ga2O3 nanorod array clumps by chemical vapor deposition.

PubMed

Shi, Feng; Wei, Xiaofeng

2012-11-01

beta-Ga2O3 nanorod array clumps were successfully synthesized on Si (111) substrates by chemical vapor deposition. The composition, microstructure, morphology, and light-emitting property of these clumps were characterized by X-ray diffraction, Fourier transform infrared spectrophotometry, X-ray photoelectron spectroscopy, scanning electron microscopy, high-resolution transmission electron microscopy, Raman spectroscopy, and photoluminescence. The results demonstrate that the sample synthesized at 1050 degrees C for 15 min was composed of monoclinic beta-Ga2O3 nanorod array clumps, where each single nanorod was about 300 nm in diameter with some nano-droplets on its tip. These results reveal that the growth mechanism agrees with the vapor-liquid-solid (VLS) process. The photoluminescence spectrum shows that the Ga2O3 nanorods have a blue emission at 438 nm, which may be attributed to defects, such as oxygen vacancies and gallium-oxygen vacancy pairs. Defect-energy aggregation confinement growth theory was proposed to explain the growth mechanism of Ga2O3 nanorod array clumps collaborated with the VLS mechanism.

High-aspect-ratio and high-flatness Cu3(SiGe) nanoplatelets prepared by chemical vapor deposition.

PubMed

Klementová, Mariana; Palatinus, Lukás; Novotný, Filip; Fajgar, Radek; Subrt, Jan; Drínek, Vladislav

2013-06-01

Cu3(SiGe) nanoplatelets were synthesized by low-pressure chemical vapor deposition of a SiH3C2H5/Ge2(CH3)6 mixture on a Cu-substrate at 500 degrees C, total pressure of 110-115 Pa, and Ge/Si molar ratio of 22. The nanoplatelets with composition Cu76Si15Ge12 are formed by the 4'-phase, and they are flattened perpendicular to the [001] direction. Their lateral dimensions reach several tens of micrometers in size, but they are only about 50 nm thick. Their surface is extremely flat, with measured root mean square roughness R(q) below 0.2 nm. The nanoplatelets grow via the non-catalytic vapor-solid mechanism and surface growth. In addition, nanowires and nanorods of various Cu-Si-Ge alloys were also obtained depending on the experimental conditions. Morphology of the resulting Cu-Si-Ge nanoobjects is very sensitive to the experimental parameters. The formation of nanoplatelets is associated with increased amount of Ge in the alloy.

Metalorganic Chemical Vapor Deposition of Ruthenium-Doped Diamond like Carbon Films

NASA Technical Reports Server (NTRS)

Sunkara, M. K.; Ueno, M.; Lian, G.; Dickey, E. C.

2001-01-01

We investigated metalorganic precursor deposition using a Microwave Electron Cyclotron Resonance (ECR) plasma for depositing metal-doped diamondlike carbon films. Specifically, the deposition of ruthenium doped diamondlike carbon films was investigated using the decomposition of a novel ruthenium precursor, Bis(ethylcyclopentadienyl)-ruthenium (Ru(C5H4C2H5)2). The ruthenium precursor was introduced close to the substrate stage. The substrate was independently biased using an applied RF power. Films were characterized using Fourier Transform Infrared Spectroscopy (FTIR), Transmission Electron Microscopy (TEM) and Four Point Probe. The conductivity of the films deposited using ruthenium precursor showed strong dependency on the deposition parameters such as pressure. Ruthenium doped sample showed the presence of diamond crystallites with an average size of approx. 3 nm while un-doped diamondlike carbon sample showed the presence of diamond crystallites with an average size of 11 nm. TEM results showed that ruthenium was atomically dispersed within the amorphous carbon network in the films.

Physical stability of API/polymer-blend amorphous solid dispersions.

PubMed

Lehmkemper, Kristin; Kyeremateng, Samuel O; Bartels, Mareike; Degenhardt, Matthias; Sadowski, Gabriele

2018-03-01

The preparation of amorphous solid dispersions (ASDs) is a well-established strategy for formulating active pharmaceutical ingredients by embedding them in excipients, usually amorphous polymers. Different polymers can be combined for designing ASDs with desired properties like an optimized dissolution behavior. One important criterion for the development of ASD compositions is the physical stability. In this work, the physical stability of API/polymer-blend ASDs was investigated by thermodynamic modeling and stability studies. Amorphous naproxen (NAP) and acetaminophen (APAP) were embedded in blends of hydroxypropyl methylcellulose acetate succinate (HPMCAS) and either poly(vinylpyrrolidone) (PVP) or poly(vinylpyrrolidone-co-vinyl acetate) (PVPVA64). Parameters for modeling the API solubility in the blends and the glass-transition temperature curves of the water-free systems with Perturbed-Chain Statistical Associating Fluid Theory and Kwei equation, respectively, were correlated to experimental data. The phase behavior for standardized storage conditions (0%, 60% and 75% relative humidity (RH)) was predicted and compared to six months-long stability studies. According to modeling and experimental results, the physical stability was reduced with increasing HPMCAS content and increasing RH. This trend was observed for all investigated systems, with both APIs (NAP and APAP) and both polymer blends (PVP/HPMCAS and PVPVA64/HPMCAS). PC-SAFT and the Kwei equation turned out to be suitable tools for modeling and predicting the physical stability of the investigated API/polymer-blends ASDs. Copyright © 2017 Elsevier B.V. All rights reserved.

Expanding the molecular-ruler process through vapor deposition of hexadecanethiol

PubMed Central

Patron, Alexandra M; Hooker, Timothy S; Santavicca, Daniel F

2017-01-01

The development of methods to produce nanoscale features with tailored chemical functionalities is fundamental for applications such as nanoelectronics and sensor fabrication. The molecular-ruler process shows great utility for this purpose as it combines top-down lithography for the creation of complex architectures over large areas in conjunction with molecular self-assembly, which enables precise control over the physical and chemical properties of small local features. The molecular-ruler process, which most commonly uses mercaptoalkanoic acids and metal ions to generate metal-ligated multilayers, can be employed to produce registered nanogaps between metal features. Expansion of this methodology to include molecules with other chemical functionalities could greatly expand the overall versatility, and thus the utility, of this process. Herein, we explore the use of alkanethiol molecules as the terminating layer of metal-ligated multilayers. During this study, it was discovered that the solution deposition of alkanethiol molecules resulted in low overall surface coverage with features that varied in height. Because features with varied heights are not conducive to the production of uniform nanogaps via the molecular-ruler process, the vapor-phase deposition of alkanethiol molecules was explored. Unlike the solution-phase deposition, alkanethiol islands produced by vapor-phase deposition exhibited markedly higher surface coverages of uniform heights. To illustrate the applicability of this method, metal-ligated multilayers, both with and without an alkanethiol capping layer, were utilized to create nanogaps between Au features using the molecular-ruler process. PMID:29181290

De-vitrification of nanoscale phase-separated amorphous thin films in the immiscible copper-niobium system

NASA Astrophysics Data System (ADS)

Puthucode, A.; Devaraj, A.; Nag, S.; Bose, S.; Ayyub, P.; Kaufman, M. J.; Banerjee, R.

2014-05-01

Copper and niobium are mutually immiscible in the solid state and exhibit a large positive enthalpy of mixing in the liquid state. Using vapour quenching via magnetron co-sputter deposition, far-from equilibrium amorphous Cu-Nb films have been deposited which exhibit a nanoscale phase separation. Annealing these amorphous films at low temperatures (~200 °C) initiates crystallization via the nucleation and growth of primary nanocrystals of a face-centred cubic Cu-rich phase separated by the amorphous matrix. Interestingly, subsequent annealing at a higher temperature (>300 °C) leads to the polymorphic nucleation and growth of large spherulitic grains of a body-centred cubic Nb-rich phase within the retained amorphous matrix of the partially crystallized film. This sequential two-stage crystallization process has been investigated in detail by combining transmission electron microscopy [TEM] (including high-resolution TEM) and atom probe tomography studies. These results provide new insights into the crystallization behaviour of such unusual far-from equilibrium phase-separated metallic glasses in immiscible systems.

Laboratory study on the adsorption of Mn(2+) on suspended and deposited amorphous Al(OH)(3) in drinking water distribution systems.

PubMed

Wang, Wendong; Zhang, Xiaoni; Wang, Hongping; Wang, Xiaochang; Zhou, Lichuan; Liu, Rui; Liang, Yuting

2012-09-01

Manganese (II) is commonly present in drinking water. This paper mainly focuses on the adsorption of manganese on suspended and deposited amorphous Al(OH)(3) solids. The effects of water flow rate and water quality parameters, including solution pH and the concentrations of Mn(2+), humic acid, and co-existing cations on adsorption were investigated. It was found that chemical adsorption mainly took place in drinking water with pHs above 7.5; suspended Al(OH)(3) showed strong adsorption capacity for Mn(2+). When the total Mn(2+) input was 3 mg/L, 1.0 g solid could accumulate approximately 24.0 mg of Mn(2+) at 15 °C. In drinking water with pHs below 7.5, because of H(+) inhibition, active reaction sites on amorphous Al(OH)(3) surface were much less. The adsorption of Mn(2+) on Al(OH)(3) changed gradually from chemical coordination to physical adsorption. In drinking water with high concentrations of Ca(2+), Mg(2+), Fe(3+), and HA, the removal of Mn(2+) was enhanced due to the effects of co-precipitation and adsorption. In solution with 1.0 mg/L HA, the residual concentration of Mn(2+) was below 0.005 mg/L, much lower than the limit value required by the Chinese Standard for Drinking Water Quality. Unlike suspended Al(OH)(3), deposited Al(OH)(3) had a much lower adsorption capacity of 0.85 mg/g, and the variation in flow rate and major water quality parameters had little effect on it. Improved managements of water age, pipe flushing and mechanical cleaning were suggested to control residual Mn(2+). Copyright © 2012 Elsevier Ltd. All rights reserved.

Heteroepitaxial growth of 3-5 semiconductor compounds by metal-organic chemical vapor deposition for device applications

NASA Technical Reports Server (NTRS)

Collis, Ward J.; Abul-Fadl, Ali

1988-01-01

The purpose of this research is to design, install and operate a metal-organic chemical vapor deposition system which is to be used for the epitaxial growth of 3-5 semiconductor binary compounds, and ternary and quaternary alloys. The long-term goal is to utilize this vapor phase deposition in conjunction with existing current controlled liquid phase epitaxy facilities to perform hybrid growth sequences for fabricating integrated optoelectronic devices.

Charging and Discharging of Amorphous Solid Water Ice: Effects of Porosity

NASA Astrophysics Data System (ADS)

Bu, Caixia; Baragiola, Raul A.

2015-11-01

Introduction: Amorphous solid water (ASW) is abundant on Saturn’s icy satellites and rings [1,2], where it is subject to bombardment of energetic ions, electrons, and photons; together with secondary electron and ion emission, this may leave the surfaces charged. Surface potential can affect the flux of incoming charged particles, altering surface evolution. We examined the role of porosity [3] on electrostatic charging and discharging of ASW films at 30-140 K.Experiment: Experiments were performed in ultra-high vacuum [4]. ASW films were deposited at 30 K onto a liquid-He-cooled quartz crystal microbalance (QCM). Film porosity was calculated from the areal mass via the QCM and thickness via a UV-visible interferometry. ASW films were charged at 30 K using 500 eV He+. Surface potentials (Vs) of the films were measured with a Kelvin probe, and infrared spectra were collected using a Fourier transform infrared spectrometer.Results: We measured Vs of the ASW film at 30 K as a function of ion fluence (F). The Vs(F) deviates from a straight line at low fluence, attributed to emitted secondary electrons due to the negative polarization voltage [5,6], and increases linearly when the Vs is positive. We also measured Vs as a function of annealing temperature. We prepared ASW films with various porosities by annealing the films to different temperatures (Ta) prior to irradiation or varying the vapor-beam incidence angle (θ). Upon heating, we observed sharp decreases of the Vs at temperatures that strongly depend on Ta and θ. Decreases of the infrared absorbance of the dangling OH bands of the charged film share similar trends as that of the Vs. We propose a model that includes porosity for electrostatic charging/discharging of ASW films at temperatures below 100 K. Results are applicable to the study of plasma-surface interactions of icy satellites and rings.References: [1] Jurac et al., J. Geophys. Res. 100, 14821 (1995); [2] A. L. Graps et al., Space Sci. Rev. 137, 435

Hydrogenated nanostructure boron doped amorphous carbon films by DC bias

NASA Astrophysics Data System (ADS)

Ishak, A.; Dayana, K.; Saurdi, I.; Malek, M. F.; Rusop, M.

2018-03-01

Hydrogenated nanostructure-boron doped amorphous carbon thin film carbon was deposited at different negative bias using custom-made deposition bias assisted-CVD. Solid of boron and palm oil were used as dopant and carbon source, respectively. The hydrogenated nanostructure amorphous films were characterized by Field emission scanning electron microscopy, Fourier transform infrared spectroscopy, Raman spectroscopy, while the photo-response studies of thin film is done by I-V measurement under light measurement. The results showed the carbon film were in nanostructure with hydrogen and boron might be incorporated in the film. The Raman spectra observed the increase of upward shift of D and G peaks as negative bias increased which related to the structural change as boron incorporated in carbon network. These structural changes were further correlated with photo-response study and the results obtained are discussed and compared.

Reactive multilayers fabricated by vapor deposition. A critical review

DOE PAGES

Adams, D. P.

2014-10-02

The reactive multilayer thin films are a class of energetic materials that continue to attract attention for use in joining applications and as igniters. Generally composed of two reactants, these heterogeneous solids can be stimulated by an external source to promptly release stored chemical energy in a sudden emission of light and heat. In our critical review article, results from recent investigations of these materials are discussed. Discussion begins with a brief description of the vapor deposition techniques that provide accurate control of layer thickness and film composition. More than 50 reactive film compositions have been reported to date, withmore » most multilayers fabricated by magnetron sputter deposition or electron-beam evaporation. In later sections, we review how multilayer ignition threshold, reaction rate, and total heat are tailored via thin film design. For example, planar multilayers with nanometer-scale periodicity exhibit rapid, self-sustained reactions with wavefront velocities up to 100 m/s. Numeric and analytical models have elucidated many of the fundamental processes that underlie propagating exothermic reactions while demonstrating how reaction rates vary with multilayer design. Recent, time-resolved diffraction and imaging studies have further revealed the phase transformations and the wavefront dynamics associated with propagating chemical reactions. Many reactive multilayers (e.g., Co/Al) form product phases that are consistent with published equilibrium phase diagrams, yet a few systems, such as Pt/Al, develop metastable products. The final section highlights current and emerging applications of reactive multilayers. Examples include reactive Ni(V)/Al and Pd/Al multilayers which have been developed for localized soldering of heat-sensitive components.« less

Characterization of Two Distinct Amorphous Forms of Valsartan by Solid-State NMR.

PubMed

Skotnicki, Marcin; Apperley, David C; Aguilar, Juan A; Milanowski, Bartłomiej; Pyda, Marek; Hodgkinson, Paul

2016-01-04

Valsartan (VAL) is an antihypertensive drug marketed in an amorphous form. Amorphous materials can have different physicochemical properties depending on preparation method, thermal history, etc., but the nature of such materials is difficult to study by diffraction techniques. This study characterizes two different amorphous forms of valsartan (AR and AM) using solid-state NMR (SSNMR) as a primary investigation tool, supported by solution-state NMR, FT-IR, TMDSC, and dissolution tests. The two forms are found to be clearly distinct, with a significantly higher level of structural arrangement in the AR form, as observed in (13)C, (15)N, and (1)H SSNMR. (13)C and (15)N NMR indicates that the fully amorphous material (AM) contains an approximately equal ratio of cis-trans conformers about the amide bond, whereas the AR form exists mainly as one conformer, with minor conformational "defects". (1)H ultrafast MAS NMR shows significant differences in the hydrogen bonding involving the tetrazole and acid hydrogens between the two materials, while (15)N NMR shows that both forms exist as a 1,2,3,4-tetrazole tautomer. NMR relaxation times show subtle differences in local and bulk molecular mobility, which can be connected with the glass transition, the stability of the glassy material, and its response to aging. Counterintuitively the fully amorphous material is found to have a significantly lower dissolution rate than the apparently more ordered AR material.

Spontaneous Oscillations and Waves during Chemical Vapor Deposition of InN

NASA Astrophysics Data System (ADS)

Jiang, F.; Munkholm, A.; Wang, R.-V.; Streiffer, S. K.; Thompson, Carol; Fuoss, P. H.; Latifi, K.; Elder, K. R.; Stephenson, G. B.

2008-08-01

We report observations of self-sustaining spatiotemporal chemical oscillations during metal-organic chemical vapor deposition of InN onto GaN. Under constant supply of vapor precursors trimethylindium and NH3, the condensed-phase cycles between crystalline islands of InN and elemental In droplets. Propagating fronts between regions of InN and In occur with linear, circular, and spiral geometries. The results are described by a model in which the nitrogen activity produced by surface-catalyzed NH3 decomposition varies with the exposed surface areas of GaN, InN, and In.

Spontaneous oscillations and waves during chemical vapor deposition of InN.

PubMed

Jiang, F; Munkholm, A; Wang, R-V; Streiffer, S K; Thompson, Carol; Fuoss, P H; Latifi, K; Elder, K R; Stephenson, G B

2008-08-22

We report observations of self-sustaining spatiotemporal chemical oscillations during metal-organic chemical vapor deposition of InN onto GaN. Under constant supply of vapor precursors trimethylindium and NH3, the condensed-phase cycles between crystalline islands of InN and elemental In droplets. Propagating fronts between regions of InN and In occur with linear, circular, and spiral geometries. The results are described by a model in which the nitrogen activity produced by surface-catalyzed NH3 decomposition varies with the exposed surface areas of GaN, InN, and In.

Formulation and process design for a solid dosage form containing a spray-dried amorphous dispersion of ibipinabant.

PubMed

Leane, Michael M; Sinclair, Wayne; Qian, Feng; Haddadin, Raja; Brown, Alan; Tobyn, Mike; Dennis, Andrew B

2013-01-01

Amorphous forms of poorly soluble drugs are more frequently being incorporated into solid dispersions for administration and extensive research has led to a reasonable understanding of how these dispersions, although still kinetically unstable, improve stability relative to the pure amorphous form. There remains however a paucity of literature describing the effects on such solid dispersions of subsequent processing into solid dosage forms such as tablets. This paper addresses this area by looking at the effects of the addition of common excipients and different manufacturing routes on the stability of a spray-dried dispersion (SDD) of the cannabinoid CB-1 antagonist, ibipinabant. A marked difference in physical stability of tablets was seen with the different fillers with microcrystalline cellulose (MCC) giving the best stability profile. It was found that minimising the number of compression steps led to improved formulation stability with a direct compression process giving the best results. Increased levels of crystallinity were seen in coated tablets most likely due to the exposure of the amorphous matrix to moisture and heat during the coating process. DSIMS analysis of the SDD particles indicated increased levels of polymer on the surface.

Room temperature visible photoluminescence of silicon nanocrystallites embedded in amorphous silicon carbide matrix

NASA Astrophysics Data System (ADS)

Coscia, U.; Ambrosone, G.; Basa, D. K.

2008-03-01

The nanocrystalline silicon embedded in amorphous silicon carbide matrix was prepared by varying rf power in high vacuum plasma enhanced chemical vapor deposition system using silane methane gas mixture highly diluted in hydrogen. In this paper, we have studied the evolution of the structural, optical, and electrical properties of this material as a function of rf power. We have observed visible photoluminescence at room temperature and also have discussed the role played by the Si nanocrystallites and the amorphous silicon carbide matrix. The decrease of the nanocrystalline size, responsible for quantum confinement effect, facilitated by the amorphous silicon carbide matrix, is shown to be the primary cause for the increase in the PL intensity, blueshift of the PL peak position, decrease of the PL width (full width at half maximum) as well as the increase of the optical band gap and the decrease of the dark conductivity.

Annealing optimization of hydrogenated amorphous silicon suboxide film for solar cell application

NASA Astrophysics Data System (ADS)

Guangzhi, Jia; Honggang, Liu; Hudong, Chang

2011-05-01

We investigate a passivation scheme using hydrogenated amorphous silicon suboxide (a-SiOx:H) film for industrial solar cell application. The a-SiOx:H films were deposited using plasma-enhanced chemical vapor deposition (PECVD) by decomposing nitrous oxide, helium and silane at a substrate temperature of around 250 °C. An extensive study has been carried out on the effect of thermal annealing on carrier lifetime and surface recombination velocity, which affect the final output of the solar cell. Minority carrier lifetimes for the deposited a-SiOx:H films without and with the thermal annealing on 4 Ω·cm p-type float-zone silicon wafers are 270 μs and 670 μs, respectively, correlating to surface recombination velocities of 70 cm/s and 30 cm/s. Optical analysis has revealed a distinct decrease of blue light absorption in the a-SiOx:H films compared to the commonly used intrinsic amorphous silicon passivation used in solar cells. This paper also reports that the low cost and high quality passivation fabrication sequences employed in this study are suitable for industrial processes.

Influence of deposition temperature and amorphous carbon on microstructure and oxidation resistance of magnetron sputtered nanocomposite Crsbnd C films

NASA Astrophysics Data System (ADS)

Nygren, Kristian; Andersson, Matilda; Högström, Jonas; Fredriksson, Wendy; Edström, Kristina; Nyholm, Leif; Jansson, Ulf

2014-06-01

It is known that mechanical and tribological properties of transition metal carbide films can be tailored by adding an amorphous carbon (a-C) phase, thus making them nanocomposites. This paper addresses deposition, microstructure, and for the first time oxidation resistance of magnetron sputtered nanocomposite Crsbnd C/a-C films with emphasis on studies of both phases. By varying the deposition temperature between 20 and 700 °C and alternating the film composition, it was possible to deposit amorphous, nanocomposite, and crystalline Crsbnd C films containing about 70% C and 30% Cr, or 40% C and 60% Cr. The films deposited at temperatures below 300 °C were X-ray amorphous and 500 °C was required to grow crystalline phases. Chronoamperometric polarization at +0.6 V vs. Ag/AgCl (sat. KCl) in hot 1 mM H2SO4 resulted in oxidation of Crsbnd C, yielding Cr2O3 and C, as well as oxidation of C. The oxidation resistance is shown to depend on the deposition temperature and the presence of the a-C phase. Physical characterization of film surfaces show that very thin C/Cr2O3/Crsbnd C layers develop on the present material, which can be used to improve the oxidation resistance of, e.g. stainless steel electrodes.

Final Report: Vapor Transport Deposition for Thin Film III-V Photovoltaics

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

Boettcher, Shannon; Greenaway, Ann; Boucher, Jason

2016-02-10

Silicon, the dominant photovoltaic (PV) technology, is reaching its fundamental performance limits as a single absorber/junction technology. Higher efficiency devices are needed to reduce cost further because the balance of systems account for about two-thirds of the overall cost of the solar electricity. III-V semiconductors such as GaAs are used to make the highest-efficiency photovoltaic devices, but the costs of manufacture are much too high for non-concentrated terrestrial applications. The cost of III-V’s is driven by two factors: (1) metal-organic chemical vapor deposition (MOCVD), the dominant growth technology, employs expensive, toxic and pyrophoric gas-phase precursors, and (2) the growth substratesmore » conventionally required for high-performance devices are monocrystalline III-V wafers. The primary goal of this project was to show that close-spaced vapor transport (CSVT), using water vapor as a transport agent, is a scalable deposition technology for growing low-cost epitaxial III-V photovoltaic devices. The secondary goal was to integrate those devices on Si substrates for high-efficiency tandem applications using interface nanopatterning to address the lattice mismatch. In the first task, we developed a CSVT process that used only safe solid-source powder precursors to grow epitaxial GaAs with controlled n and p doping and mobilities/lifetimes similar to that obtainable via MOCVD. Using photoelectrochemical characterization, we showed that the best material had near unity internal quantum efficiency for carrier collection and minority carrier diffusions lengths in of ~ 8 μm, suitable for PV devices with >25% efficiency. In the second task we developed the first pn junction photovoltaics using CSVT and showed unpassivated structures with open circuit photovoltages > 915 mV and internal quantum efficiencies >0.9. We also characterized morphological and electrical defects and identified routes to reduce those defects. In task three we grew

Raman studies on molecular and ionic forms in solid layers of nitrogen dioxide - Temperature and light induced effects

NASA Astrophysics Data System (ADS)

Givan, A.; Loewenschuss, A.

1990-12-01

Raman spectra of zero-pressure-formed N2O4 solid layers are reported. Sample composition is extremely dependent upon deposition conditions. For ordered and pure solid N2O4(D2h), produced by slow NO2 deposition, temperature cycling over the range in which the solid is stable shows no significant spectral changes and does not result in autoionization, as argued in a previous Raman study. Fast and low temperature deposited layers are amorphous and multicomponent, showing bands of disordered and isomeric molecular N2O4 and of ionic NO + NO3, nitrosonium nitrate. For nitrosonium nitrate, three solid modifications can be characterized spectroscopically. In the amorphous phase, a light induced, temperature dependent, reversible transition between molecular and ionic nitrogen tetroxide is observed below 150 K. The paths leading to nitrosonium nitrate formation are examined.

Why Chemical Vapor Deposition Grown MoS2 Samples Outperform Physical Vapor Deposition Samples: Time-Domain ab Initio Analysis.

PubMed

Li, Linqiu; Long, Run; Prezhdo, Oleg V

2018-06-13

Two-dimensional transition metal dichalcogenides (TMDs) have drawn strong attention due to their unique properties and diverse applications. However, TMD performance depends strongly on material quality and defect morphology. Experiments show that samples grown by chemical vapor deposition (CVD) outperform those obtained by physical vapor deposition (PVD). Experiments also show that CVD samples exhibit vacancy defects, while antisite defects are frequently observed in PVD samples. Our time-domain ab initio study demonstrates that both antisites and vacancies accelerate trapping and nonradiative recombination of charge carriers, but antisites are much more detrimental than vacancies. Antisites create deep traps for both electrons and holes, reducing energy gaps for recombination, while vacancies trap primarily holes. Antisites also perturb band-edge states, creating significant overlap with the trap states. In comparison, vacancy defects overlap much less with the band-edge states. Finally, antisites can create pairs of electron and hole traps close to the Fermi energy, allowing trapping by thermal activation from the ground state and strongly contributing to charge scattering. As a result, antisites accelerate charge recombination by more than a factor of 8, while vacancies enhance the recombination by less than a factor of 2. Our simulations demonstrate a general principle that missing atoms are significantly more benign than misplaced atoms, such as antisites and adatoms. The study rationalizes the existing experimental data, provides theoretical insights into the diverse behavior of different classes of defects, and generates guidelines for defect engineering to achieve high-performance electronic, optoelectronic, and solar-cell devices.

The role of hydrogenated amorphous silicon oxide buffer layer on improving the performance of hydrogenated amorphous silicon germanium single-junction solar cells

NASA Astrophysics Data System (ADS)

Sritharathikhun, Jaran; Inthisang, Sorapong; Krajangsang, Taweewat; Krudtad, Patipan; Jaroensathainchok, Suttinan; Hongsingtong, Aswin; Limmanee, Amornrat; Sriprapha, Kobsak

2016-12-01

Hydrogenated amorphous silicon oxide (a-Si1-xOx:H) film was used as a buffer layer at the p-layer (μc-Si1-xOx:H)/i-layer (a-Si1-xGex:H) interface for a narrow band gap hydrogenated amorphous silicon germanium (a-Si1-xGex:H) single-junction solar cell. The a-Si1-xOx:H film was deposited by plasma enhanced chemical vapor deposition (PECVD) at 40 MHz in a same processing chamber as depositing the p-type layer. An optimization of the thickness of the a-Si1-xOx:H buffer layer and the CO2/SiH4 ratio was performed in the fabrication of the a-Si1-xGex:H single junction solar cells. By using the wide band gap a-Si1-xOx:H buffer layer with optimum thickness and CO2/SiH4 ratio, the solar cells showed an improvement in the open-circuit voltage (Voc), fill factor (FF), and short circuit current density (Jsc), compared with the solar cells fabricated using the conventional a-Si:H buffer layer. The experimental results indicated the excellent potential of the wide-gap a-Si1-xOx:H buffer layers for narrow band gap a-Si1-xGex:H single junction solar cells.

Electrical Characterization of Amorphous Silicon MIS-Based Structures for HIT Solar Cell Applications.

PubMed

García, Héctor; Castán, Helena; Dueñas, Salvador; Bailón, Luis; García-Hernansanz, Rodrigo; Olea, Javier; Del Prado, Álvaro; Mártil, Ignacio

2016-12-01

A complete electrical characterization of hydrogenated amorphous silicon layers (a-Si:H) deposited on crystalline silicon (c-Si) substrates by electron cyclotron resonance chemical vapor deposition (ECR-CVD) was carried out. These structures are of interest for photovoltaic applications. Different growth temperatures between 30 and 200 °C were used. A rapid thermal annealing in forming gas atmosphere at 200 °C during 10 min was applied after the metallization process. The evolution of interfacial state density with the deposition temperature indicates a better interface passivation at higher growth temperatures. However, in these cases, an important contribution of slow states is detected as well. Thus, using intermediate growth temperatures (100-150 °C) might be the best choice.

Degradation of L-Ascorbic Acid in the Amorphous Solid State.

PubMed

Sanchez, Juan O; Ismail, Yahya; Christina, Belinda; Mauer, Lisa J

2018-03-01

Ascorbic acid degradation in amorphous solid dispersions was compared to its degradation in the crystalline state. Physical blends and lyophiles of ascorbic acid and polymers (pectins and polyvinylpyrrolidone [PVP]) were prepared initially at 50:50 (w/w), with further studies using the polymer that best inhibited ascorbic acid crystallization in the lyophiles in 14 vitamin : PVP ratios. Samples were stored in controlled environments (25 to 60 °C, 0% to 23% RH) for 1 mo and analyzed periodically to track the physical appearance, change in moisture content, physical state (powder x-ray diffraction and polarized light microscopy), and vitamin loss (high performance liquid chromatography) over time. The glass transition temperatures of select samples were determined using differential scanning calorimetry, and moisture sorption profiles were generated. Ascorbic acid in the amorphous form, even in the glassy amorphous state, was more labile than in the crystalline form in some formulations at the highest storage temperature. Lyophiles stored at 25 and 40 °C and those in which ascorbic acid had crystallized at 60 °C (≥70% ascorbic acid : PVP) had no significant difference in vitamin loss (P > 0.05) relative to physical blend controls, and the length of storage had little effect. At 60 °C, amorphous ascorbic acid lyophiles (≤60% ascorbic acid : PVP) lost significantly more vitamin (P < 0.05) relative to physical blend controls after 1 wk, and vitamin loss significantly increased over time. In these lyophiles, vitamin degradation also significantly increased (P < 0.05) at lower proportions of ascorbic acid, a scenario likely encountered in foods wherein vitamins are naturally present or added at low concentrations and production practices may promote amorphization of the vitamin. Vitamin C is one of the most unstable vitamins in foods. This study documents that amorphous ascorbic acid is less stable than crystalline ascorbic acid in some environments (for example

Compensated amorphous silicon solar cell

DOEpatents

Devaud, Genevieve

1983-01-01

An amorphous silicon solar cell including an electrically conductive substrate, a layer of glow discharge deposited hydrogenated amorphous silicon over said substrate and having regions of differing conductivity with at least one region of intrinsic hydrogenated amorphous silicon. The layer of hydrogenated amorphous silicon has opposed first and second major surfaces where the first major surface contacts the electrically conductive substrate and an electrode for electrically contacting the second major surface. The intrinsic hydrogenated amorphous silicon region is deposited in a glow discharge with an atmosphere which includes not less than about 0.02 atom percent mono-atomic boron. An improved N.I.P. solar cell is disclosed using a BF.sub.3 doped intrinsic layer.

Preparation and analysis of particulate metal deposits

NASA Technical Reports Server (NTRS)